CN103769073B - A kind of preparation method of potassium doped nanometer titanium dioxide photocatalyst - Google Patents

A kind of preparation method of potassium doped nanometer titanium dioxide photocatalyst Download PDF

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CN103769073B
CN103769073B CN201410017821.6A CN201410017821A CN103769073B CN 103769073 B CN103769073 B CN 103769073B CN 201410017821 A CN201410017821 A CN 201410017821A CN 103769073 B CN103769073 B CN 103769073B
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potassium
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butyl titanate
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CN103769073A (en
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景晓辉
程海军
丁欣宇
曹宇锋
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Nantong University
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Abstract

The present invention relates to a kind of preparation method of potassium doped nanometer titanium dioxide photocatalyst.The present invention is doped chemical with potassium, and potassium is incorporated into TiO 2lattice in, prevent the compound in light induced electron and hole, impel spectral response range to move to visible region, effectively improve the photocatalytic activity of titanium dioxide.Potassium doped titanium dioxide photocatalytic activity prepared by the inventive method is high, good to the treatment effect of organic wastewater; Present invention process is simple, condition is easily controlled, production cost is low, be convenient to large-scale production.

Description

A kind of preparation method of potassium doped nanometer titanium dioxide photocatalyst
Technical field
The present invention relates to a kind of preparation method of potassium doped nanometer titanium dioxide photocatalyst.
Background technology
The improvement that nano titanium oxide is used for pollutant as catalyst has the advantages such as catalyst itself is stable, non-secondary pollution, applicable pollutant are wide.But the electronics of optical excitation generation and the very easily compound in hole, cause quantum yield very low, limit TiO 2catalysis technique application in practice; In addition, TiO 2be wide bandgap semiconductor, the ultraviolet light needing energy higher just can make the electronics in its valence band be excited, and accounts for most visible light parts and then fail effectively to utilize in solar spectrum.So, effectively reduce the right compound of photo-generate electron-hole, improve TiO 2photocatalytic activity and efficiency, expansion TiO 2spectral response amplitude, just can make TiO 2catalyst is better applied.
Doped with metal elements prepares high activity TiO 2effective ways [the Long Huijin of visible light catalyst, Wang Enjun, Dong Jiangzhou, Wang Lingling, the research [J] of Cao Yong strong .In ions doped titanium dioxide nanotube visible light catalysis activity. chemical journal, 200967 (14): 1533 ~ 1538], doped with metal elements utilizes physics or chemical method exactly, and metallic element is incorporated into TiO in the form of an ion 2in lattice, in its forbidden energy gap, introduce impurity energy level and defect level, thus widen TiO 2the spectral response range of photochemical catalyst, more effectively utilizes visible luminous energy.Meanwhile, in titanium dioxide lattice, mix Suitable metal elements, become the trap of catching photo-generated carrier, suppress the compound in electronics and hole, improve TiO 2photocatalysis efficiency and quantum yield [TongTZ, ZhangJL, TianBZ, ChenF, HeDN.PreparationofF 3+dopedTiO 2catalystsbycontrolledhydrolysisoftitaniumalkoxideandstud yontheirphotocatalyticactivityformethylorangedegradation [J] .JournalofHazardousMaterials, 2008,155 (3): 572-579.].
The factor of impact doping effect is comparatively complicated, and different types of metal ion can cause the effect of different doping, and playing of having improves TiO 2photolytic activity, widens the effect of absorbing wavelength, the then counterproductive had.Even if congener metal ion, also different doping effects may be caused because doping method is different.Many factors, as doping content, ion combination valency, sintering temperature etc. all can affect the photocatalytic activity after metal ion mixing.
Although doped with metal elements TiO 2research report more, but most doped chemical concentrates on as the rare earth metals such as La, Ce, Er, Pr, Gd, Nd, Sm, Zn, Fe, Ag, transition metal and noble metal so far, and these doped with metal elements preparation costs are high, are difficult to obtain practical application.
Summary of the invention
The object of the present invention is to provide a kind of photocatalytic activity high, process is simple, and production cost is low, the potassium doped nanometer titanium dioxide photocatalyst of being convenient to large-scale production and preparation method thereof.
