CN105214637B - A kind of metatitanic acid cesium silicate photochemical catalyst and its preparation method and application - Google Patents
A kind of metatitanic acid cesium silicate photochemical catalyst and its preparation method and application Download PDFInfo
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Abstract
The invention discloses a kind of metatitanic acid cesium silicate photochemical catalyst and its preparation method and application, which is CsSi2TiO6.5Its pattern is irregular particle shape or form of spherical particles, and it can be prepared using high temperature solid-state method, sol-gel method, production cost is low, equipment requirement is simple, and the metatitanic acid cesium silicate photochemical catalyst good dispersion of preparation, uniform granularity, chemical stability are good, have very strong light absorption, has the function of decomposing harmful chemical under the irradiation of ultraviolet light, and repetition stability is good, has potential applications well prospect.
Description
Technical field
The present invention relates to one kind, and ultraviolet light photocatalysis material, preparation method and application more particularly to a kind of titanium may be implemented
Sour cesium silicate photochemical catalyst and its preparation method and application, belongs to inorganic field of photocatalytic material.
Background technique
Currently, science and technology economical increasingly prosperity, the mankind have enjoyed comfortable life, but product with the development of human society
The bitter pill that living environment constantly deteriorates is tasted, the deterioration of ecological environment increasingly restricts the sustainable development of future society.?
In various environmental pollutions, most generally, it is main and influence it is maximum be chemical contamination.Thus, it efficiently controls and administers and is various
Chemical pollutant is in comprehensive environmental improvement to the destruction for constituting human survival most basic water resource, soil and atmospheric environment
Emphasis, exploitation can be the key that environmental protection the innoxious practical technique of various chemical pollutants.Due to low efficiency, pollutant
Cannot be thoroughly innoxious, it is also easy to produce secondary pollution；It is only capable of handling specific pollutant；Or energy consumption is high, is not suitable for large-scale promotion
Etc. drawback presence, thus, exploitation efficiently, low energy consumption, chemical pollutant applied widely and having deep oxidation ability
Clearance technique is always the target that environmental protection technology is pursued.Photocatalysis technology is exactly one gradually to grow up from the 1970s
The emerging environmental protection technology of door.
Fujishima in 1972 and Honda discovery is in irradiated TiO2On can continue occur water redox it is anti-
It answers, from that point on to the numerous studies of semiconductor light-catalyst.Light-catalyzed reaction is to absorb photon by semiconductor particle to generate
What electron-hole caused.After inorganic semiconductor is by the photon irradiation for being greater than forbidden bandwidth energy, electronics is transitted to from valence band
Empty conduction band, forms photohole in valence band, forms light induced electron in conduction band, electronics has reproducibility, and hole has oxygen
The property changed, and organic pollutant is finally decomposed to CO2And H2The innocuous substances such as O.
In many metal oxide semiconductors, TiO2It is the most of research, but its forbidden bandwidth is 3.2 electron volts
Spy, corresponding light wave absorbing wavelength are 387.5 nanometers, and light absorption is only limitted to ultra-violet (UV) band, TiO2The photoproduction generated after light irradiates
Electronics is easy to be again compound with hole, or is captured and lose activity by metastable state surface.It therefore can be by studying novel nothing
Machine photochemical catalyst improves photocatalysis effect.
In the prior art, patent CN103170323A reports titanate photocatalyst A2TiO4And preparation method thereof, simultaneously
Patent CN103599772A reports a kind of titanate nanotube composite photocatalyst and its preparation method and application, obtains one
Tie up the CdS/ titanate nanotube composite photo-catalyst of tubular structure.On these report bases about titanate photocatalyst
On, we have studied a kind of novel metatitanic acid cesium silicate photochemical catalyst CsSi2TiO6.5, the compound is with excellent ultraviolet light
Responsible photocatalytic performance, preparation method and application are not reported so far.
Summary of the invention
For above-mentioned existing technical problem, the present invention provides that a kind of preparation process is simple, and production cost is low, while can be with
Realize the metatitanic acid cesium silicate photochemical catalyst and its preparation method and application of ultraviolet light photocatalysis.
To achieve the above object, the present invention provides a kind of metatitanic acid cesium silicate photochemical catalyst, chemical formula CsSi2TiO6.5,
Pattern is irregular particle shape or form of spherical particles.
