CN103881122A - Preparation method of polyvinyl chloride/nano-tin dioxide composite film with high visible light catalytic activity - Google Patents
Preparation method of polyvinyl chloride/nano-tin dioxide composite film with high visible light catalytic activity Download PDFInfo
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- CN103881122A CN103881122A CN201410159111.7A CN201410159111A CN103881122A CN 103881122 A CN103881122 A CN 103881122A CN 201410159111 A CN201410159111 A CN 201410159111A CN 103881122 A CN103881122 A CN 103881122A
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Abstract
The invention discloses a preparation method of a polyvinyl chloride/nano-tin dioxide composite film with high visible light catalytic activity and belongs to the technical field of environmental purification photocatalyst new materials. The preparation method comprises the following steps: firstly preparing nano-tin dioxide by adopting a microwave heating method, then dispersing the obtained nano-tin dioxide in tetrahydrofuran to form a translucent suspension, then mixing the suspension with a tetrahydrofuran solution containing polyvinyl chloride at a certain ratio, uniformly stirring, then coating to form a film by adopting a spin-coating method, and performing heat treatment after volatilization of a solvent to obtain the polyvinyl chloride/nano-tin dioxide composite film with the high visible light catalytic activity. The preparation method disclosed by the invention has the advantage of extensive raw material sources, the preparation method is simple, and the obtained composite film has excellent light catalytic activity under visible light and stability, can be easily separated and recovered from a degradation solution and is suitable for industrial applications.
Description
Technical field
The preparation method who the present invention relates to a kind of polyvinyl chloride/nano tindioxide composite membrane of high visible light catalytic activity, belongs to environmental purification photocatalyst new material technology field.
Background technology
Along with the rapid growth of industrialization and population, environmental pollution and energy shortage have become global crisis and have caused extensive concern.In all kinds of environmental purification, clean energy research, conductor photocatalysis is acknowledged as the Green Chemical Technology most with application prospect.Photocatalitic Technique of Semiconductor is chemical energy or electric energy take nano semiconductor material as catalyzer by light energy conversion, has widespread use in fields such as photocatalytic degradation environmental pollutant, water decomposition hydrogen manufacturing, solar cell photoelectric conversions.
Conductor photocatalysis material is the key of photocatalysis technology, also be study hotspot problem, Chinese scholars has been carried out research deeply and widely to many eurypalynous conductor photocatalysis materials such as metal oxide, metallic sulfide, silver-colored based compound, bismuth based compound always.Wherein nano titanium oxide, tindioxide have that photocatalytic activity is high, oxidation capacity is strong, corrosion-resistant, chemical stability good and the advantage such as inexpensive, wide material sources, especially nano-stannic oxide also has excellent air-sensitive and photoelectric properties, can be used for photocatalyst, solar cell, sensor, lithium ion battery etc., is the photocatalyst material that a class has application future most.But tindioxide is the N-shaped semiconductor material of broad stopband (Eg=3.3eV～3.6eV), only under ultraviolet excitation, just can show excellent photocatalysis performance, but UV-light only accounts for 3%～5% in sunlight, this has limited the practical application of tindioxide to a great extent.The method of modifying of taking in order to expand its photoresponse scope have ion doping, with other semiconductor material (as ZnO, CdS, Fe
2o
3, Ag
3pO
4) compound, compound etc. with Graphene and carbonaceous material, these methods can significantly improve the visible light catalysis activity of tindioxide, but also have the problems such as volume is wayward, process is complicated.
Another important factor that affects the actual commercial application of Nano semiconductor photocatalyst material is, the particle diameter of nano particle is very little, adopt common separation method to be difficult to its Separation and Recovery from pollutent waste water, employing high speed centrifugation or membrane separation plant separate slow and cost is expensive.The main method of taking in application is at present that photocatalyst nano particle is loaded on some carrier, but carrier itself is not while thering is no photo-catalysis capability, can affect to a certain extent the catalytic efficiency of photocatalyst material.