Technical solution of the present invention is:
A preparation method for potassium doped nanometer titanium dioxide photocatalyst, is characterized in that, described preparation comprises following concrete steps:
(1) under room temperature and stirring, butyl titanate is slowly added drop-wise in absolute ethyl alcohol by the volume ratio being 1:3.5 ~ 3.7 by butyl titanate and absolute ethyl alcohol, the volume ratio being 1:3.0 ~ 3.3 by acetylacetone,2,4-pentanedione and butyl titanate adds acetylacetone,2,4-pentanedione, the volume ratio being 1:1.3 ~ 1.5 by triton x-100 and butyl titanate adds triton x-100, then add polyethylene glycol in the ratio of 0.05 ~ 0.06g (polyethylene glycol)/mL (butyl titanate), continue stirring and obtain solution A;
(2) under room temperature and stirring, by the doping content of the molar percentage 4.5% ~ 6.5% of Ti element in K element and butyl titanate, potassium hydroxide or potassium nitrate or potash or potassium chloride or potassium sulfate are joined in redistilled water, adding by redistilled water and absolute ethyl alcohol is again the water prepared of 1:3 volume ratio and alcohol mixeding liquid, and be 2 ~ 3 with the salt acid for adjusting pH value of 1:1, stir to obtain solution B;
(3) solution B is slowly added drop-wise in solution A by the volume ratio being 1:3.2 ~ 3.4 by solution B and solution A under stirring, continues to stir to obtain yellowish vitreosol;
(4) colloidal sol at room temperature left standstill, after natural ageing to gel, put it into the inherent 100 ° of C ~ 120 ° C of baking oven and be dried to xerogel;
(5) xerogel is milled into powdery, puts in people's Muffle furnace, be warming up to 550 ° of C ~ 650 ° C roasting 2.5 ~ 3.0h, naturally cool to room temperature, take out grinding and namely obtain potassium dopen Nano TiO 2photochemical catalyst.
Further, in described step (1), mixing time is 2 hours.
Further, in described step (2), mixing time is 0.2 hour.
Further, in described step (3), mixing time is 2 hours.
Further, in described step (5), by 5 ° of C/min temperature programming to 550 ° C ~ 650 ° C roasting 2.5 ~ 3.0h.
The present invention has following feature and beneficial effect:
(1) the potassium dopen Nano TiO for preparing of the present invention 2photochemical catalyst, K +evenly spread to TiO 2in lattice, inhibit TiO 2particle size growth, refinement crystal grain, adds specific area, improves photocatalytic activity.
(2) K +enter TiO 2ti is replaced in lattice 4+, cause distortion of lattice and expansion, cause Lacking oxygen and lattice defect, become photo-generate electron-hole and catch trap, effectively stop the compound in electronics and hole, improve catalytic activity.The K mixed +enter TiO 2lattice also replaces Ti + 4, in forbidden band, form acceptor level, forbidden band narrowed, widened TiO 2visible light-responded scope, make K +doped Ti O 2there is higher visible light catalysis activity.
(3) process is simple, and easy to operate, raw material is easy to get, and preparation cost is low.
Accompanying drawing explanation
Fig. 1 is potassium dopen Nano TiO prepared by the embodiment of the present invention 2 2with non-dopen Nano TiO 2x-ray (XRD) spectrogram contrast;
Fig. 2 is potassium dopen Nano TiO prepared by the embodiment of the present invention 5 2eDS power spectrum;
Fig. 3 is non-doped Ti O 2eDS power spectrum;
Fig. 4 is potassium dopen Nano TiO prepared by the embodiment of the present invention 8 2uv-visible absorption spectra figure;
Fig. 5 is non-doped Ti O 2the uv-visible absorption spectra figure of powder.
Detailed description of the invention
Embodiment 1:
Under stirring, the butyl titanate of 20mL is slowly added drop-wise to after in the absolute ethyl alcohol of 70mL, adds the acetylacetone,2,4-pentanedione of 6.7mL and the triton x-100 of 15.4mL respectively, then add 1g polyethylene glycol, continue stirring and obtain solution A in 2 hours; 0.1532g potassium hydroxide is joined in 8mL redistilled water, then to add by redistilled water and absolute ethyl alcohol be the water prepared of 1:3 volume ratio and alcohol mixeding liquid, and be 3 with the salt acid for adjusting pH value of 1:1, stir 0.2 hour to obtain solution B; Solution B is slowly added drop-wise in solution A by the volume ratio being 1:3.2 by solution B and solution A, dropwises that rear continuation stirring at room temperature left standstill after 2 hours, natural ageing is to gel.Baking oven is put in 100 DEG C of oven dry after gel being poured into pallet, pour crucible into after xerogel being milled into powdery, put in people's Muffle furnace, by 5 ° of C/min temperature programmings to 550 ° C roasting 2.5h, then naturally cool to room temperature, take out grinding and namely obtain the potassium dopen Nano TiO that doping content is 4.5% 2photochemical catalyst.
