CN106111101A - A kind of composite titanic acid barium photocatalyst and its preparation method and application - Google Patents
A kind of composite titanic acid barium photocatalyst and its preparation method and application Download PDFInfo
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Abstract
The present invention relates to a kind of composite titanic acid barium photocatalyst and its preparation method and application.The molecular formula of described composite titanic acid barium photocatalyst is Ba0.5M0.5TiO3, described M is Sr, Ca or Mg.Preparation method is as follows: weigh Sr, Ca or Mg salt, adds titanium dioxide, barium hydroxide and water, and in micro-wave diminishing pot, under pressure 0.5 1.5MPa, microwave hydrothermal reacts 10 40 minutes, cooling, and washing is centrifugal, is dried, obtains target product.The present invention expands BaTiO3Visible light-responded scope, reduce the compound of electronics and hole, thus improve BaTiO3Utilization rate to solar energy, improves its visible light catalysis activity.The composite titanic acid barium photocatalyst of the present invention is under visible ray effect, and photocatalysis effect is good, and the degradation rate in conjunction with radiation of visible light degraded organic pollutants is high.
Description
Technical field
The invention belongs to photocatalyst field, the composite titanic acid barium photocatalyst prepared more particularly to microwave-hydrothermal method and
The application of its catalytic degradation organic pollutants under visible light.
Background technology
Barium metatitanate. (BaTiO3) energy gap and TiO2Close, it is a kind of semi-conducting material, there is stable chemical nature, urge
Change activity height, low cost, the feature such as nontoxic, thus can be as good photocatalyst.It is possible not only to make being converted into of luminous energy
Learn energy, and the toxic organic pollutant of the various difficult for biological degradation in photochemical catalytic oxidation water body and air can be realized, degraded
End product is CO2, H2O and other inorganic ions.
BaTiO3Ultraviolet light can be absorbed, produce electronics (e-) and hole (h+), h+Organic pollution is made to aoxidize, e-Energy and O2
Reaction produces O2-, ultimately generate OH-Free radical, makes organic pollution oxidation Decomposition.But, BaTiO3Have as photocatalyst
Two big defects: one is, BaTiO3Energy gap is 3.3eV, makes Barium metatitanate. can only have response to ultraviolet light, and can not effectively utilize
Visible light part in sunlight, sunlight utilization rate is low.Two are, electronics (e-) and hole (h+) be easily combined, reduce catalysis
The photocatalysis efficiency of agent.
Water resource is the mankind, the binding site of resource and environment three digest journals, is the material base of all life activity, in society
Economic development can there is very important status.Along with development and the progress of society of the mankind, people the most profoundly recognize
Know to the fwaater resources protection importance to socio-economic development.Due to the quick stable development of China's dye industry, dyeing
Become the discharge rich and influential family of industrial wastewater.According to incompletely statistics, the dyeing waste water of China's discharge every day is about 300～4,000,000 tons,
Annual emissions is about 6.5 hundred million tons.Compared with developed country, the unit water consumption of China's textile printing and dyeing industry is the 1.5 of developed country
～2.0 times, unit total amount of pollutants discharged is 1.2～1.8 times of developed country.Along with the aggravation of water resources crisis, the most rationally have
Effect ground processes waste water so that it is turns waste into wealth, is the important subject of environmental conservation and comprehensive energy utilization.
Summary of the invention
The invention aims to expand BaTiO3Visible light-responded scope, reduce the compound of electronics and hole, from
And improve BaTiO3Utilization rate to solar energy, improves its visible light catalysis activity, and therefore the present invention is to BaTiO3Surface is repaiied
Decorations, it is provided that a kind of under visible ray effect, the composite titanic acid barium photocatalyst that photocatalysis effect is good, and combine radiation of visible light fall
The method solving organic pollutants.
The technical solution used in the present invention is: a kind of composite titanic acid barium photocatalyst, described composite titanic acid barium photocatalysis
The molecular formula of agent is Ba0.5M0.5TiO3, described M is Sr, Ca or Mg.
The preparation method of above-mentioned composite titanic acid barium photocatalyst, method is as follows: weigh Sr, Ca or Mg salt, adds dioxy
Changing titanium, barium hydroxide and water, in micro-wave diminishing pot, under pressure 0.5-1.5MPa, microwave hydrothermal reacts 10-40 minute, cold
But, washing, centrifugal, it is dried, obtains target product.
The preparation method of above-mentioned composite titanic acid barium photocatalyst, described Sr, Ca or Mg salt is Strontium hydrate., hydroxide
Calcium or magnesium hydroxide.