Summary of the invention
The technical problem to be solved in the present invention is to provide polyvinyl chloride/nano tindioxide composite membrane of a kind of high visible light catalytic activity and preparation method thereof.The composite membrane standby with this legal system shows excellent photocatalytic activity and stability under visible ray, solved the problem of photocatalyst material Separation and Recovery difficulty simultaneously.
For solving the problems of the technologies described above technical scheme of the present invention be, first adopt microwave heating method to prepare nano-stannic oxide, then gained nano-stannic oxide is scattered in and in tetrahydrofuran (THF), forms translucent suspension, afterwards this suspension is mixed with the tetrahydrofuran solution containing polyvinyl chloride with certain proportion, after stirring, adopt spin-coating method coating film forming, after tetrahydrofuran solvent volatilization, can obtain the polyvinyl chloride/nano tindioxide composite membrane of high visible light catalytic activity through thermal treatment.
The preparation method of the polyvinyl chloride/nano tindioxide composite membrane of high visible light catalytic activity of the present invention mainly comprises the steps:
A preparation method for the polyvinyl chloride/nano tindioxide composite membrane of high visible light catalytic activity, is characterized in that comprising the steps:
A. by SnCl
45H
2o solid is dissolved in dehydrated alcohol, is mixed with the ethanolic soln that tin tetrachloride concentration is 0.50～0.60mol/L; Separately strong aqua is joined in distilled water and diluted, be mixed with the dilute ammonia solution that ammonia concn is 0.83～0.92mol/L;
B. the tin tetrachloride ethanolic soln 20mL～30mL described in removing step a joins in flask, under agitation condition, splash into the dilute ammonia solution 0.10～0.20mL described in step a, slowly add again afterwards 100～150mL distilled water, continue to stir 10min～15min reaction solution is mixed;
C. will put into microwave reactor containing the flask of reaction solution described in b in steps, first regulating microwave reactor power is 400W, temperature rise rate is 8 ℃/min～12 ℃/min, while under agitation reacting 7min～9min, reacting liquid temperature reaches 90 ℃～95 ℃, reaction solution is become gradually muddy and then is become white suspension from achromaticity and clarification, continue reaction 1min～3min, and then adjusting microwave reactor power is 700W, make reaction solution at 95 ℃～105 ℃ back flow reaction 8min～10min, reacting complete at room temperature filters gained suspension after airtight ageing 1h～5h, separate, obtain filter cake,
D. after step c gained filter cake being placed in to beaker, put into microwave oven, in employing, low fire, moderate heat, high fire and moderate heat respectively heat 3min～5min, and intermittently 1min～1.5min of firepower conversion, obtains white powder, and gained white powder is ground, and obtains nano-stannic oxide;
E. steps d gained nano-stannic oxide is scattered in tetrahydrofuran (THF), the mass percentage concentration of controlling nano-stannic oxide is 1.0%～3.0%, stirs 20min～40min, forms the homodisperse translucent suspension of nano-stannic oxide; In addition polyvinyl chloride is dissolved in tetrahydrofuran (THF) to the tetrahydrofuran solution that to be mixed with containing polyvinyl chloride mass concentration be 0.5%～2.0%;
F. be 1:2～1:5 according to the mass ratio of polyvinyl chloride and nano-stannic oxide, the tetrahydrofuran solution of polyvinyl chloride described in step e is mixed with nano-stannic oxide suspension, stirring 10min～15min mixes it, adopt afterwards spin-coating method coating film forming, after tetrahydrofuran solvent volatilization, be placed in again thermal treatment 1h～3h at 130 ℃～150 ℃, obtain polyvinyl chloride/nano tindioxide composite membrane.
