CN106111101B - A kind of composite titanic acid barium photochemical catalyst and its preparation method and application - Google Patents
A kind of composite titanic acid barium photochemical catalyst 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 photochemical catalysts and its preparation method and application.The molecular formula of the composite titanic acid barium photochemical catalyst is Ba0.5M0.5TiO3, the M is Sr, Ca or Mg.Preparation method is as follows：Sr, Ca or Mg salt are weighed, titanium dioxide, barium hydroxide and water is added, in micro-wave diminishing pot, at pressure 0.5-1.5MPa, microwave hydrothermal reacts 10-40 minutes, and it is cooling, it washs, is centrifuged, it is dry, obtain target product.The present invention expands BaTiO3Visible light-responded range, reduce the compound of electrons and holes, to improve BaTiO3To the utilization rate of solar energy, its visible light catalysis activity is improved.For composite titanic acid barium photochemical catalyst of the invention under visible light action, photocatalysis effect is good, and the degradation rate in conjunction with radiation of visible light degradation organic pollutants is high.
Description
Technical field
The invention belongs to photochemical catalyst field, composite titanic acid barium photochemical catalyst more particularly to microwave-hydrothermal method preparation and
The application of its catalytic degradation organic pollutants under visible light.
Background technique
Barium titanate (BaTiO3) forbidden bandwidth and TiO2It is close, it is a kind of semiconductor material, there is chemical property stabilization, urge
Change the features such as activity is high, at low cost, nontoxic, thus can be used as good photochemical catalyst.It can not only make being converted into of luminous energy
Energy is learned, and the toxic organic pollutant of the various difficult for biological degradation in photochemical catalytic oxidation water body and air may be implemented, is degraded
Final product is CO2, H2O and other inorganic ions.
BaTiO3Ultraviolet light can be absorbed, electronics (e is generated-) and hole (h+), h+Aoxidize organic pollutant, e-Energy and O2
Reaction generates O2-, ultimately generate OH-Free radical makes organic pollutant oxygenolysis.However, BaTiO3Have as photochemical catalyst
Two big defects：First is that BaTiO3Forbidden bandwidth is 3.3eV, makes barium titanate that can only have response to ultraviolet light, and cannot be efficiently used
Visible light part in sunlight, sun light utilization efficiency are low.Second is that electronics (e-) and hole (h+) be easy compound, reduce catalysis
The photocatalysis efficiency of agent.
Water resource is the binding site of the mankind, resource and environment three digest journals, is the movable material base of all life, in society
There can be very important status in economic development.With the development and social progress of the mankind, people increasingly recognize profoundly
Fwaater resources protection is known to the importance of socio-economic development.Due to the quick stable development of China's dye industry, dyeing
Have become the discharge rich and influential family of industrial wastewater.According to incompletely statistics, the dyeing waste water that China is discharged daily is about 300~4,000,000 tons,
Annual emissions are 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.With the aggravation of water resources crisis, how rationally to have
Effect ground processing waste water, makes it turn waste into wealth, is the important subject of environmental protection and comprehensive energy utilization.
Summary of the invention
The purpose of the invention is to expand BaTiO3Visible light-responded range, reduce the compound of electrons and holes, from
And improve BaTiO3To the utilization rate of solar energy, its visible light catalysis activity is improved, therefore the present invention is to BaTiO3It is repaired on surface
Decorations provide one kind under visible light action, the good composite titanic acid barium photochemical catalyst of photocatalysis effect, and radiation of visible light is combined to drop
The method for solving organic pollutants.
The technical solution adopted by the present invention is that：A kind of composite titanic acid barium photochemical catalyst, the composite titanic acid barium photocatalysis
The molecular formula of agent is Ba0.5M0.5TiO3, the M is Sr, Ca or Mg.
The preparation method of above-mentioned composite titanic acid barium photochemical catalyst, method are as follows：Sr, Ca or Mg salt are weighed, dioxy is added
Change titanium, barium hydroxide and water, in micro-wave diminishing pot, at pressure 0.5-1.5MPa, microwave hydrothermal reacts 10-40 minutes, cold
But, it washs, is centrifuged, it is dry, obtain target product.
The preparation method of above-mentioned composite titanic acid barium photochemical catalyst, Sr, Ca or Mg salt are strontium hydroxide, hydroxide
Calcium or magnesium hydroxide.