Embodiment 2:
Present embodiment is as different from Example 1: sintering temperature is 650 ° of C, and other is identical with embodiment 1.Gained potassium dopen Nano TiO 2with non-dopen Nano TiO 2x-ray (XRD) spectrogram contrast see Fig. 1.
As can be seen from Figure 1, to non-doped Ti O 2, there is Rutile Type in crystal, and to doped Ti O 2, can find out that 101 diffraction maximum peak shapes come to a point due to potassium doping, peak value grow, not occur Rutile Type diffraction maximum.Show K +doping prevents the generation of Rutile Type.XRD does not detect potassium oxide diffraction maximum, shows K +mix completely and evenly spread to TiO 2lattice in and define solid solution with it.Potassium dopen Nano TiO is gone out according to Scherrer formulae discovery 2size of microcrystal is 17.9nm, and non-doped Ti O 2particle diameter is 30.7nm, and K is described +doping inhibit TiO 2particle size growth, refinement crystal grain.The full-automatic specific surface area analysis instrument fast of Micromeritics company ASAP2010 type is adopted to determine potassium dopen Nano TiO 2bET be 57.43m 2/ g, and non-doped Ti O 2bET be 35.07m 2/ g, shows that potassium doping prevents TiO 2reunion, add specific area.According to solid-state physics band theory, at TiO 2in crystal, Ti 4+o 2-ion coordination number is 6, the Ti of hexa-coordinate 4+radius is 0.074nm, K +radius be 0.133nm.Work as K +during doping, K +ti in lattice can be replaced 4+position, due to K +ionic radius be greater than Ti 4+ionic radius, K +replace Ti 4+after inherently cause TiO 2lattice dilatation and distortion, cause Lacking oxygen and lattice defect, become photo-generate electron-hole and catch trap, effectively stops the compound in electronics and hole, improve catalytic activity.The K mixed +enter TiO 2lattice also replaces Ti + 4, in forbidden band, form acceptor level, forbidden band narrowed, by TiO 2the visible ray that photoresponse scope is widened.
The potassium dopen Nano TiO adopting this example to prepare 2be, under the ultraviolet light of 1g/L and 300 watt, 98.5% is reached to its degradation rate during 10mg/L methyl orange solution photocatalytic degradation 20min at catalyst amount, and non-doped Ti O under the same conditions 2only have 65.2% to the degradation rate of methyl orange, photocatalytic degradation reaction rate constant is non-doped Ti O 22.02 times of reaction rate constant.Under 20 watts of visible rays, 99.1% is reached to its degradation rate during 6mg/L activated dyeing wastewater degraded 30min.
Embodiment 3:
Present embodiment is as different from Example 1: the potassium hydroxide added is 0.2213g, obtains the potassium dopen Nano TiO that doping content is 6.5% 2, other is identical with embodiment 1.
Embodiment 4:
Present embodiment is as different from Example 3: sintering temperature is 650 ° of C, and other is identical with embodiment 3.
Embodiment 5:
Under stirring, the butyl titanate of 20mL is slowly added drop-wise to after in the absolute ethyl alcohol of 74mL, adds the acetylacetone,2,4-pentanedione of 6.1mL and the triton x-100 of 13.3mL respectively, then add 1.2g polyethylene glycol, continue stirring and obtain solution A in 2 hours; 0.1973g potassium chloride is joined in 10mL redistilled water, then to add by redistilled water and absolute ethyl alcohol be the water prepared of 1:3 volume ratio and alcohol mixeding liquid, and be 2 with the salt acid for adjusting pH value of 1:1, stir 0.2 hour to obtain solution B; Solution B is slowly added drop-wise in solution A by the volume ratio being 1:3.4 by solution B and solution A, dropwises that rear continuation stirring at room temperature left standstill after 2 hours, natural ageing is to gel.Baking oven is put in 120 DEG C of oven dry after gel being poured into pallet, pour crucible into after xerogel being milled into powdery, put in people's Muffle furnace, by 5 ° of C/min temperature programmings to 550 ° C roasting 3h, then naturally cool to room temperature, take out grinding and namely obtain the potassium dopen Nano TiO that doping content is 4.5% 2photochemical catalyst.
Gained potassium dopen Nano TiO 2with non-dopen Nano TiO 2fig. 2,3 is shown in energy spectrum analysis (adopting Japanese HORIBA company EDS instrument), and energy spectrum analysis shows K +be incorporated into TiO 2in lattice.
Embodiment 6:
Present embodiment is as different from Example 5: sintering temperature is 650 ° of C, and other is identical with embodiment 5.