The present invention provides a kind of preparation method of above-mentioned metatitanic acid cesium silicate photochemical catalyst again, using high temperature solid-state method, including
Following specific steps:
(1) chemical formula CsSi is pressed2TiO6.5The stoichiometric ratio of middle each element is weighed respectively containing cesium ion Cs+Chemical combination
Object contains silicon ion Si4+Compound, contain titanium ion Ti4+Compound, grind and be uniformly mixed；
(2) by precalcining 1~2 time in air atmosphere of step (1) gains, calcination temperature is 200~600 DEG C, calcining
Time is 2~10 hours；
(3) it by step (2) gains natural cooling, grinds and after mixing, then calcined in air atmosphere, calcining is warm
Degree is 600~900 DEG C, and calcination time is 2~15 hours；
(4) by step (3) gains natural cooling, metatitanic acid cesium silicate material C sSi is obtained2TiO6.5。
Further, the Cs containing cesium ion+Compound be cesium oxide, cesium carbonate, caesium bicarbonate, one in cesium nitrate
Kind；The Si containing silicon ion4+Compound be one of silica and silicic acid；Described contains titanium ion Ti4+Change
Conjunction object is titanium dioxide.
Further, the precalcining temperature of step (2) is 300~600 DEG C, and calcination time is 3~10 hours；Step (3)
Calcination temperature be 600~850 DEG C, calcination time be 3~12 hours.
The present invention provides a kind of preparation method of above-mentioned metatitanic acid cesium silicate photochemical catalyst again, using sol-gel method, including
Following specific steps:
(A) chemical formula CsSi is pressed2TiO6.5The stoichiometric ratio of middle each element is weighed respectively containing cesium ion Cs+Chemical combination
Object contains silicon ion Si4+Compound, contain titanium ion Ti4+Compound；Cesium ion Cs will be contained first+Compound it is molten
Solution obtains clear solution, then 0.5~2.0 times of addition by metal cation mole amount in deionized water or dilute nitric acid solution
Complexing agent citric acid or oxalic acid；Secondly it will contain silicon ion Si4+Compound dilute nitric acid dissolution, while dehydrated alcohol is added, and
It is diluted with deionized water；Titanium ion Ti will be contained again4+Compound be added glacial acetic acid solution, in 50~100 DEG C of temperature
Under the conditions of heating stirring, until complete hydrolysis；Finally obtain the mixed liquor of each raw material；
(B) each raw material mixed liquor for obtaining step (A) is slowly mixed together, and after continuing stirring 1~2 hour, is stood, drying,
Obtain fluffy presoma；
(C) precursors powder that step (B) obtains is placed in crucible, prior to calcining 2 in air atmosphere in Muffle furnace
~3 times, calcination temperature is 200~650 DEG C, calcination time 2~13 hours, then naturally cools to room temperature, obtains metatitanic acid silicic acid
Caesium material C sSi2TiO6.5。
Further, the Cs containing cesium ion+Compound be cesium oxide, cesium carbonate, caesium bicarbonate, one in cesium nitrate
Kind；The Si containing silicon ion4+Compound be ethyl orthosilicate；Described contains titanium ion Ti4+Compound be metatitanic acid four
One of butyl ester and tetraisopropyl titanate.
Further, the calcination temperature of step (C) is 300~600 DEG C, and calcination time is 3~12 hours.
A kind of application the present invention also provides above-mentioned metatitanic acid cesium silicate photochemical catalyst as inorganic catalysis material.
Compared with prior art, the metatitanic acid cesium silicate photochemical catalyst CsSi of technical solution of the present invention preparation2TiO6.5No
Ultraviolet light photocatalysis effect only may be implemented, be also equipped with following advantage:
1, the present invention prepares metatitanic acid cesium silicate photochemical catalyst CsSi2TiO6.5Production method be to calcine in air atmosphere
It being made, firing temperature is lower, and preparation process is simple, and it is easily operated, it is potential catalysis material.
2, metatitanic acid cesium silicate photochemical catalyst CsSi prepared by the present invention2TiO6.5Energy band band gap is relatively narrow, in ultraviolet light
Under, the photochemical catalyst can high efficiency photocatalysis degradation of methylene blue, have good photocatalytic activity.
3, the present invention prepares metatitanic acid cesium silicate photochemical catalyst CsSi2TiO6.5To prepare raw material sources abundant, it is cheap,
And low energy consumption, environmentally friendly, the metatitanic acid cesium silicate properties of catalyst of synthesis is stablized.