The application in degradable organic pollutant under visible light of above-mentioned composite titanic acid barium photochemical catalyst.Method is as follows：In
In waste water containing organic pollutant, composite titanic acid barium photochemical catalyst is added, degrades under visible light.
Preferably, above-mentioned application, the concentration for adjusting organic pollutant is 10~25.0mg/L；Composite titanic acid barium photocatalysis
0.5~2.5g/L of agent usage amount；Visible power is 105~315W, and light application time is 0~14.0h.
It is furthermore preferred that above-mentioned application, the concentration for adjusting organic pollutant is 10.0mg/L；Composite titanic acid barium photochemical catalyst
Usage amount 2.0g/L；Visible power is 315W, light application time 4h.
The beneficial effects of the invention are as follows：
1. the compound titanate photochemical catalyst prepared using method of the invention, the compound BaTiO of Mg, Ca and Sr3Do not change
Become its lattice structure.BaTiO3Diffraction maximum also without there is abnormal phenomenon, therefore Mg, Ca and Sr it is compound to BaTiO3Crystalline substance
The influence very little of type structure.Ba0.5Mg0.5TiO3、Ba0.5Ca0.5TiO3And Ba0.5Sr0.5TiO3The partial size of three kinds of catalyst is respectively
16.07,13.64 and 12.58nm.Composite titanic acid barium photochemical catalyst prepared by the present invention has preferable photocatalysis performance.
2. the composite titanic acid barium photochemical catalyst prepared using method of the invention, Ba0.5Ca0.5TiO3, Ba0.5Mg0.5TiO3With
Ba0.5Sr0.5TiO3Dispersibility it is all relatively good, shape is spherical shape, and the size of particle is more uniform.
3. the composite titanic acid barium photochemical catalyst prepared using method of the invention, expands BaTiO3Visible light-responded model
It encloses, reduces the compound of electrons and holes, to improve BaTiO3To the utilization rate of solar energy, under visible light, to organic dirt
The degradation rate of object is contaminated up to 100%.
Detailed description of the invention
Fig. 1 a is Ba prepared by embodiment 10.5Mg0.5TiO3The XRD diagram of photochemical catalyst.
Fig. 1 b is Ba prepared by embodiment 10.5Ca0.5TiO3The XRD diagram of photochemical catalyst.
Fig. 1 c is Ba prepared by embodiment 10.5Sr0.5TiO3The XRD diagram of photochemical catalyst.
Fig. 2 is the UV-vis spectrum of azo-fuchsine solution under different condition.
Specific embodiment
The preparation of 1 composite titanic acid barium photochemical catalyst of embodiment
(1) composite titanic acid barium Ba0.5Mg0.5TiO3Photochemical catalyst
Accurately claim to obtain 0.2304g magnesium hydroxide, 0.6311g titanium dioxide and 1.2461g barium hydroxide octahydrate, weighing
Drug afterwards is put into micro-wave diminishing pot, adds 14.4mL distilled water, guarantees Ba:Sr:Ti molar ratio is 0.5:0.5:1.Then it seals
Micro-wave diminishing pot is closed, is placed in microwave synthesizer, guarantees that pressure is under 1.5MPa, microwave hydrothermal reacts 30 minutes.Natural cooling
Amorphous state catalyst to after room temperature, with the multiple washing precipitate of distilled water, in scavenger precipitation object.Centrifugation is then placed in set
It is standby, it is run under medium speed.Supernatant is removed after centrifugation, surplus materials is placed in baking oven drying 12 hours at 105 DEG C, finally
Obtain Ba0.5Mg0.5TiO3Nanoparticle.
(2) composite titanic acid barium Ba0.5Ca0.5TiO3Photochemical catalyst
0.2927g calcium hydroxide, 0.6311g titanium dioxide and 1.2461g barium hydroxide octahydrate are accurately weighed, weighing
Drug afterwards is put into micro-wave diminishing pot, adds 14.4mL distilled water, guarantees Ba:Sr:Ti molar ratio is 0.5:0.5:1.Then it seals
Micro-wave diminishing pot is closed, is placed in microwave synthesizer, guarantees that pressure is under 1.5MPa, microwave hydrothermal reacts 30 minutes.Natural cooling
Amorphous state catalyst to after room temperature, with the multiple washing precipitate of distilled water, in scavenger precipitation object.Centrifugation is then placed in set
It is standby, it is run under medium speed.Supernatant is removed after centrifugation, residue is placed in drying 12 hours at 105 DEG C of baking oven, final to obtain
Ba0.5Ca0.5TiO3Nanoparticle.
