CN101524642A - Hydrothermal surface fluorination method for preparing high photocatalytic activity mesoporous titanium dioxide powder - Google Patents
Hydrothermal surface fluorination method for preparing high photocatalytic activity mesoporous titanium dioxide powder Download PDFInfo
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- CN101524642A CN101524642A CN200910061468A CN200910061468A CN101524642A CN 101524642 A CN101524642 A CN 101524642A CN 200910061468 A CN200910061468 A CN 200910061468A CN 200910061468 A CN200910061468 A CN 200910061468A CN 101524642 A CN101524642 A CN 101524642A
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- surface fluorination
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Abstract
The invention relates to a hydrothermal surface fluorination method for preparing high photocatalytic activity mesoporous titanium dioxide powder. The method is as follows: ammonium hydrogen fluoride aqueous solution is put into 200ml of polyfluortetraethylene lining, alcohol solution of tetrabutyl titanate is dropwise added into the lining, and tetrabutyl titanate is hydrolyzed and produces precipitation. And then the lining is put into another 200ml of a stainless steel reaction kettle, after the reaction kettle is sealed, the reaction kettle is heated to be 120-200 DEG C and keeps for 5-24 hours, after the reaction is over, the reaction kettle is cooled to room temperature, supernatant liquor is discarded, the obtained precipitation is sequentially washed with distilled water and ethanol, dried in vacuum and ground into fine powder, thus obtaining surface fluorination mesoporous titanium dioxide photocatalyst. The obtained photocatalyst has high activity. The method is simple, environmental friendly.
Description
Technical field
The present invention relates to hydrothermal surface fluorination and handle the method that improves the optically catalytic TiO 2 activity.
Technical background
Since Fujishima in 1972 and Honda found the optically catalytic TiO 2 decomposition water, titanium dioxide and other conductor photocatalysis materials were owing to have potential widely application in water and air purification and field of solar energy and paid close attention to.In various oxides and non-oxidized substance conductor photocatalysis material, titanium dioxide is with the lasting stability of its biological and chemical inertia, strong oxidability, cheapness and anti-light and chemical attack and become only catalysis material.From practical application and commercial angle, the photocatalytic activity of titanium dioxide must further improve.In recent years, many degree of crystallinity and photocatalytic activities of discovering fluorine doping can raising anatase phase titanium dioxide, surface fluorination then becomes a kind of new method of titanium dioxide surface modification.Surface fluorination can be realized by the hydroxyl of titanium dioxide surface and the ion-exchange reactions between the fluorine ion simply.
Titanium dioxide (F-TiO behind the surface fluorination
2) demonstrate the photocatalytic activity higher in the photochemical catalytic oxidation acid orange 7 in the aqueous solution and the process of phenol than the titanium dioxide of not fluoridizing.The degree of fluorination of titanium dioxide largely depends on the pH value, has the highest degree of fluorination (about 99%) when pH equals 3-4.Studies show that the surface after fluoridizing helps the generation of hydroxyl radical free radical (non-surface hydroxyl), and hydroxyl radical free radical helps to improve oxidability.Because surface fluorination thing itself can not react F-TiO with the valence band hole
2But the raising attribution of suspension photochemical catalytic oxidation ability is increase (reaction 2) of hydroxyl radical free radical, and the TiO that does not fluoridize
2The hydroxyl radical free radical on surface more trends towards being adsorbed on surface (reaction 3).
These reactions show: F-TiO
2Light-catalyzed reaction in the suspension can be away from TiO
2Carry out the solution inside on surface.Current titanium dioxide surface fluorination process is to realize (reaction 3) by the hydroxyl of titanium dioxide surface and the ion-exchange reactions between the fluorine ion, adopts the surface fluorination titanium dioxide of this method preparation to show lower photocatalytic activity usually in the gas-phase photocatalysis reaction.
This patent has proposed a kind of hydrothermal surface fluorination and has handled the method that improves the optically catalytic TiO 2 activity, promptly by the sediment of hydrothermal treatment consists butyl titanate (TBOT) in the mixed solution of ammonium acid fluoride, second alcohol and water, a step is prepared the surface fluorination mesoporous titanium dioxide powder with highlight catalytic active.
Summary of the invention
The objective of the invention is to consider the deficiency that common preparation high-activity nano titanium dioxide photocatalytic method exists, proposed a kind of hydrothermal surface fluorination method for preparing high photocatalytic activity mesoporous titanium dioxide powder according to present domestic and international research present situation.This method is simple, low temperature, water are solvent, environmental friendliness.Adopting this method can prepare grain size is 10-12nm, and mesoporous aperture is 5.5-6.5nm, and specific area is 120-125m
2The high activity mesopore titania photocatalyst of/g.