Detailed description of the invention
Fig. 1 is that the embodiment of the present invention 1 prepares sample CsSi2TiO6.5X-ray powder diffraction pattern；
Fig. 2 is that the embodiment of the present invention 1 prepares sample CsSi2TiO6.5SEM figure；
Fig. 3 is that the embodiment of the present invention 1 prepares sample CsSi2TiO6.5Ultraviolet-visible diffuse reflectance spectrum figure；
Fig. 4 is that the embodiment of the present invention 1 prepares sample CsSi2TiO6.5To organic dyestuff under ultraviolet light difference light application time
The degradation curve figure of methylene blue；
Fig. 5 is that the embodiment of the present invention 1 prepares sample CsSi2TiO6.5The kinetic curve of degradating organic dye methylene blue
Figure；
Fig. 6 is that the embodiment of the present invention 5 prepares sample CsSi2TiO6.5X-ray powder diffraction pattern；
Fig. 7 is that the embodiment of the present invention 5 prepares sample CsSi2TiO6.5SEM figure；
Fig. 8 is that the embodiment of the present invention 5 prepares sample CsSi2TiO6.5Ultraviolet-visible diffuse reflectance spectrum figure；
Fig. 9 is that the embodiment of the present invention 5 prepares sample CsSi2TiO6.5To organic dyestuff under ultraviolet light difference light application time
The degradation curve figure of methylene blue；
Figure 10 is that the embodiment of the present invention 5 prepares sample CsSi2TiO6.5The kinetic curve of degradating organic dye methylene blue
Figure.
Specific embodiment
The invention will be further described with reference to the accompanying drawings and examples.
Metatitanic acid cesium silicate photochemical catalyst chemical formula of the present invention is CsSi2TiO6.5, solid phase method, sol-gel method can be used
Preparation, specific implementation method are as follows.
Embodiment 1:
CsSi is prepared using high temperature solid-state method2TiO6.5, i.e., using the various oxides or carbonate as raw material according to target
Constitutional chemistry metering ratio is mixed, then is synthesized in air atmosphere under normal pressure.
Firstly, according to chemical formula CsSi2TiO6.5, cesium oxide Cs is weighed respectively2O:1.41 grams, silica SiO2: 1.2
Gram, titanium dioxide TiO2: it 0.8 gram, grinds and is uniformly mixed in the agate mortar, select air atmosphere to calcine for the first time, temperature
It is 300 DEG C, calcination time is 3 hours, is then cooled to room temperature, takes out sample.Then, preceding step sample is fully ground mixing again
Uniformly, it is calcined in air atmosphere, calcination temperature is 600 DEG C, and calcination time is 10 hours, is cooled to room temperature, and sample is taken out.Most
Afterwards, it is placed in Muffle furnace in air and calcines after preceding step sample being fully ground, calcination temperature is 850 DEG C, and calcination time is 12 small
When, then it is cooled to room temperature, takes out sample to get metatitanic acid cesium silicate CsSi is arrived2TiO6.5Powder.
Referring to attached drawing 1, the present embodiment 1 prepares the X-ray powder diffraction figure of sample, and XRD test result is shown, prepared
Metatitanic acid cesium silicate CsSi2TiO6.5For monophase materials, exist without any other miscellaneous phase, and crystallinity is preferable.
Referring to attached drawing 2, the present embodiment 1 prepares the SEM figure of sample, and the material crystalline is functional, and particle diameter distribution is uniform, puts down
Equal partial size is in 2 microns.
In order to verify metatitanic acid cesium silicate CsSi2TiO6.5The characteristic of photochemical catalyst weighs 100 milligrams of CsSi2TiO6.5, lead to
Crossing the crushing means such as ball mill makes particle diameter become smaller, and uses 500 watts of mercury lamps as light source, degrade 250 milliliters, 10 mg/litres
Methylene blue solution.Take within every 15 minutes a sample, after two hours of illumination, will sampling centrifugation, take its supernatant, with it is ultraviolet-
Absorbance of the visible spectrophotometer in wavelength 664-666 nanometers measurement methylene blue solution.According to Lambert-Beer's law,
Calculate the removal rate of methylene blue solution.
Referring to attached drawing 3, sample CsSi prepared by the present embodiment 12TiO6.5Ultraviolet-visible diffuse reflectance spectrum figure, from figure
As can be seen that a length of 394 nanometers of shearing wave of the sample, in UV light region.
