CN102989446B - Preparation method of F-MnTiO3 - Google Patents
Preparation method of F-MnTiO3 Download PDFInfo
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- CN102989446B CN102989446B CN201210445196.6A CN201210445196A CN102989446B CN 102989446 B CN102989446 B CN 102989446B CN 201210445196 A CN201210445196 A CN 201210445196A CN 102989446 B CN102989446 B CN 102989446B
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Abstract
The invention discloses a preparation method and application of MnTiO3 and F-MnTiO3. According to a hydro-thermal synthesis method which is taken as the preparation method, titanate nanowires are taken as a Ti source, MnCl2 is taken as a Mn source, NaF is taken as an F source; the hydro-thermal synthesis method can be used for preparing the MnTiO3 and the F-MnTiO3 which are uniform in feature and diameter and of sheet-shaped structures on the condition of adding NaOH; and the MnTiO3 and the F-MnTiO3 are catalyzed and degraded to obtain organic dyestuff named rhodamine B under the irradiation of visible light. The MnTiO3 and the F-MnTiO3 both have catalytic degradation performance under visible light, and the F-MnTiO3 has higher catalytic performance than the MnTiO3 since an F element is doped in the F-MnTiO3 material, wherein F is an element with greatest electronegativity and can be combined with photoproduction electrons to restrain the combination of the photoproduction electrons and electron holes and further improve the photocatalytic efficiency of visible light. The preparation method provided by the invention is safe and rapid and is high in stability.
Description
Technical field
The present invention relates to visible-light photocatalysis material, particularly relate to MnTiO
3and F-MnTiO
3preparation method, and MnTiO
3and F-MnTiO
3nanometer visible-light photocatalysis material under visible light, the application of catalytic degradation organic dyestuff rhodamine B aspect.
Background technology
In recent years, along with industrial expansion, environmental problem and energy crisis have become two large bottlenecks of restriction human development.Along with the developing rapidly of global industry, the transition exploitation of the energy and going from bad to worse of ecological environment, make protection of the environment, maintain the ecological balance and realize the common recognition that sustainable development has become current international community.Photocatalysis technology is expected to become the crisis solving fossil energy exhaustion, and photocatalytic degradation removes toxic organic pollutant by the solution environmental problem of economy.
From Fujishima Late Cambrian TiO in 1972
2single Crystalline Electrodes can photocatalytic water come at normal temperatures, TiO
2studied by vast researcher as a kind of novel catalysis material.Report semiconductor grain photodissociation arene compound from Fujililm etc., the research and apply of semi-conducting material in the depollution of environment is obtained and develops fast.The advantages such as not only speed is fast for conductor photocatalysis, nothing selects row, degradation of organic substances completely, have become the technology of the noticeable and possible extensive uses in field such as pollutant process and purification of air.But through the research extensively and profoundly of nearly 40 years, photocatalysis technology is still difficult to realize high efficiency low cost solar energy to be changed, and its topmost reason is with TiO
2for the semiconductor light-catalyst of representative generally has larger energy gap (anatase TiO
2energy gap be 3.2eV, rutile TiO
2energy gap be 3.02eV), can only absorb the ultraviolet light in sunshine, and wavelength is in 5% of the not enough total solar energy of the ultraviolet light of below 400nm, the visible ray accounting for about 43% of sunshine gross energy mainly concentrates on 400-700nm wave band.
Therefore, how making full use of visible ray is the problem that researcher needs to solve, and the semiconductor light-catalyst that research and preparation can absorb visible ray improves solar energy utilization ratio, finally realizes the key of industrialization.
Summary of the invention
The object of the invention is for the deficiencies in the prior art, a kind of MnTiO is provided
3and F-MnTiO
3preparation method and use, MnTiO of the present invention
3and F-MnTiO
3as visible-light photocatalysis material catalytic degradation organic dyestuff rhodamine B.