The above-mentioned application in composite titanic acid barium photocatalyst degradable organic pollutant under visible light.Method is as follows: in
In waste water containing organic pollution, add composite titanic acid barium photocatalyst, degrade under visible ray.
Preferably, above-mentioned application, the concentration of regulation organic pollution is 10～25.0mg/L；Composite titanic acid barium photocatalysis
Agent usage amount 0.5～2.5g/L；Visible power is 105～315W, and light application time is 0～14.0h.
It is furthermore preferred that above-mentioned application, the concentration of regulation organic pollution is 10.0mg/L；Composite titanic acid barium photocatalyst
Usage amount 2.0g/L；Visible power is 315W, and light application time is 4h.
The invention has the beneficial effects as follows:
1. using compound titanate photocatalyst prepared by the method for the present invention, Mg, Ca and Sr are combined BaTiO3Do not change
Become its lattice structure.BaTiO3Diffraction maximum abnormal phenomenon, therefore Mg the most do not occur, Ca and Sr compound to BaTiO3Crystalline substance
The impact of type structure is the least.Ba0.5Mg0.5TiO3、Ba0.5Ca0.5TiO3And Ba0.5Sr0.5TiO3The particle diameter of three kinds of catalyst is respectively
16.07,13.64 and 12.58nm.Composite titanic acid barium photocatalyst prepared by the present invention has preferable photocatalysis performance.
2. use composite titanic acid barium photocatalyst prepared by the method for the present invention, Ba0.5Ca0.5TiO3, Ba0.5Mg0.5TiO3With
Ba0.5Sr0.5TiO3Dispersibility relatively good, be shaped as spherical, the size of granule is more uniform.
3. the composite titanic acid barium photocatalyst using the method for the present invention to prepare, expands BaTiO3Visible light-responded model
Enclose, reduce the compound of electronics and hole, thus improve BaTiO3Utilization rate to solar energy, under visible light, to organic dirt
The degradation rate of dye thing is up to 100%.
Accompanying drawing explanation
Fig. 1 a is the Ba of embodiment 1 preparation0.5Mg0.5TiO3The XRD figure of photocatalyst.
Fig. 1 b is the Ba of embodiment 1 preparation0.5Ca0.5TiO3The XRD figure of photocatalyst.
Fig. 1 c is the Ba of embodiment 1 preparation0.5Sr0.5TiO3The XRD figure of photocatalyst.
Fig. 2 is the UV-vis spectrum of azo-fuchsine solution under different condition.
Detailed description of the invention
The preparation of embodiment 1 composite titanic acid barium photocatalyst
(1) composite titanic acid barium Ba0.5Mg0.5TiO3Photocatalyst
Accurately claim to obtain 0.2304g magnesium hydroxide, 0.6311g titanium dioxide and 1.2461g barium hydroxide octahydrate, weighing
After medicine put into micro-wave diminishing pot, add 14.4mL distilled water, it is ensured that Ba:Sr:Ti mol ratio is 0.5:0.5:1.Then seal
Closing micro-wave diminishing pot, be placed in microwave synthesizer, it is ensured that pressure is under 1.5MPa, microwave hydrothermal reacts 30 minutes.Natural cooling
After room temperature, with distilled water repeatedly washing precipitate, the amorphous state catalyst in scavenger precipitation thing.It is then placed in centrifugal setting
Standby, run under medium speed.After Li Xin remove supernatant, surplus materials be placed in baking oven at 105 DEG C be dried 12 hours, finally
Obtain Ba0.5Mg0.5TiO3Nanoparticle.
(2) composite titanic acid barium Ba0.5Ca0.5TiO3Photocatalyst
Accurately weigh 0.2927g calcium hydroxide, 0.6311g titanium dioxide and 1.2461g barium hydroxide octahydrate, weighing
After medicine put into micro-wave diminishing pot, add 14.4mL distilled water, it is ensured that Ba:Sr:Ti mol ratio is 0.5:0.5:1.Then seal
Closing micro-wave diminishing pot, be placed in microwave synthesizer, it is ensured that pressure is under 1.5MPa, microwave hydrothermal reacts 30 minutes.Natural cooling
After room temperature, with distilled water repeatedly washing precipitate, the amorphous state catalyst in scavenger precipitation thing.It is then placed in centrifugal setting
Standby, run under medium speed.Removing supernatant after Li Xin, residue is placed at 105 DEG C of baking oven and is dried 12 hours, final
Ba0.5Ca0.5TiO3Nanoparticle.