Embodiment 7:
Present embodiment is as different from Example 5: the potassium chloride added is 0.2411g, obtains the potassium dopen Nano TiO that doping content is 5.5% 2, other is identical with embodiment 5.
Embodiment 8:
Present embodiment is as different from Example 7: sintering temperature is 650 ° of C, and other is identical with embodiment 7.
Gained potassium dopen Nano TiO 2uv-visible absorption spectra as Fig. 4, and non-dopen Nano TiO 2uv-visible absorption spectra as Fig. 5.From Fig. 4, Fig. 5, potassium doping not only makes TiO 2maximum absorption band there occurs obvious red shift, and makes TiO 2the red shift of absorption band edge to visible region, potassium doped Ti O 2light absorption also apparently higher than not titania-doped, potassium doping enhance the absorption of titanium dioxide to visible ray, improve the utilization rate of solar energy.Under 20 watts of visible rays, 99.3% is reached to its degradation rate during 6mg/L activated dyeing wastewater degraded 30min.
Embodiment 9:
Present embodiment is as different from Example 5: the potassium chloride added is 0.285g, obtains the potassium dopen Nano TiO that doping content is 6.5% 2, other is identical with embodiment 5.
Embodiment 10:
Present embodiment is as different from Example 9: sintering temperature is 650 ° of C, and other is identical with embodiment 9.
Embodiment 11:
Under stirring, the butyl titanate of 30mL is slowly added drop-wise to after in the absolute ethyl alcohol of 105mL, adds the acetylacetone,2,4-pentanedione of 9.3mL and the triton x-100 of 21.4mL respectively, then add 1.8g polyethylene glycol, continue stirring and obtain solution A in 2 hours; 0.4034g potassium nitrate is joined in 15mL redistilled water, then to add by redistilled water and absolute ethyl alcohol be the water prepared of 1:3 volume ratio and alcohol mixeding liquid, and be 2 with the salt acid for adjusting pH value of 1:1, stir 0.2 hour to obtain solution B; Solution B is slowly added drop-wise in solution A by the volume ratio being 1:3.4 by solution B and solution A, dropwises that rear continuation stirring at room temperature left standstill after 2 hours, natural ageing is to gel.Baking oven is put in 120 DEG C of oven dry after gel being poured into pallet, pour crucible into after xerogel being milled into powdery, put in people's Muffle furnace, by 5 ° of C/min temperature programmings to 550 ° C roasting 3h, then naturally cool to room temperature, take out grinding and namely obtain the potassium dopen Nano TiO that doping content is 4.5% 2photochemical catalyst.
Embodiment 12:
Present embodiment is as different from Example 11: sintering temperature is 650 ° of C, and other is identical with embodiment 11.
Embodiment 13:
Present embodiment is as different from Example 11: the potassium nitrate added is 0.5827g, obtains the potassium dopen Nano TiO that doping content is 6.5% 2, other is identical with embodiment 11.
Embodiment 14:
Present embodiment is as different from Example 13: sintering temperature is 650 ° of C, and other is identical with embodiment 13.
Embodiment 15:
Under stirring, the butyl titanate of 30mL is slowly added drop-wise to after in the absolute ethyl alcohol of 108mL, adds the acetylacetone,2,4-pentanedione of 9.4mL and the triton x-100 of 21.5mL respectively, then add 1.8g polyethylene glycol, continue stirring and obtain solution A in 2 hours; 0.6954g potassium sulfate is joined in 15mL redistilled water, then to add by redistilled water and absolute ethyl alcohol be the water prepared of 1:3 volume ratio and alcohol mixeding liquid, and be 3 with the salt acid for adjusting pH value of 1:1, stir 0.2 hour to obtain solution B; Solution B is slowly added drop-wise in solution A by the volume ratio being 1:3.3 by solution B and solution A, dropwises that rear continuation stirring at room temperature left standstill after 2 hours, natural ageing is to gel.Baking oven is put in 110 DEG C of oven dry after gel being poured into pallet, pour crucible into after xerogel being milled into powdery, put in people's Muffle furnace, by 5 ° of C/min temperature programmings to 550 ° C roasting 3h, then naturally cool to room temperature, take out grinding and namely obtain the potassium dopen Nano TiO that doping content is 4.5% 2photochemical catalyst.
Embodiment 16:
Present embodiment is as different from Example 15: sintering temperature is 650 ° of C, and other is identical with embodiment 15.
Embodiment 17:
Present embodiment is as different from Example 15: the potassium nitrate added is 1.0045g, obtains the potassium dopen Nano TiO that doping content is 6.5% 2, other is identical with embodiment 15.
Embodiment 18:
Present embodiment is as different from Example 17: sintering temperature is 650 ° of C, and other is identical with embodiment 17.