Referring to attached drawing 4, sample CsSi prepared by the present embodiment 12TiO6.5To organic under the different UV Light time
The degradation curve of dyestuff methylene blue.It can be seen from the figure that the degradation rate of the sample photocatalytic degradation methylene blue 340 minutes
Reach 79.94%, illustrates the pure phase CsSi prepared2TiO6.5Material has certain photocatalytic activity.
Referring to attached drawing 5, sample CsSi prepared by the present embodiment 12TiO6.5The dynamics of degradating organic dye methylene blue is bent
Line chart, it can be seen from the figure that the apparent kinetics rate constant of the sample photocatalytic degradation methylene blue is 0.00554 point
Clock-1。
Embodiment 2:
Or high temperature solid-state method is used, first according to chemical formula CsSi2TiO6.5, cesium carbonate Cs is weighed respectively2CO3: 1.63
Gram, silicic acid H2SiO3: 1.56 grams, titanium dioxide TiO2: it 0.8 gram, grinds and is uniformly mixed in the agate mortar, select air gas
Atmosphere is calcined for the first time, and temperature is 350 DEG C, and calcination time is 3 hours, is then cooled to room temperature, takes out sample.Then, by preceding step sample
Product are fully ground uniformly mixed again, calcine in air atmosphere, and calcination temperature is 500 DEG C, and calcination time is 4 hours, cooling
To room temperature, sample is taken out.It is calcined finally, being placed in Muffle furnace in air after preceding step sample is fully ground, calcination temperature 600
DEG C, calcination time is 3 hours, is then cooled to room temperature, takes out sample to get metatitanic acid cesium silicate CsSi is arrived2TiO6.5Powder, and lead to
Crossing the crushing means such as ball mill makes particle diameter become smaller, and is convenient for follow-up test.
When characteristic test, 100 milligrams of photochemical catalyst CsSi are weighed2TiO6.5, use 500 watts of mercury lamps as light source, degradation
250 milliliters, the methylene blue solutions of 10 mg/litres.A sample is taken within every 15 minutes, after two hours of illumination, sampling is centrifuged, is taken
Its supernatant measures the absorbance of methylene blue solution with ultraviolet-visible spectrophotometer in wavelength 664-666 nanometers.Root
According to Lambert-Beer's law, the removal rate of methylene blue solution is calculated.It is found that CsSi made from the present embodiment2TiO6.5It is main
Structure and morphology performance, luminescent properties are similar to Example 1, also demonstrate that the metatitanic acid cesium silicate photochemical catalyst can be used as inorganic light
Catalysis material is applied.
Embodiment 3:
Or high temperature solid-state method is used, head is according to chemical formula CsSi2TiO6.5, caesium bicarbonate CsHCO is weighed respectively3: 1.94
Gram, silica SiO2: 1.2 grams, titanium dioxide TiO2: it 0.8 gram, grinds and is uniformly mixed in the agate mortar, select air gas
Atmosphere is calcined for the first time, and temperature is 400 DEG C, and calcination time is 5 hours, is then cooled to room temperature, takes out sample.Then, by preceding step sample
Product are fully ground uniformly mixed again, calcine in air atmosphere, and calcination temperature is 600 DEG C, and calcination time is 6 hours, cooling
To room temperature, sample is taken out.It is calcined finally, being placed in Muffle furnace in air after preceding step sample is fully ground, calcination temperature 800
DEG C, calcination time is 10 hours, is then cooled to room temperature, takes out sample to get metatitanic acid cesium silicate CsSi is arrived2TiO6.5Powder, and lead to
Crossing the crushing means such as ball mill makes particle diameter become smaller, and is convenient for follow-up test.
When photo-catalysis capability is tested, 100 milligrams of photochemical catalyst CsSi are weighed2TiO6.5, use 500 watts of mercury lamps as light source,
250 milliliters of degradation, the methylene blue solutions of 10 mg/litres.Take within every 15 minutes a sample, after two hours of illumination, will sample from
The heart takes its supernatant, measures the extinction of methylene blue solution in wavelength 664-666 nanometers with ultraviolet-visible spectrophotometer
Degree.According to Lambert-Beer's law, the removal rate of methylene blue solution is calculated.It is found that CsSi made from the present embodiment2TiO6.5's
Primary structure pattern performance, luminescent properties are similar to Example 1, also demonstrate that the metatitanic acid cesium silicate photochemical catalyst can be used as nothing
Machine catalysis material is applied.