(3) composite titanic acid barium Ba0.5Sr0.5TiO3Photochemical catalyst
Eight hydronium(ion) strontium oxide strontia of 1.0498g, 0.6311g titanium dioxide and 1.2461g barium hydroxide octahydrate are weighed, title
Drug after amount is put into micro-wave diminishing pot, adds 13.86mL distilled water, guarantees Ba:Sr:Ti molar ratio is 0.5:0.5:1.Then
Micro-wave diminishing pot is closed, is placed in microwave synthesizer, under conditions of guaranteeing that pressure is 1.5MPa, microwave hydrothermal reacts 30 minutes.
Micro-wave diminishing pot is taken out, the amorphous state after naturally cooling to room temperature, with the multiple washing precipitate of distilled water, in scavenger precipitation object
Catalyst.It is then placed in centrifugation apparatus, is run under medium speed.Supernatant is removed after centrifugation, surplus materials is placed in baking oven and exists
It is 12 hours dry under conditions of 105 DEG C, finally obtain Ba0.5Sr0.5TiO3Nanoparticle.
The compound titanate photochemical catalyst prepared using method of the invention, from the Ba of Fig. 1 a- Fig. 1 c0.5Mg0.5TiO3,
Ba0.5Ca0.5TiO3And Ba0.5Sr0.5TiO3XRD diagram as it can be seen that do not occur other diffraction maximums in XRD diagram, urge for three kinds as seen from the figure
Agent is perovskite structure.This explanation passes through the compound BaTiO of Mg, Ca and Sr3Its lattice structure is not changed.BaTiO3Spread out
Peak is penetrated also without there is abnormal phenomenon, therefore Mg, Ca and Sr are compound to BaTiO3Crystalline structure influence very little.
Ba0.5Ca0.5TiO3, Ba0.5Mg0.5TiO3And Ba0.5Sr0.5TiO3Dispersed preferable, shape is spherical shape, the ruler of particle
Very little size is more uniform.Ba is calculated0.5Mg0.5TiO3、Ba0.5Ca0.5TiO3And Ba0.5Sr0.5TiO3The partial size of three kinds of catalyst point
It Wei not 16.07,13.64 and 12.58nm.It follows that the size order of particle is Ba0.5Mg0.5TiO3>Ba0.5Ca0.5TiO3>
Ba0.5Sr0.5TiO3, Ba0.5Sr0.5TiO3The size of particle is minimum, Ba0.5Mg0.5TiO3Particle size it is maximum, this three kinds of explanation
Ba in catalyst0.5Sr0.5TiO3Partial size is minimum and catalytic activity highest.Illustrate composite titanic acid barium photocatalysis prepared by the present invention
Agent has preferable photocatalysis performance.
Application of the composite titanic acid barium photochemical catalyst of the different synthesis condition preparations of embodiment 2 in degradable organic pollutant
It is that target organic pollutant does degradation experiment with rhodamine B (Rh B).
Biodegrading process：Adjusting rhodamine B solution concentration is 10mg/L, catalyst amounts 2g/L, and illumination power is
315W, illumination 4 hours.
(1) influence of the composite titanic acid barium photochemical catalyst synthesized under different pressures to degradation rate
The synthetic method of composite titanic acid barium photochemical catalyst：Method is the same as embodiment 1, difference：Synthesis pressure is respectively
0.5MPa, 1.0MPa, 1.5MPa.Degradation rate is shown in Table 1.
The influence (554nm) that the different synthesis pressures of table 1 degrade to rhodamine B solution
Table 1 shows the influence that different microwave synthesis pressures degrade to rhodamine B solution.It is found that being pressed as microwave synthesizes
The increase of power, the degradation effect of rhodamine B solution is become better and better under three kinds of catalyst.The results show that microwave attenuation materials pressure
The degradation effect of rhodamine B is best when for 1.5MPa.Therefore, the present invention synthesizes pressure using 1.5MPa as optimal microwave
Power.