Preferably, in described step b, the mass concentration of tin tetrachloride in reaction solution is 0.08mol/L～0.12mol/L, and the mass ratio of tin tetrachloride and water is 1:30～1:35.。
Preferably, adopt microwave heating reaction solution in step c, power is that 400W the reaction time is 9min～11min, and power is that 700W the reaction time is 9min～10min.
Preferably, in steps d microwave heating adopt in low fire, moderate heat, high fire and the each 3min of moderate heat, between firepower conversion, stop heating 1min.
Preferably, in step f, the mass ratio of polyvinyl chloride and nano-stannic oxide is 1:2～1:4, and the thermal treatment temp of polyvinyl chloride/nano tindioxide composite membrane is 140 ℃～150 ℃, and heat treatment time is 2h～3h.
The advantage that the present invention compared with prior art has is:
(1) polyvinyl chloride/nano tindioxide composite membrane after heat treatment, the polyvinyl chloride molecular chain on film surface can remove hydrogenchloride and produce carbon-carbon double bond formation conjugated structure, can improve the absorption of composite membrane to visible ray, and light induced electron can inject the conduction band of nano-stannic oxide, the separation efficiency that improves light induced electron/hole in composite membrane, therefore prepared composite membrane has excellent visible light catalysis activity and stability.
(2) polyvinyl chloride is polymers for general use, and source is wide, and cost is low; In addition, waste polyvinyl chloride can be for the preparation of this composite membrane, and this just prepares surrounding purifying material for polyvinyl chloride recycling provides an approach.
(3) preparation method of the present invention is fairly simple, and composite membrane very easily separates with degradation solution, has solved photocatalyst and has reclaimed difficult problem, is suitable for industrial applications.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope diagram sheet of the prepared polyvinyl chloride/nano tindioxide composite membrane of embodiment 1;
Fig. 2 is the transmission electron micrograph of the prepared polyvinyl chloride/nano tindioxide composite membrane of embodiment 1;
Fig. 3 is that the UV-Vis DRS of the prepared polyvinyl chloride/nano tindioxide composite membrane (a) of embodiment 1 and nano-stannic oxide (b) absorbs collection of illustrative plates;
Fig. 4 is that polyvinyl chloride/nano tindioxide composite membrane is cycled to used in catalyzed degradation rhodamine B experimental result picture under visible ray.
Embodiment
The present invention is described in detail to use specific embodiment below:
Embodiment 1
Take SnCl
45H
2o solid 4.20g is dissolved in 20mL dehydrated alcohol, under agitation condition, splash into the dilute ammonia solution 0.10mL of 0.85mol/L, and then slowly add 100mL distilled water, and continue to stir 15min, after question response liquid mixes, the flask that reaction solution is housed is put into microwave reactor, first under 400W power, heat, when reaction 7min, reacting liquid temperature rises to 90 ℃ of left and right, and reaction solution becomes white suspension from achromaticity and clarification, being reacted to regulating power after 10min is 700W, continues reaction 10min.By gained suspension ageing 3h in confined conditions, incline after supernatant liquor and filter, obtain filter cake, filter cake is put into microwave oven after being placed in beaker, in first using, low fire heating 3min, opens afterwards fire door heat radiation 1min, respectively heats 3min with moderate heat, high fire and moderate heat respectively, the 1min that all dispels the heat between same each conversion firepower, grinds gained nano-stannic oxide.Taking 0.10g nano-stannic oxide joins in 4.90g tetrahydrofuran (THF), stirring 2h is uniformly dispersed to nano-stannic oxide, then be 1:3 according to the mass ratio of polyvinyl chloride and nano-stannic oxide, add the tetrahydrofuran solution 3.33g that the polyvinyl chloride mass concentration for preparing is in advance 1.0%, filling into tetrahydrofuran (THF), to make total amount of liquid be 10.0g, airtight stirring 20min mixes to it, adopt afterwards spin-coating method coating film forming, after tetrahydrofuran solvent volatilization, be placed in again thermal treatment 2h at 150 ℃, obtain polyvinyl chloride/nano tindioxide composite membrane.