(3) composite titanic acid barium Ba0.5Sr0.5TiO3Photocatalyst
Weigh 1.0498g eight hydronium(ion) strontium oxide, 0.6311g titanium dioxide and 1.2461g barium hydroxide octahydrate, claiming
Micro-wave diminishing pot put into by medicine after amount, adds 13.86mL distilled water, it is ensured that Ba:Sr:Ti mol ratio is 0.5:0.5:1.Then
Closing micro-wave diminishing pot, be placed in microwave synthesizer, it is ensured that under conditions of pressure is 1.5MPa, microwave hydrothermal reacts 30 minutes.
Take out micro-wave diminishing pot, after naturally cooling to room temperature, with distilled water repeatedly washing precipitate, the amorphous state in scavenger precipitation thing
Catalyst.It is then placed in centrifugation apparatus, runs under medium speed.Removing supernatant after Li Xin, surplus materials is placed in baking oven and exists
It is dried 12 hours under conditions of 105 DEG C, finally obtains Ba0.5Sr0.5TiO3Nanoparticle.
Use compound titanate photocatalyst prepared by the method for the present invention, from the Ba of Fig. 1 a-Fig. 1 c0.5Mg0.5TiO3,
Ba0.5Ca0.5TiO3And Ba0.5Sr0.5TiO3XRD figure visible, XRD figure does not occur other diffraction maximums, urges for three kinds as seen from the figure
Agent is perovskite structure.This explanation is combined BaTiO by Mg, Ca and Sr3Do not change its lattice structure.BaTiO3Spread out
Penetrating peak and abnormal phenomenon the most do not occur, therefore Mg, Ca and Sr are compound to BaTiO3The impact of crystalline structure the least.
Ba0.5Ca0.5TiO3, Ba0.5Mg0.5TiO3And Ba0.5Sr0.5TiO3Dispersibility is preferable, is shaped as spherical, the chi of granule
Very little size is more uniform.Calculate Ba0.5Mg0.5TiO3、Ba0.5Ca0.5TiO3And Ba0.5Sr0.5TiO3The particle diameter of three kinds of catalyst divides
It is not 16.07,13.64 and 12.58nm.It follows that the size order of granule is Ba0.5Mg0.5TiO3>Ba0.5Ca0.5TiO3>
Ba0.5Sr0.5TiO3, Ba0.5Sr0.5TiO3The size of granule is minimum, Ba0.5Mg0.5TiO3Particle size maximum, this explanation three kinds
Ba in catalyst0.5Sr0.5TiO3Particle diameter minimum and to be catalyzed activity the highest.Composite titanic acid barium photocatalysis prepared by the present invention is described
Agent has preferable photocatalysis performance.
Composite titanic acid barium photocatalyst prepared by the different synthesis condition of embodiment 2 application in degradable organic pollutant
It is that target organic pollution does degradation experiment with rhodamine B (Rh B).
Biodegrading process: regulation rhodamine B solution concentration is 10mg/L, and catalyst amounts is 2g/L, and illumination power is
315W, illumination 4 hours.
(1) the composite titanic acid barium photocatalyst of the synthesis impact on degradation rate under different pressures
The synthetic method of composite titanic acid barium photocatalyst: method is with embodiment 1, difference: synthesis pressure is respectively
0.5MPa, 1.0MPa, 1.5MPa.Degradation rate is shown in Table 1.
The different synthesis pressure impact (554nm) on rhodamine B solution degradation of table 1
Table 1 shows the different microwave synthesis pressure impact on rhodamine B solution degradation.Understand, along with microwave synthesis pressure
The increase of power, under three kinds of catalyst, the degradation effect of rhodamine B solution is become better and better.Result shows, microwave attenuation materials pressure
It is best for the degradation effect of rhodamine B during 1.5MPa.Therefore, the present invention is using 1.5MPa as optimal microwave synthesis pressure
Power.
(2) the composite titanic acid barium photocatalyst of the synthesis impact on degradation rate under different generated times
The synthetic method of composite titanic acid barium photocatalyst: method is with embodiment 1, difference: generated time is respectively as follows:
10min, 20min, 30min, 40min.Degradation rate is shown in Table 2.
The impact (554nm) that rhodamine B is degraded by the different generated time of table 2
Table 2 shows, along with generated time changes to 40min from 10min, the degraded of rhodamine B reduces after taking the lead in increasing.When
When generated time is 30min, the degradation effect of rhodamine B is best.At this moment, Ba is used0.5Mg0.5TiO3、Ba0.5Ca0.5TiO3With
Ba0.5Sr0.5TiO3The ascending order of degradation rate: Ba0.5Mg0.5TiO3<Ba0.5Ca0.5TiO3<Ba0.5Sr0.5TiO3.This table
Bright, the prolongation of generated time, the microwave activity of three catalyst also increases.But increase the time further, the crystalline substance of three kinds of catalyst
Volume defect can taper into, thus the activity of catalyst can be gradually lowered.Comparatively, Ba0.5Sr0.5TiO3Photocatalytic activity
The highest.Therefore, the present invention chooses 30min is optimal generated time.