The object of the invention is to be achieved through the following technical solutions: a kind of MnTiO
3the preparation method of visible-light photocatalysis material, comprises the following steps:
(1) prepare titanate nanowire by hydro-thermal method: the Ti plate of 0.15-0.3g is placed on ultrasonic 15min in the beaker that acetone is housed, then use distilled water flushing 3 times; Be that the NaOH solution of 2mol/L joins in polytetrafluoroethyllining lining autoclave by 15-25mL concentration, then cleaned Ti plate put into NaOH solution, autoclave is sealed and is placed in the baking oven of 220-240 DEG C and react 8-10h; Reaction terminates rear taking-ups Ti plate, and with distilled water flushing 3 times, and it is dry to put into drying box, namely at the surface of Ti plate acquisition titanate nanowire.
(2) MnTiO is prepared by hydro-thermal method
3visible-light photocatalysis material: under room temperature, puts into 10mL MnCl by 0.4g NaOH particle
2in saturated solution, magnetic agitation is dissolved completely to NaOH, then solution is transferred in polytetrafluoroethyllining lining autoclave, then solution put into by the Ti plate that the surface of previous step being prepared has a titanate nanowire, finally autoclave to be sealed and the baking oven putting into 240 DEG C reacts 4h; Reaction terminates rear taking-up Ti plate, and with distilled water flushing 3 times, and put into 60 DEG C of dry 6h of drying box, namely obtain MnTiO
3visible-light photocatalysis material.
A kind of F-MnTiO
3the preparation method of visible-light photocatalysis material, comprises the following steps:
(1) prepare titanate nanowire by hydro-thermal method: the Ti plate of 0.15-0.3g is placed on ultrasonic 15min in the beaker that acetone is housed, then use distilled water flushing 3 times; Be that the NaOH solution of 2mol/L joins in polytetrafluoroethyllining lining autoclave by 15-25mL concentration, then cleaned Ti plate put into NaOH solution, autoclave is sealed and is placed in the baking oven of 220-240 DEG C and react 8-10h; Reaction terminates rear taking-ups Ti plate, and with distilled water flushing 3 times, and it is dry to put into drying box, namely at the surface of Ti plate acquisition titanate nanowire.
(2) F-MnTiO is prepared by hydro-thermal method
3visible-light photocatalysis material: under room temperature, puts into 10mL MnCl by the NaOH particle of 0.4g and the NaF powder of 1g
2in saturated solution, magnetic agitation is dissolved completely to NaOH and NaF, then solution is transferred in polytetrafluoroethyllining lining autoclave, solution put into by Ti plate surface prepared by the 1st step being had titanate nanowire again, finally that autoclave is airtight and the baking oven putting into 240 DEG C reacts 2h, reaction terminates rear taking-up Ti plate, and with distilled water flushing 3 times, and put into 60 DEG C of dry 6h of drying box, namely obtain F-MnTiO
3visible-light photocatalysis material.
MnTiO3 and F-MnTiO
3visible-light photocatalysis material can be used for visible light photocatalytic degradation organic dyestuff, is specially: by 6mg MnTiO
3(concentration is 5.0*10 to put into 30mL rhodamine B
-6mol/L) in solution, ultrasonic disperse 5min, and stir 30min at lucifuge condition lower magnetic force; Then irradiate (filtering ultraviolet light with the optical filter of 420nm) with the xenon lamp of 500W.
The invention has the beneficial effects as follows, apply the MnTiO that method of the present invention can be crossed fast, stably prepare laminated structure
3and F-MnTiO
3nanometer visible-light photocatalysis material, these two kinds of nanometer visible-light photocatalysis materials can under the irradiation of visible ray, catalytic degradation organic dyestuff rhodamine B effectively.