The scanning electron microscope diagram sheet of the prepared polyvinyl chloride/nano tindioxide composite membrane of the present embodiment as shown in Figure 1, can find out that stannic oxide particle is dispersed in composite membrane.The transmission electron micrograph of the polyvinyl chloride/nano tindioxide composite membrane being shown by Fig. 2 can find out, stannic oxide particle is to be flowers shape by the elliposoidal nano-stannic oxide of the about 10nm～20nm of median size to assemble and form.Fig. 3 is that the prepared polyvinyl chloride/nano tindioxide composite membrane (a) of the present embodiment 1 absorbs collection of illustrative plates with the UV-Vis DRS of nano-stannic oxide (b), X-coordinate is wavelength nm, ordinate zou is absorbancy, as seen from Figure 3, the photoabsorption in whole visible spectrum of polyvinyl chloride/nano tindioxide composite membrane is significantly higher than the photoabsorption of nano-stannic oxide.
The photocatalysis performance test of prepared polyvinyl chloride/nano tindioxide composite membrane is as follows: in wall surface has prepared the reactor of polyvinyl chloride/nano tindioxide composite membrane, adding 120mL concentration is the rhodamine B solution of 4mg/L, under dark condition, bubbling 120min reaches after balance to adsorbing, open visible light source (300W xenon lamp added a cover spectral filter filtering the following light of 400nm) irradiation, from reaction system, sample 3mL at interval of 20min, adopt spectrophotometer to measure absorbancy at rhodamine B maximum absorption wavelength 552nm place, obtained the degraded situation of rhodamine B in solution by the variation of absorbancy.Experiment records, and during take prepared polyvinyl chloride/nano tindioxide composite membrane as photocatalyst illumination degrading 100min, the degradation rate of rhodamine B is reached to 93%, and under similarity condition, nano-stannic oxide is 43% to the degradation rate of rhodamine B.
Embodiment 2
Take SnCl
45H
2o solid 6.30g is dissolved in 30mL dehydrated alcohol, under agitation condition, splash into the dilute ammonia solution 0.15mL of 0.90mol/L, and then slowly add 150mL distilled water, continue to stir 15min, after question response liquid mixes, the flask that reaction solution is housed is put into microwave reactor, first reacting by heating 10min under 400W power, then regulating power is that 700W continues reaction 10min.By gained suspension ageing 5h in confined conditions, incline after supernatant liquor and filter, filter cake is put into microwave oven after being placed in beaker, low fire heating 3min in first using, open afterwards fire door heat radiation 1min, respectively heat 3min with moderate heat, high fire and moderate heat respectively again, the 1min that all dispels the heat between same each conversion firepower, grinds gained nano-stannic oxide.Taking prepared nano-stannic oxide 0.10g joins in 4.90g tetrahydrofuran (THF), stirring 2h is uniformly dispersed to nano-stannic oxide, then be 1:3.5 according to the mass ratio of polyvinyl chloride and nano-stannic oxide, add the tetrahydrofuran solution 2.86g that the polyvinyl chloride mass concentration for preparing is in advance 1.0%, filling into tetrahydrofuran (THF), to make total amount of liquid be 10.0g, airtight stirring 20min mixes to it, adopt afterwards spin-coating method coating film forming, after tetrahydrofuran solvent volatilization, be placed in again thermal treatment 2.5h at 145 ℃, obtain polyvinyl chloride/nano tindioxide composite membrane.Experiment records when the prepared polyvinyl chloride/nano tindioxide of this embodiment composite membrane is photocatalyst illumination degrading 100min the degradation rate of rhodamine B is reached to 91%.