(2) influence of the composite titanic acid barium photochemical catalyst synthesized under different generated times to degradation rate
The synthetic method of composite titanic acid barium photochemical catalyst：Method is the same as embodiment 1, difference：Generated time is respectively：
10min, 20min, 30min, 40min.Degradation rate is shown in Table 2.
The influence (554nm) that the different generated times of table 2 degrade to rhodamine B
Table 2 shows that, as generated time changes to 40min from 10min, the degradation of rhodamine B takes the lead in reducing after increasing.When
When generated time is 30min, the degradation effect of rhodamine B is best.At this moment, using Ba0.5Mg0.5TiO3、Ba0.5Ca0.5TiO3With
Ba0.5Sr0.5TiO3The ascending sequence of degradation rate：Ba0.5Mg0.5TiO3<Ba0.5Ca0.5TiO3<Ba0.5Sr0.5TiO3.This table
Bright, the microwave activity of the extension of generated time, three catalyst also increases.But the time is further increased, the crystalline substance of three kinds of catalyst
Volume defect can gradually become smaller, thus the activity of catalyst can gradually decrease.Comparatively, Ba0.5Sr0.5TiO3Photocatalytic activity
Highest.Therefore, it is best generated time that the present invention, which chooses 30min,.
Application of the composite titanic acid barium photochemical catalyst in degradable organic pollutant under the different degradation conditions of embodiment 3
It is that target organic pollutant does degradation experiment with rhodamine B (Rh B).
Composite titanic acid barium photochemical catalyst：The three kinds of photochemical catalysts prepared using embodiment 1.
Biodegrading process is as follows：Adjusting rhodamine B solution concentration is 10mg/L, catalyst amounts 2g/L, illumination power
For 315W, illumination 4 hours.
(1) influence of the different illumination conditions to degradation rate
The composite titanic acid barium photochemical catalyst prepared using embodiment 1, is degraded, degradation rate is such as under different illumination conditions
Shown in table 3 and Fig. 2.
Table 3
Seen from table 3, compared with stoste, after separately visible light irradiation rhodamine B solution 4h, only faint reduction, degradation
Rate is 2.23%.And when visible light is in conjunction with catalyst, Ba0.5Mg0.5TiO3、Ba0.5Ca0.5TiO3And Ba0.5Sr0.5TiO3Table
Reveal very high catalytic activity.The sequence of degradation rate from big to small is：Ba0.5Sr0.5TiO3>Ba0.5Ca0.5TiO3>
Ba0.5Mg0.5TiO3.This explanation is under composite titanic acid barium combination radiation of visible light, and rhodamine B can significantly be degraded, and sieve
Phenyl ring, naphthalene nucleus and azo bond in red bright B is by a degree of destruction.
By Fig. 2 ultraviolet-visible (UV-vis) spectrum it is found that rhodamine B solution is there are three main absorption peak, 554nm,
At 353nm and 252nm, azo bond, naphthalene oxygen ring and the phenyl ring in rhodamine B molecule are respectively corresponded.Separately visible light irradiates sieve
After red bright B solution 4h, only faint reduction；Catalyst Ba is used alone in (c-e) display in Fig. 20.5Mg0.5TiO3、
Ba0.5Ca0.5TiO3And Ba0.5Sr0.5TiO3When, the absorbance decrease to some degree of rhodamine B, this three kinds of catalyst of explanation
There is certain suction-operated to rhodamine B.Suction-operated size is：Ba0.5Sr0.5TiO3>Ba0.5Ca0.5TiO3>
Ba0.5Mg0.5TiO3.(f-h) is shown under three kinds of catalyst and visible light cooperation condition in Fig. 2, the fast prompt drop of rhodamine B absorption peak
It is low, and tri- absorption peaks of 554nm, 353nm and 252nm simultaneously decline, show azo bond in rhodamine B molecule, naphthalene oxygen ring and
Phenyl ring is gradually degraded.The result shows that the strong and weak sequence of their photocatalytic activity is：Ba0.5Sr0.5TiO3>Ba0.5Ca0.5TiO3>
Ba0.5Mg0.5TiO3.Therefore, Ba0.5Sr0.5TiO3Nano-particle catalyst combination Visible Light Induced Photocatalytic dyestuff effect is best.