Embodiment 4:
High temperature solid-state method is used again, first according to chemical formula CsSi2TiO6.5, cesium carbonate Cs is weighed respectively2CO3: 1.63
Gram, silica SiO2: 1.2 grams, titanium dioxide TiO2: it 0.8 gram, grinds and is uniformly mixed in the agate mortar, select air gas
Atmosphere is calcined for the first time, and temperature is 450 DEG C, and calcination time is 8 hours, is cooled to room temperature, takes out sample.Then, again by preceding step sample
It is secondary to be fully ground uniformly mixed, it is calcined in air atmosphere, calcination temperature is 550 DEG C, and calcination time is 9 hours, is cooled to room
Temperature takes out sample.It is calcined finally, being placed in Muffle furnace in air after preceding step sample is fully ground, calcination temperature is 750 DEG C,
Calcination time is 11 hours, is then cooled to room temperature, takes out sample to get metatitanic acid cesium silicate CsSi is arrived2TiO6.5Powder, and pass through
The crushing means such as ball mill make particle diameter become smaller, and are convenient for follow-up test.
When experiment, 100 milligrams of photochemical catalysts are weighed, use 500 watts of mercury lamps as light source, 250 milliliters of degradation, 10 milligrams/
The methylene blue solution risen.A sample is taken within every 15 minutes, after two hours of illumination, sampling is centrifuged, its supernatant is taken, with purple
Absorbance of the outside-visible spectrophotometer in wavelength 664-666 nanometers measurement methylene blue solution.It is fixed according to Lambert-Beer
Rule, calculates the removal rate of methylene blue solution.It is found that CsSi made from the present embodiment2TiO6.5Primary structure pattern performance,
Luminescent properties are similar to Example 1.
Embodiment 5:
It is prepared using sol-gel method, according to chemical formula CsSi2TiO6.5, cesium nitrate CsNO is weighed respectively3: 1.95 grams, just
Silester Si (OC2H5)4: 1.05 grams, butyl titanate: 3.41 grams, oxalic acid H2C2O4-2H2O:0.46 grams.Firstly, by nitric acid
Caesium is dissolved in deionized water, obtains clear solution, then stir by 0.5 times of addition complexing agent oxalic acid of metal cation mole amount
It mixes；Secondly ethyl orthosilicate is gone to dissolve with dust technology, while a certain amount of dehydrated alcohol is added, and carried out with deionized water dilute
It releases；Suitable glacial acetic acid solution, heating stirring, until complete hydrolysis is added in butyl titanate again；Then, by the mixed of each raw material
Close liquid be mixed to form vitreosol, be then allowed to stand, dry after obtain fluffy presoma.
Presoma is calcined in air atmosphere, calcination temperature is 300 DEG C, and calcination time is 3 hours, is subsequently cooled to room
Temperature takes out sample；The raw material of first time calcining is sufficiently mixed grinding uniformly again, is forged for the second time in air atmosphere
It burns, 500 DEG C of calcination temperature, calcination time 5 hours, is then cooled to room temperature, take out sample；It is put after finally it is fully ground again
It in Muffle furnace, calcines in air atmosphere, calcination temperature is 600 DEG C, and calcination time is 12 hours, and air atmosphere is selected to carry out
Calcining is cooled to room temperature, takes out sample to get CsSi is arrived2TiO6.5Powder.
Referring to attached drawing 6, the present embodiment 5 prepares the X-ray powder diffraction pattern of sample, and XRD test result shows that use is molten
CsSi made from glue-gel method2TiO6.5For monophase materials, not any other impurity thing mutually exists.
Referring to attached drawing 7, the present embodiment 5 prepares the SEM figure of sample, and the material crystalline is functional, and particle diameter distribution is uniform, puts down
Equal partial size is in 50 rans, it is seen that the grain diameter of sol-gal process preparation is smaller than material particle size prepared by high temperature solid-state method
It is more.
Referring to attached drawing 8, the present embodiment 5 prepares sample CsSi2TiO6.5Ultraviolet-visible diffuse reflectance spectrum figure, can from figure
To find out, a length of 397 nanometers of the shearing wave of the sample, in UV light region.