Embodiment 3
Take SnCl
45H
2o solid 4.20g is dissolved in 20mL dehydrated alcohol, under agitation condition, splash into the dilute ammonia solution 0.10mL of 0.85mol/L, and then slowly add 100mL distilled water, continue to stir 15min, after question response liquid mixes, the flask that reaction solution is housed is put into microwave reactor, first reacting by heating 10min under 400W power, then regulating power is that 700W continues reaction 10min.Gained suspension is filtered after ageing 2h in confined conditions, filter cake is put into microwave oven after being placed in beaker, low fire heating 3min in first using, open afterwards fire door heat radiation 1min, respectively heat 3min with moderate heat, high fire and moderate heat respectively again, the 1min that all dispels the heat between same each conversion firepower, grinds gained nano-stannic oxide.Taking prepared nano-stannic oxide 0.10g joins in 4.90g tetrahydrofuran (THF), stirring 2h is uniformly dispersed to nano-stannic oxide, then be 1:4 according to the mass ratio of polyvinyl chloride and nano-stannic oxide, add the tetrahydrofuran solution 5.0g that the polyvinyl chloride mass concentration for preparing is in advance 0.50%, airtight stirring 20min mixes to it, adopt afterwards spin-coating method by coating film forming, after tetrahydrofuran solvent volatilization, be placed in again thermal treatment 2h at 150 ℃, obtain polyvinyl chloride/nano tindioxide composite membrane.Experiment records when the prepared polyvinyl chloride/nano tindioxide of this embodiment composite membrane is photocatalyst illumination degrading 100min the degradation rate of rhodamine B is reached to 90%.
Embodiment 4
Taking the prepared nano-stannic oxide 0.10g of embodiment 1 joins in 4.90g tetrahydrofuran (THF), stirring 2h is uniformly dispersed to nano-stannic oxide, then be 1:3 according to the mass ratio of polyvinyl chloride and nano-stannic oxide, add the tetrahydrofuran solution 3.33g that the polyvinyl chloride mass concentration for preparing is in advance 1.0%, filling into tetrahydrofuran (THF), to make total amount of liquid be 10.0g, airtight stirring 20min mixes to it, adopt afterwards spin-coating method by this suspension coating film forming, after solvent evaporates, be placed in again thermal treatment 2h at 150 ℃, obtain polyvinyl chloride/nano tindioxide composite membrane.Rhodamine B degradation that this composite membrane is circulated under visible ray tests to investigate its photochemical catalysis stability.In circulation experiment, after polyvinyl chloride/nano tindioxide composite membrane photocatalytic degradation rhodamine B aqueous solution 100min, composite membrane is through washing, dry, and then once for the test of photocatalytic degradation rhodamine B.Circulate under the visible ray experimental result picture of catalyzed degradation rhodamine B of polyvinyl chloride/nano tindioxide composite membrane as shown in Figure 4 can be found out, after 10 times recycle, this composite membrane is still keeping good photocatalytic activity, show that this composite membrane has excellent photochemical catalysis stability, the X-coordinate of Fig. 4 is time min, and ordinate zou is degradation rate.