Composite titanic acid barium photocatalyst application in degradable organic pollutant under the different degradation condition of embodiment 3
It is that target organic pollution does degradation experiment with rhodamine B (Rh B).
Composite titanic acid barium photocatalyst: use three kinds of photocatalysts of embodiment 1 preparation.
Biodegrading process is as follows: regulation rhodamine B solution concentration is 10mg/L, and catalyst amounts is 2g/L, illumination power
For 315W, illumination 4 hours.
(1) different illumination conditions impact on degradation rate
Using the composite titanic acid barium photocatalyst of embodiment 1 preparation, degrade under different illumination conditions, degradation rate is such as
Shown in table 3 and Fig. 2.
Table 3
From table 3, compared with stock solution, after separately visible light irradiates rhodamine B solution 4h, the faintest reduction, degraded
Rate is 2.23%.And when visible ray is combined with catalyst, Ba0.5Mg0.5TiO3、Ba0.5Ca0.5TiO3And Ba0.5Sr0.5TiO3Table
Reveal the highest catalysis activity.Degradation rate order from big to small is: Ba0.5Sr0.5TiO3>Ba0.5Ca0.5TiO3>
Ba0.5Mg0.5TiO3.This explanation is under composite titanic acid barium combines radiation of visible light, and rhodamine B can significantly be degraded, and sieve
Phenyl ring, naphthalene nucleus and azo bond in red bright B are all by a certain degree of destruction.
From Fig. 2 ultraviolet-visible (UV-vis) spectrum, rhodamine B solution has three main absworption peaks, 554nm,
At 353nm and 252nm, correspond to the azo bond in rhodamine B molecule, naphthalene oxygen ring and phenyl ring respectively.Separately visible light irradiates sieve
After red bright B solution 4h, the faintest reduction；In Fig. 2, (c e) display is used alone catalyst Ba0.5Mg0.5TiO3、
Ba0.5Ca0.5TiO3And Ba0.5Sr0.5TiO3Time, the absorbance decrease to some degree of rhodamine B, this illustrates three kinds of catalyst
Rhodamine B is had certain adsorption.Adsorption size is: Ba0.5Sr0.5TiO3>Ba0.5Ca0.5TiO3>
Ba0.5Mg0.5TiO3.Under in Fig. 2, (f h) shows three kinds of catalyst and visible ray cooperation condition, the fast prompt drop of rhodamine B absworption peak
Low, and tri-absworption peaks of 554nm, 353nm and 252nm decline simultaneously, show the azo bond in rhodamine B molecule, naphthalene oxygen ring and
Phenyl ring is gradually degraded.Result shows, their photocatalytic activity power order is: Ba0.5Sr0.5TiO3>Ba0.5Ca0.5TiO3>
Ba0.5Mg0.5TiO3.Therefore, Ba0.5Sr0.5TiO3It is best that nano-particle catalyst combines Visible Light Induced Photocatalytic dyestuff effect.
(2) the different light application time impacts on degradation rate
In biodegrading process, only change light application time, be respectively as follows: 0,2,4,6,8,10h.Degradation rate is shown in Table 4.
The impact (554nm) that rhodamine B is degraded by the different light application time of table 4
In table 4, with the Ba using microwave synthesis 30min and 1.5MPa to prepare0.5Mg0.5TiO3、Ba0.5Ca0.5TiO3With
Ba0.5Sr0.5TiO3For catalyst, under visible light illumination, catalyst amounts is to Luo Dan under 2.0g/L, 315W irradiation power
Bright B solution is degraded.It can be seen that along with the prolongation of light irradiation time, the degradation rate of rhodamine B solution is also gradually increased.
Use Ba0.5Mg0.5TiO3、Ba0.5Ca0.5TiO3And Ba0.5Sr0.5TiO3The ascending order of degradation rate: Ba0.5Mg0.5TiO3<
Ba0.5Ca0.5TiO3<Ba0.5Sr0.5TiO3.Therefore, Ba0.5Sr0.5TiO3Catalysis activity is the highest.
(3) the different illumination power impacts on degradation rate
In biodegrading process, only changing illumination power, respectively 105W, 210W, 315W, degradation rate is shown in Table 5.