When photocatalysis characteristic is tested, 100 milligrams of photochemical catalyst CsSi are weighed2TiO6.5Powder, use 500 watts of mercury lamps as
Light source, 250 milliliters of degradation, the methylene blue solutions of 10 mg/litres.Take within every 15 minutes a sample that will take after two hours of illumination
Sample centrifugation, takes its supernatant, with ultraviolet-visible spectrophotometer in wavelength 664-666 nanometers measurement methylene blue solution
Absorbance.According to Lambert-Beer's law, the removal rate of methylene blue solution is calculated.
Referring to attached drawing 9, the present embodiment 5 prepares sample CsSi2TiO6.5To there is engine dyeing under the different UV Light time
Expect the degradation curve of methylene blue.It can be seen from the figure that the degradation rate of the sample photocatalytic degradation methylene blue reaches for 260 minutes
To 88.39%, illustrate the pure phase CsSi prepared2TiO6.5Material has certain photocatalytic activity.
Referring to attached drawing 10, the present embodiment 5 prepares sample CsSi2TiO6.5The dynamics of degradating organic dye methylene blue is bent
Line chart, it can be seen from the figure that the apparent kinetics rate constant of the sample photocatalytic degradation methylene blue is 0.00853 point
Clock-1。
Embodiment 6:
It is prepared using sol-gel method, according to chemical formula CsSi2TiO6.5, cesium oxide Cs is weighed respectively2O:1.41 grams, just
Silester Si (OC2H5)4: 1.05 grams, tetraisopropyl titanate: 2.85 grams, oxalic acid H2C2O4-2H2O:0.91 grams；It first will oxidation
Caesium is dissolved in dust technology, obtains clear solution, then stir by 1.0 times of addition complexing agent oxalic acid of metal cation mole amount；
Secondly ethyl orthosilicate is gone to dissolve with dust technology, while a certain amount of dehydrated alcohol is added, and be diluted with deionized water；
Suitable glacial acetic acid solution, heating stirring is added in tetraisopropyl titanate again, until complete hydrolysis, the mixed liquor of each raw material is mixed
Close stirring form vitreosol, be then allowed to stand, dry after obtain fluffy presoma.
Presoma is calcined in air atmosphere, calcination temperature is 350 DEG C, and calcination time is 5 hours, is subsequently cooled to room
Temperature takes out sample；The raw material of first time calcining is sufficiently mixed grinding uniformly again, is forged for the second time in air atmosphere
It burns, 400 DEG C of calcination temperature, calcination time 6 hours, is then cooled to room temperature, take out sample；It is put after finally it is fully ground again
It in Muffle furnace, calcines in air atmosphere, calcination temperature is 500 DEG C, and calcination time is 10 hours, and air atmosphere is selected to carry out
Calcining is cooled to room temperature, takes out sample to get titanate CsSi is arrived2TiO6.5Powder.
When photocatalysis characteristic is verified, 100 milligrams of photochemical catalysts can be weighed, use 500 watts of mercury lamps as light source, degradation 250
The methylene blue solution of milliliter, 10 mg/litres.A sample is taken within every 15 minutes, after two hours of illumination, sampling is centrifuged, it is taken
Supernatant measures the absorbance of methylene blue solution with ultraviolet-visible spectrophotometer in wavelength 664-666 nanometers.According to
Lambert-Beer's law calculates the removal rate of methylene blue solution.
By observation, CsSi manufactured in the present embodiment2TiO6.5The primary structure of powder, may be implemented ultraviolet light photocatalysis
Effect, the kinetic curve of degradation rate and degradation of methylene blue to methylene blue are similar to Example 5.
Embodiment 7:
Or it is prepared using sol-gel method, according to chemical formula CsSi2TiO6.5, cesium carbonate Cs is weighed respectively2CO3: 1.63
Gram, ethyl orthosilicate Si (OC2H5)4: 1.05 grams, butyl titanate: 3.41 grams, oxalic acid H2C2O4-2H2O:1.36 grams；First will
Cesium carbonate is dissolved in dust technology, obtains clear solution, then stir by 1.5 times of addition complexing agent oxalic acid of metal cation mole amount
It mixes；Secondly ethyl orthosilicate is gone to dissolve with dust technology, while a certain amount of dehydrated alcohol is added, and carried out with deionized water dilute
It releases；Suitable glacial acetic acid solution, heating stirring, until complete hydrolysis is added in butyl titanate again；By the mixed liquor of each raw material
Mixing forms vitreosol, be then allowed to stand, dry after obtain fluffy presoma.