Accompanying drawing explanation
Fig. 1 is MnTiO of the present invention
3(in figure a) and F-MnTiO
3(in figure, b) XRD of visible-light photocatalysis material schemes;
Fig. 2 is F-MnTiO of the present invention
3the EDX figure of visible-light photocatalysis material;
Fig. 3 is MnTiO of the present invention
3sEM figure under visible-light photocatalysis material low power;
Fig. 4 is MnTiO of the present invention
3sEM figure under visible-light photocatalysis material high power;
Fig. 5 is F-MnTiO of the present invention
3sEM figure under visible-light photocatalysis material low power;
Fig. 6 is F-MnTiO of the present invention
3sEM figure under visible-light photocatalysis material high power;
Fig. 7 is under radiation of visible light condition, does not add photochemical catalyst, and the uv-visible absorption spectra figure of rhodamine B solution schemes over time;
Fig. 8 is under radiation of visible light condition, adds MnTiO
3visible-light photocatalyst, the uv-visible absorption spectra figure of rhodamine B solution schemes over time;
Fig. 9 is under radiation of visible light condition, adds F-MnTiO
3visible-light photocatalyst, the uv-visible absorption spectra figure of rhodamine B solution schemes over time;
Figure 10 is visible light photocatalysis efficiency chart.
Detailed description of the invention
MnTiO of the present invention
3the preparation method of visible-light photocatalysis material, comprises the following steps:
1, titanate nanowire is prepared by hydro-thermal method.
This step is specially: the Ti plate of 0.15-0.3g is placed on ultrasonic 15min in the beaker that acetone is housed, and then uses distilled water flushing 3 times; Be that the NaOH solution of 2mol/L joins in polytetrafluoroethyllining lining autoclave by 15-25mL concentration, then cleaned Ti plate put into NaOH solution, autoclave is sealed and is placed in the baking oven of 220-240 DEG C and react 8-10h; Reaction terminates rear taking-ups Ti plate, and with distilled water flushing 3 times, and it is dry to put into drying box, namely at the surface of Ti plate acquisition titanate nanowire.
2, MnTiO is prepared by hydro-thermal method
3visible-light photocatalysis material.
This step is specially: under room temperature, and 0.4g NaOH particle is put into 10mL MnCl
2in saturated solution, magnetic agitation is dissolved completely to NaOH, then solution is transferred in polytetrafluoroethyllining lining autoclave, then solution put into by the Ti plate that the surface of previous step being prepared has a titanate nanowire, finally autoclave to be sealed and the baking oven putting into 240 DEG C reacts 4h; Reaction terminates rear taking-up Ti plate, and with distilled water flushing 3 times, and put into 60 DEG C of dry 6h of drying box, namely obtain MnTiO
3visible-light photocatalysis material.
In Fig. 1, a is laminated structure MnTiO of the present invention
3the XRD collection of illustrative plates of visible-light photocatalysis material, the XRD figure of a can with standard diagram JCPDS(no.29-0902) mapping completely, the material prepared by explanation is MnTiO
3; Other assorted peaks are not had, the MnTiO prepared by explanation in spectrogram
3material purity is high, free from admixture.
Fig. 4 is laminated structure MnTiO of the present invention
3sEM figure under visible-light photocatalysis material high power.As seen from Figure 4, prepared MnTiO
3material is sheet, and particle diameter about 1 μm, thickness is about 100nm, and pattern is roughly the same, without other patterns.
F-MnTiO of the present invention
3the preparation of visible-light photocatalysis material comprises the following steps:
1, titanate nanowire is prepared by hydro-thermal method.
This step is specially: the Ti plate of 0.15-0.3g is placed on ultrasonic 15min in the beaker that acetone is housed, and then uses distilled water flushing 3 times; Be that the NaOH solution of 2mol/L joins in polytetrafluoroethyllining lining autoclave by 15-25mL concentration, then cleaned Ti plate put into NaOH solution, autoclave is sealed and is placed in the baking oven of 220-240 DEG C and react 8-10h; Reaction terminates rear taking-ups Ti plate, and with distilled water flushing 3 times, and it is dry to put into drying box, namely at the surface of Ti plate acquisition titanate nanowire.