Embodiment 19:
Under stirring, the butyl titanate of 30mL is slowly added drop-wise to after in the absolute ethyl alcohol of 108mL, adds the acetylacetone,2,4-pentanedione of 9.4mL and the triton x-100 of 21.5mL respectively, then add 1.8g polyethylene glycol, continue stirring and obtain solution A in 2 hours; 0.5487g potash is joined in 15mL redistilled water, then to add by redistilled water and absolute ethyl alcohol be the water prepared of 1:3 volume ratio and alcohol mixeding liquid, and be 3 with the salt acid for adjusting pH value of 1:1, stir 0.2 hour to obtain solution B; Solution B is slowly added drop-wise in solution A by the volume ratio being 1:3.3 by solution B and solution A, dropwises that rear continuation stirring at room temperature left standstill after 2 hours, natural ageing is to gel.Baking oven is put in 110 DEG C of oven dry after gel being poured into pallet, pour crucible into after xerogel being milled into powdery, put in people's Muffle furnace, by 5 ° of C/min temperature programmings to 550 ° C roasting 3h, then naturally cool to room temperature, take out grinding and namely obtain the potassium dopen Nano TiO that doping content is 4.5% 2photochemical catalyst.
Embodiment 20:
Present embodiment is as different from Example 19: sintering temperature is 650 ° of C, and other is identical with embodiment 19.
Embodiment 21:
Present embodiment is as different from Example 19: the potash added is 0.7926g, obtains the potassium dopen Nano TiO that doping content is 6.5% 2, other is identical with embodiment 19.
Embodiment 22:
Present embodiment is as different from Example 21: sintering temperature is 650 ° of C, and other is identical with embodiment 21.
Adopt potassium dopen Nano TiO prepared by the present invention 2under the ultraviolet light of 300 watts, all more than 98% is reached to its degradation rate during 10mg/L methyl orange solution degraded 20min, under 20 watts of visible rays, all more than 99% is reached to its degradation rate during 6mg/L activated dyeing wastewater degraded 30min.

Claims (5)

1. a preparation method for potassium doped nanometer titanium dioxide photocatalyst, is characterized in that, described preparation comprises following concrete steps:
(1) under room temperature and stirring, butyl titanate is slowly added drop-wise in absolute ethyl alcohol by the volume ratio being 1:3.5 ~ 3.7 by butyl titanate and absolute ethyl alcohol, the volume ratio being 1:3.0 ~ 3.3 by acetylacetone,2,4-pentanedione and butyl titanate adds acetylacetone,2,4-pentanedione, the volume ratio being 1:1.3 ~ 1.5 by triton x-100 and butyl titanate adds triton x-100, then add polyethylene glycol in the ratio of 0.05 ~ 0.06g polyethylene glycol/mL butyl titanate, continue stirring and obtain solution A;
(2) under room temperature and stirring, by the doping content of the molar percentage 4.5% ~ 6.5% of Ti element in K element and butyl titanate, potassium hydroxide or potassium nitrate or potash or potassium chloride or potassium sulfate are joined in redistilled water, adding by redistilled water and absolute ethyl alcohol is again the water prepared of 1:3 volume ratio and alcohol mixeding liquid, and be 2 ~ 3 with the salt acid for adjusting pH value of 1:1, stir to obtain solution B;
(3) solution B is slowly added drop-wise in solution A by the volume ratio being 1:3.2 ~ 3.4 by solution B and solution A under stirring, continues to stir to obtain yellowish vitreosol;
(4) colloidal sol at room temperature left standstill, after natural ageing to gel, put it into inherent 100 DEG C ~ 120 DEG C of baking oven and be dried to xerogel;
(5) xerogel is milled into powdery, puts in people's Muffle furnace, be warming up to 550 DEG C ~ 650 DEG C roasting 2.5 ~ 3.0h, naturally cool to room temperature, take out grinding and namely obtain potassium dopen Nano TiO 2photochemical catalyst.
2. preparation method according to claim 1, is characterized in that: in described step (1), mixing time is 2 hours.
3. preparation method according to claim 1, is characterized in that: in described step (2), mixing time is 0.2 hour.
4. preparation method according to claim 1, is characterized in that: in described step (3), mixing time is 2 hours.
5. preparation method according to claim 1, is characterized in that: in described step (5), by 5 DEG C/min temperature programming to 550 DEG C ~ 650 DEG C of roasting 2.5 ~ 3.0h.
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CN105664995B (en) * 2016-03-08 2018-06-01 济宁学院 A kind of multielement codoped nanaotitania catalysis material
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