Presoma is calcined in air atmosphere, calcination temperature is 400 DEG C, and calcination time is 5 hours, is subsequently cooled to room
Temperature takes out sample；The raw material of first time calcining is sufficiently mixed grinding uniformly again, is forged for the second time in air atmosphere
It burns, 500 DEG C of calcination temperature, calcination time 8 hours, is then cooled to room temperature, take out sample；It is put after finally it is fully ground again
It in Muffle furnace, calcines in air atmosphere, calcination temperature is 550 DEG C, and calcination time is 11 hours, and air atmosphere is selected to carry out
Calcining is cooled to room temperature, takes out sample to get CsSi is arrived2TiO6.5Powder.
When photocatalysis characteristic is verified, 100 milligrams of photochemical catalysts are weighed, use 500 watts of mercury lamps as light source, 250 milli of degradation
It rises, the methylene blue solution of 10 mg/litres.A sample is taken within every 15 minutes, after two hours of illumination, sampling is centrifuged, is taken thereon
Clear liquid measures the absorbance of methylene blue solution with ultraviolet-visible spectrophotometer in wavelength 664-666 nanometers.According to bright
Primary-Beer law calculates the removal rate of methylene blue solution.
Test result shows CsSi manufactured in the present embodiment2TiO6.5Ultraviolet light light may be implemented in the primary structure of powder
The kinetic curve of catalytic action, degradation rate and degradation of methylene blue to methylene blue is similar to Example 5.
Embodiment 8:
Or it is prepared using sol-gel method, according to chemical formula CsSi2TiO6.5, cesium nitrate CsNO is weighed respectively3: 1.95
Gram, ethyl orthosilicate Si (OC2H5)4: 1.05 grams, butyl titanate: 3.41 grams, oxalic acid H2C2O4-2H2O:1.81 grams；First will
Cesium carbonate is dissolved in dust technology, obtains clear solution, then stir by 2 times of addition complexing agent oxalic acid of metal cation mole amount
It mixes；Secondly ethyl orthosilicate is gone to dissolve with dust technology, while a certain amount of dehydrated alcohol is added, and carried out with deionized water dilute
It releases；Suitable glacial acetic acid solution, heating stirring, until complete hydrolysis is added in butyl titanate again；By the mixed liquor of each raw material
Mixing forms vitreosol, be then allowed to stand, dry after obtain fluffy presoma.
Presoma is calcined in air atmosphere, calcination temperature is 350 DEG C, and calcination time is 6 hours, is subsequently cooled to room
Temperature takes out sample；The raw material of first time calcining is sufficiently mixed grinding uniformly again, is forged for the second time in air atmosphere
It burns, 420 DEG C of calcination temperature, calcination time 7 hours, is then cooled to room temperature, take out sample；It is put after finally it is fully ground again
It in Muffle furnace, calcines in air atmosphere, calcination temperature is 580 DEG C, and calcination time is 9 hours, and air atmosphere is selected to carry out
Calcining is cooled to room temperature, takes out sample to get CsSi is arrived2TiO6.5Powder.
When photocatalysis characteristic is verified, 100 milligrams of photochemical catalysts are weighed, use 500 watts of mercury lamps as light source, 250 milli of degradation
It rises, the methylene blue solution of 10 mg/litres.A sample is taken within every 15 minutes, after two hours of illumination, sampling is centrifuged, is taken thereon
Clear liquid measures the absorbance of methylene blue solution with ultraviolet-visible spectrophotometer in wavelength 664-666 nanometers.According to bright
Primary-Beer law calculates the removal rate of methylene blue solution.
By observation, CsSi manufactured in the present embodiment2TiO6.5The primary structure of powder, to the degradation rate of methylene blue and
The kinetic curve of degradation of methylene blue is similar to Example 5.
To sum up, the chemical formula of each embodiment preparation is CsSi2TiO6.5Photochemical catalyst, it has been confirmed by experiments that have it is excellent
Ultraviolet light response photocatalysis performance, preparation process is simple, easily operated.
Claims (1)
1. a kind of application of metatitanic acid cesium silicate photochemical catalyst as inorganic catalysis material, which is characterized in that the metatitanic acid cesium silicate
The chemical formula of photochemical catalyst is CsSi2TiO6.5, pattern is irregular particle shape or form of spherical particles；The metatitanic acid cesium silicate
Photochemical catalyst has photocatalytic activity under ultraviolet light.
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