2, F-MnTiO is prepared by hydro-thermal method
3visible-light photocatalysis material.
This step is specially: under room temperature, and the NaOH particle of 0.4g and the NaF powder of 1g are put into 10mL MnCl
2in saturated solution, magnetic agitation is dissolved completely to NaOH and NaF, then solution is transferred in polytetrafluoroethyllining lining autoclave, solution put into by Ti plate surface prepared by the 1st step being had titanate nanowire again, finally that autoclave is airtight and the baking oven putting into 240 DEG C reacts 2h, reaction terminates rear taking-up Ti plate, and with distilled water flushing 3 times, and put into 60 DEG C of dry 6h of drying box, namely obtain F-MnTiO
3visible-light photocatalysis material.
In Fig. 1, b is laminated structure F-MnTiO of the present invention
3the XRD collection of illustrative plates of visible-light photocatalysis material.Can find out that in Fig. 1, in b and Fig. 1, a is basically identical, not have the peak of F to produce, illustrate that the content of mixed F element is little, being not enough to peak in XRD collection of illustrative plates, in order to prove the existence of F element further, having made EDX collection of illustrative plates.
Fig. 2 is laminated structure F-MnTiO of the present invention
3the EDX collection of illustrative plates of visible-light photocatalysis material.As can be seen from Figure 2, in spectrogram, there is the peak of element M n, Ti, O, F and Pt, illustrate containing Mn, Ti, O and F(in interpret sample: when the peak of Pt derives from and is SEM, the Pt of plating.) four kinds of elements, further demonstrating prepared material is F-MnTiO
3.
Fig. 6 is the SEM figure under laminated structure F-MnTiO3 visible-light photocatalysis material high power of the present invention.As seen from Figure 6, prepared F-MnTiO
3material is sheet, and particle diameter is about 800nm, and thickness is about 80nm, and pattern is roughly the same, without other patterns.
The MnTiO that the present invention prepares
3and F-MnTiO
3visible-light photocatalysis material can be used for visible light photocatalytic degradation organic dyestuff.This application is specially: by 6mg MnTiO
3or F-MnTiO
3(concentration is 5.0*10 to put into 30mL rhodamine B
-6mol/L) in solution, ultrasonic disperse 5min, and stir 30min at lucifuge condition lower magnetic force; Then irradiate (filtering ultraviolet light with the optical filter of 420nm) with the xenon lamp of 500W, at set intervals, get a certain amount of rhodamine B solution and make ultraviolet visible absorption spectra figure, calculate the concentration of rhodamine B according to ultraviolet-ray visible absorbing value, and then judge visible light catalyst MnTiO
3(or F-MnTiO
3) visible light photocatalysis ability.
Fig. 7 is under radiation of visible light condition, does not add photochemical catalyst, and the uv-visible absorption spectra figure of rhodamine B solution schemes over time; Fig. 8 adds MnTiO
3visible-light photocatalyst, the uv-visible absorption spectra figure of rhodamine B solution schemes over time; Fig. 9 adds F-MnTiO
3visible-light photocatalyst, the uv-visible absorption spectra figure of rhodamine B solution schemes over time.Figure is known for comparison diagram 7, Fig. 8 and Fig. 9 tri-width, and under the condition not adding visible-light photocatalyst, along with the increase of irradiation time, the maximal ultraviolet-visible absorbance peak value of rhodamine B solution is substantially constant; When adding MnTiO
3or F-MnTiO
3during visible-light photocatalyst, the maximal ultraviolet-visible absorbance peak value of rhodamine B solution, along with the increase of radiation of visible light time, reduces gradually, and, when adding F-MnTiO
3time, it is larger that the maximal ultraviolet of rhodamine B solution-visible absorbance peak value reduces.