Claims (5)
1. a preparation method for the polyvinyl chloride/nano tindioxide composite membrane of high visible light catalytic activity, is characterized in that comprising the steps:
A. by SnCl
45H
2o solid is dissolved in dehydrated alcohol, is mixed with the ethanolic soln that tin tetrachloride concentration is 0.50～0.60mol/L; Separately strong aqua is joined in distilled water and diluted, be mixed with the dilute ammonia solution that ammonia concn is 0.83～0.92mol/L;
B. the tin tetrachloride ethanolic soln 20mL～30mL described in removing step a joins in flask, under agitation condition, splash into the dilute ammonia solution 0.10～0.20mL described in step a, slowly add again afterwards 100～150mL distilled water, continue to stir 10min～15min reaction solution is mixed;
C. will put into microwave reactor containing the flask of reaction solution described in b in steps, first regulating microwave reactor power is 400W, temperature rise rate is 8 ℃/min～12 ℃/min, while under agitation reacting 7min～9min, reacting liquid temperature reaches 90 ℃～95 ℃, reaction solution is become gradually muddy and then is become white suspension from achromaticity and clarification, continue reaction 1min～3min, and then adjusting microwave reactor power is 700W, make reaction solution at 95 ℃～105 ℃ back flow reaction 8min～10min, reacting complete at room temperature filters gained suspension after airtight ageing 1h～5h, separate, obtain filter cake,
D. after step c gained filter cake being placed in to beaker, put into microwave oven, in employing, low fire, moderate heat, high fire and moderate heat respectively heat 3min～5min, and intermittently 1min～1.5min of firepower conversion, obtains white powder, and gained white powder is ground, and obtains nano-stannic oxide;
E. steps d gained nano-stannic oxide is scattered in tetrahydrofuran (THF), the mass percentage concentration of controlling nano-stannic oxide is 1.0%～3.0%, stirs 20min～40min, forms the homodisperse translucent suspension of nano-stannic oxide; In addition polyvinyl chloride is dissolved in tetrahydrofuran (THF) to the tetrahydrofuran solution that to be mixed with containing polyvinyl chloride mass concentration be 0.5%～2.0%;
F. be 1:2～1:5 according to the mass ratio of polyvinyl chloride and nano-stannic oxide, the tetrahydrofuran solution of polyvinyl chloride described in step e is mixed with nano-stannic oxide suspension, stirring 10min～15min mixes it, adopt afterwards spin-coating method coating film forming, after tetrahydrofuran solvent volatilization, be placed in again thermal treatment 1h～3h at 130 ℃～150 ℃, obtain polyvinyl chloride/nano tindioxide composite membrane.
2. the preparation method of the polyvinyl chloride/nano tindioxide composite membrane of a kind of high visible light catalytic activity as claimed in claim 1, it is characterized in that, in described step b, the mass concentration of tin tetrachloride in reaction solution is 0.08mol/L～0.12mol/L, and the mass ratio of tin tetrachloride and water is 1:30～1:35.
3. the preparation method of the polyvinyl chloride/nano tindioxide composite membrane of a kind of high visible light catalytic activity as claimed in claim 1, it is characterized in that, in step c, adopt microwave heating reaction solution, power is that 400W the reaction time is 9min～11min, and power is that 700W the reaction time is 9min～10min.
4. the preparation method of the polyvinyl chloride/nano tindioxide composite membrane of a kind of high visible light catalytic activity as claimed in claim 1, it is characterized in that, in steps d microwave heating adopt in low fire, moderate heat, high fire and the each 3min of moderate heat, between firepower conversion, stop heating 1min.
5. the preparation method of the polyvinyl chloride/nano tindioxide composite membrane of a kind of high visible light catalytic activity as claimed in claim 1, it is characterized in that, in step f, the mass ratio of polyvinyl chloride and nano-stannic oxide is 1:2～1:4, the thermal treatment temp of polyvinyl chloride/nano tindioxide composite membrane is 140 ℃～150 ℃, and heat treatment time is 2h～3h.
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| CN110467216A (en) * | 2019-08-16 | 2019-11-19 | 江西理工大学 | A kind of micron order hollow square shape SnO2And preparation method |
| CN110482595A (en) * | 2019-08-16 | 2019-11-22 | 江西理工大学 | A kind of microwave-assisted liquid phase synthesis SnO2The method of micron ball |
| CN111760461A (en) * | 2020-06-24 | 2020-10-13 | 上海应用技术大学 | Preparation method of polyvinylidene fluoride mixed matrix film |
| CN112574446A (en) * | 2020-12-09 | 2021-03-30 | 黎银茵 | PVC composite membrane with high visible light catalytic activity and preparation method thereof |
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| CN112574446A (en) * | 2020-12-09 | 2021-03-30 | 黎银茵 | PVC composite membrane with high visible light catalytic activity and preparation method thereof |
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