(2) influence of the different light application times to degradation rate
In biodegrading process, only change light application time, respectively：0,2,4,6,8,10h.Degradation rate is shown in Table 4.
The influence (554nm) that the different light application times of table 4 degrade to rhodamine B
In table 4, using the Ba of microwave synthesis 30min and 1.5MPa preparation0.5Mg0.5TiO3、Ba0.5Ca0.5TiO3With
Ba0.5Sr0.5TiO3For catalyst, under visible light illumination, to Luo Dan under catalyst amounts 2.0g/L, 315W irradiation power
Bright B solution is degraded.As can be seen that with the extension 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 sequence of degradation rate：Ba0.5Mg0.5TiO3<
Ba0.5Ca0.5TiO3<Ba0.5Sr0.5TiO3.Therefore, Ba0.5Sr0.5TiO3Catalytic activity highest.
(3) influence of the different illumination power to degradation rate
In biodegrading process, only change illumination power, respectively 105W, 210W, 315W, degradation rate is shown in Table 5.
Influence (554nm) of 5 visible power of table to degrading to rhodamine B
As shown in Table 5, power is bigger, and rhodamine B solution degradation rate is higher.Wherein with Ba0.5Sr0.5TiO3For catalyst
When, rhodamine B solution degradation rate always compares Ba0.5Ca0.5TiO3And Ba0.5Mg0.5TiO3Catalyst is high.Use Ba0.5Mg0.5TiO3、
Ba0.5Ca0.5TiO3And Ba0.5Sr0.5TiO3The ascending sequence of degradation rate：Ba0.5Mg0.5TiO3<Ba0.5Ca0.5TiO3<
Ba0.5Sr0.5TiO3.Therefore, Ba0.5Sr0.5TiO3Catalytic activity highest.
Application of the 4 composite titanic acid barium photochemical catalyst of embodiment in degradable organic pollutant
Composite titanic acid barium photochemical catalyst：The Ba prepared using embodiment 10.5Sr0.5TiO3Photochemical catalyst.
Biodegrading process is as follows：Adjusting organic pollutant solution concentration is 10mg/L, catalyst amounts 2g/L, illumination function
Rate is 315W.Organic pollutant is respectively neopelex (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.
6 Ba of table0.5Sr0.5TiO3In conjunction with the degradation efficiency of radiation of visible light different structure pollutant
Table 6 shows that, as the radiation of visible light time increases, the degradation rate of 5 kinds of pollutants is gradually increased.But since chemistry is tied
Structure is different, and degradation efficiency is also different.As illumination 4h, neopelex (SDBS) is completely degraded；Luo Dan when illumination 6h
Bright B (Rh B) is completely degraded；Bisphenol-A (BPA), phenol (Phenol) and diuron (Diuron) degradation rate point when illumination 14h
It Wei 100%, 70.23% and 81.40%.Degrading sequentially is from fast to slow：SDBS > Rh B > BPA > Diuron >
Phenol。
Claims (5)
1. a kind of preparation method of composite titanic acid titanate catalyst, it is characterised in that：Weigh strontium hydroxide, calcium hydroxide or hydroxide
Titanium dioxide, barium hydroxide and water is added in magnesium, in micro-wave diminishing pot, at pressure 0.5-1.5MPa, and microwave hydrothermal reaction
It is 10-40 minutes, cooling, it washs, centrifugation is dried to obtain target product, molecular formula Ba0.5M0.5TiO3, the M be Sr,
Ca or Mg.
2. the composite titanic acid titanate catalyst prepared according to the method for claim 1 is under visible light in degradable organic pollutant
Application.
3. application according to claim 2, it is characterised in that method is as follows：In the waste water containing organic pollutant, add
Enter composite titanic acid barium photochemical catalyst, degrades under visible light.
4. application according to claim 3, it is characterised in that：The concentration for adjusting organic pollutant is 10~25.0mg/L；
0.5~2.5g/L of composite titanic acid barium photochemical catalyst usage amount；Visible power is 105~315W, and light application time is 0~14.0h.
5. application according to claim 4, it is characterised in that：The concentration for adjusting organic pollutant is 10.0mg/L；It is compound
Barium titanate photocatalyst usage amount 2.0g/L；Visible power is 315W, light application time 4h.
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