Figure 10 is visible light photocatalysis efficiency chart.As can be seen from the figure, when visible ray light application time is 4h, the degradation rate of rhodamine B self only has 8.4%, and the degradation rate adding MnTiO3 is 64.2%, and adds F-MnTiO
3degradation rate then up to 91.0%.Can draw further, MnTiO
3and F-MnTiO
3under visible light illumination, all there is Photocatalytic Degradation Property, and F-MnTiO
3with MnTiO
3compare and there is higher visible light photocatalysis performance.
MnTiO
3and F-MnTiO
3as nanometer visible-light photocatalysis material, its principle is as follows: MnTiO
3and F-MnTiO
3material is semi-conducting material, and energy gap is 1.5eV, and semi-conducting material is excited under visible light illumination, and electronics transits to conduction band positions from valence band, forms light induced electron at conduction band, forms photohole in valence band.Create electron-hole pair, electronics has reproducibility, and hole has oxidisability, and the water reaction of hole and semiconductor nano material adsorption generates the very high OH free radical of oxidisability, OH free radical can with organic dyestuff rhodamine B generation oxidation reaction, to reach the effect of catalytic degradation rhodamine B.F-MnTiO
3catalytic efficiency compare MnTiO
3the high reason of catalytic efficiency be, MnTiO
3material is excited under visible light illumination, and produce electronics and hole, the electronics produced and hole are easy to compound again, will reduce the amount in hole like this, and then reduces photocatalysis efficiency; And F-MnTiO
3mixed F element in material, F is the maximum element of electronegativity, and it can be combined with light induced electron, thus inhibits the compound in light induced electron and hole, and then improves photocatalysis efficiency.
Claims (1)
1. a F-MnTiO
3the preparation method of visible-light photocatalysis material, is characterized in that, comprises the following steps:
(1) prepare titanate nanowire by hydro-thermal method: the Ti plate of 0.15-0.3g is placed on ultrasonic 15min in the beaker that acetone is housed, then use distilled water flushing 3 times; Be that the NaOH solution of 2mol/L joins in polytetrafluoroethyllining lining autoclave by 15-25mL concentration, then cleaned Ti plate put into NaOH solution, autoclave is sealed and is placed in the baking oven of 220-240 DEG C and react 8-10h; Reaction terminates rear taking-ups Ti plate, and with distilled water flushing 3 times, and it is dry to put into drying box, namely at the surface of Ti plate acquisition titanate nanowire;
(2) F-MnTiO is prepared by hydro-thermal method
3visible-light photocatalysis material: under room temperature, puts into 10mL MnCl by the NaOH particle of 0.4g and the NaF powder of 1g
2in saturated solution, magnetic agitation is dissolved completely to NaOH and NaF, then solution is transferred in polytetrafluoroethyllining lining autoclave, solution put into by Ti plate surface prepared by the 1st step being had titanate nanowire again, finally that autoclave is airtight and the baking oven putting into 240 DEG C reacts 2h, reaction terminates rear taking-up Ti plate, and with distilled water flushing 3 times, and put into 60 DEG C of dry 6h of drying box, namely obtain F-MnTiO
3visible-light photocatalysis material.
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RU2675547C1 (en) * | 2017-07-17 | 2018-12-19 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Саратовский государственный технический университет имени Гагарина Ю.А." (СГТУ имени Гагарина Ю.А.) | Method for producing a material, photoactive in a visible region of a spectrum |
CN107552042B (en) * | 2017-09-01 | 2019-11-12 | 常州大学 | Sheet manganese titanate coats attapulgite loaded CeO2Low temperature Photo-SCR denitrating catalyst and preparation method |
CN108423713B (en) * | 2018-04-13 | 2020-01-14 | 哈尔滨工业大学 | Preparation method and application of manganese titanate nanosheet material |
CN109529771A (en) * | 2019-01-11 | 2019-03-29 | 北方工业大学 | In-situ self-regeneration adsorbent and preparation method thereof |
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