The impact (554nm) on rhodamine B is degraded of table 5 visible power
As shown in Table 5, power is the biggest, and rhodamine B solution degradation rate is the highest.Wherein with Ba0.5Sr0.5TiO3For catalyst
Time, rhodamine B solution degradation rate is always than Ba0.5Ca0.5TiO3And Ba0.5Mg0.5TiO3Catalyst is high.Use Ba0.5Mg0.5TiO3、
Ba0.5Ca0.5TiO3And Ba0.5Sr0.5TiO3The ascending order of degradation rate: Ba0.5Mg0.5TiO3<Ba0.5Ca0.5TiO3<
Ba0.5Sr0.5TiO3.Therefore, Ba0.5Sr0.5TiO3Catalysis activity is the highest.
The application in degradable organic pollutant of the embodiment 4 composite titanic acid barium photocatalyst
Composite titanic acid barium photocatalyst: use the Ba of embodiment 1 preparation0.5Sr0.5TiO3Photocatalyst.
Biodegrading process is as follows: regulation organic pollutant solution concentration is 10mg/L, and catalyst amounts is 2g/L, illumination merit
Rate is 315W.Organic pollution is respectively dodecylbenzene sodium sulfonate (SDBS), rhodamine B (Rh B), bisphenol-A (BPA), enemy's grass
Grand (Diuron), phenol (Phenol), light application time is respectively 0h, 2h, 4h, 6h, 8h, 10h, 12h, 14h, and degradation rate is shown in Table 6.
Table 6 Ba0.5Sr0.5TiO3Degradation efficiency in conjunction with radiation of visible light different structure pollutant
Table 6 shows, along with the radiation of visible light time increases, the degradation rate of 5 kinds of pollutant is gradually increased.But owing to chemistry is tied
Structure is different, and degradation efficiency is the most different.As illumination 4h, dodecylbenzene sodium sulfonate (SDBS) is completely degraded；Luo Dan during illumination 6h
Bright B (Rh B) is completely degraded；During illumination 14h, bisphenol-A (BPA), phenol (Phenol) and diuron (Diuron) degradation rate divide
It is not 100%, 70.23% and 81.40%.Degraded order from fast to slow is: SDBS ＞ Rh B ＞ BPA ＞ Diuron ＞
Phenol。
Claims (7)
1. a composite titanic acid barium photocatalyst, it is characterised in that the molecular formula of described composite titanic acid barium photocatalyst is
Ba0.5M0.5TiO3, described M is Sr, Ca or Mg.
2. the preparation method of the composite titanic acid barium photocatalyst described in claim 1, it is characterised in that method is as follows: weigh Sr,
Ca or Mg salt, adds titanium dioxide, barium hydroxide and water, in micro-wave diminishing pot, under pressure 0.5-1.5MPa, microwave hydrothermal
React 10-40 minute, cooling, washing, centrifugal, it is dried, obtains target product.
The preparation method of composite titanic acid barium photocatalyst the most according to claim 2, it is characterised in that: described Sr, Ca
Or Mg salt is Strontium hydrate., calcium hydroxide or magnesium hydroxide.
4. the application in the composite titanic acid barium photocatalyst degradable organic pollutant under visible light described in claim 1.
Application the most according to claim 4, it is characterised in that method is as follows: in the waste water containing organic pollution, adds
Enter composite titanic acid barium photocatalyst, degrade under visible ray.
Application the most according to claim 5, it is characterised in that: the concentration of regulation organic pollution is 10～25.0mg/L；
Composite titanic acid barium photocatalyst usage amount 0.5～2.5g/L；Visible power is 105～315W, and light application time is 0～14.0h.
Application the most according to claim 6, it is characterised in that: the concentration of regulation organic pollution is 10.0mg/L；Compound
Barium titanate photocatalyst usage amount 2.0g/L；Visible power is 315W, and light application time is 4h.
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| CN106721879A (en) * | 2016-12-05 | 2017-05-31 | 南京悠谷知识产权服务有限公司 | One kind purification preservation device |
| CN106807400A (en) * | 2017-03-13 | 2017-06-09 | 辽宁大学 | A kind of compound bismuth ferrite photocatalyst and its preparation method and application |
| CN106964338A (en) * | 2017-03-28 | 2017-07-21 | 辽宁大学 | A kind of WO3/ titanate composite photocatalyst and its preparation method and application |
| CN110734086A (en) * | 2019-11-19 | 2020-01-31 | 湖南博深实业集团有限公司 | Preparation method of titanate based on electronic industry |
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| CN110734086A (en) * | 2019-11-19 | 2020-01-31 | 湖南博深实业集团有限公司 | Preparation method of titanate based on electronic industry |
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