The technical scheme that realizes the object of the invention is:
A kind of hydrothermal surface fluorination method for preparing the highlight catalytic active nano titania powder is characterized in that Preparation of Catalyst and surface fluorination handle a step and finish, and method step is followed successively by:
1st, the configuration ammonium acid fluoride aqueous solution and butyl titanate ethanolic solution, solution allocation is: 0.01-1 gram ammonium acid fluoride adds 150 ml waters; 12 milliliters of butyl titanates add in the 10-40 milliliter ethanol;
2nd, the ethanolic solution of the butyl titanate that is disposed dropwise joins in the ammonium acid fluoride aqueous solution under magnetic agitation;
3rd, this mixed solution is transferred in 200 milliliters of water heating kettles, 80% volume of water heating kettle is filled, cover water heating kettle completely, at 100-200 ℃ of hydro-thermal reaction 5-24 hour;
4th, the white solid of gained precipitation is collected water and ethanol washing successively, then in vacuum drying chamber in 30-100 ℃ dry 1-3 hour down, promptly make the highlight catalytic active nano titania powder.
The preferred for preparation condition is: the described ammonium acid fluoride aqueous solution adds the configuration of 120 ml waters by 0.29-0.57 gram ammonium acid fluoride;
Described butyl titanate ethanolic solution adds 30 milliliters of ethanol configurations by butyl titanate 5-10 milliliter, preferably adds 30 milliliters of ethanol configurations by butyl titanate 6-7 milliliter;
Described hydrothermal temperature is 140-160 ℃;
The described hydro-thermal reaction time is 8-12 hour;
The 4th step in vacuum drying chamber in 80 ℃ of dryings 2 hours.
The photocatalytic activity that prepared high activity surface is fluoridized titanium dioxide characterizes by the airborne acetone of photocatalytic degradation.Experimentation is as follows: TiO
2The test of the photocatalytic degradation acetone of sample is to carry out in 15 liters of airtight rectangular vessels, and the initial concentration of acetone is 275 ± 25ppm.The preparation process of photochemical catalyst sample is with TiO
2It is on 7 centimetres the culture dish that suspension evenly is coated onto 3 diameters, with culture dish 80 ℃ dry down, it is stand-by to be cooled to room temperature then.The quality of each test specimen remains on 0.3 gram.During experiment culture dish is put into reactor, in reactor, inject acetone with microsyringe then.Reactor directly is connected with a drier that contains calcium chloride, so that the initial humidity in the control reactor.Before UV-irradiation, allow acetone steam and catalyst reach the adsorption-desorption balance.Measure the ultraviolet ray intensity that shines sample surfaces with ultraviolet light photometer (UV-A type, photoelectric instrument factory of Beijing Normal University makes), its intensity is 2.5mW/cm
2, and the wavelength peak of ultraviolet light is 365nm.The concentration of acetone, carbon dioxide and steam adopts the infrared multi-component gas monitor of optoacoustic (photoacoustic IR multigas monitor, INNOVA air techinstruments model 1312) to carry out online check and analysis in the reactor.TiO
2The photocatalytic activity of sample comes quantitatively characterizing by comparing each apparent reaction rate constant.The photocatalysis oxidation reaction of acetone is a pseudo first order reaction, and its kinetics equation can be expressed as: ln (C
0/ C)=and kt, k is the apparent speed constant, C
0With C be respectively concentration in the initial and course of reaction of acetone.In addition, prepared product application aspect the dyestuff contaminant in degradation water is also verified by the test of the rhodamine B aqueous solution that fades.Along with the carrying out of light-catalyzed reaction, the change in concentration of rhodamine B detects by the absorptance of measuring its aqueous solution.Its absorptance by day island proper Tianjin UV-2550 ultraviolet-uisible spectrophotometer measure.
The characterizing method that high activity surface is fluoridized the micro-structural of titanium dioxide optical catalyst is: at the Cu target is that X-ray source, sweep speed are that X-ray diffraction (XRD) spectrogram that obtains on the x-ray diffractometer (HZG41/B-PC type) of 0.05 degree/second is determined crystalline phase and crystallite dimension.The specific area of powder sample is that the method by nitrogen absorption is to test on the n2 absorption apparatus device of MicromeriticsASAP 2020 (USA) in model.All samples all outgased 2 hours down at 100 ℃ earlier before test.The Brunauer-Emmett-Teller of sample (BET) surface area (S
BET) be to utilize relative pressure (P/P by multiple spot BET method
0) be that the interior adsorpting data of 0.05～0.3 scope calculates.By desorption isotherm, adopt Barret-Joyner-Halender (BJH) method, and suppose that the hole is the cylindrical shape hole, determine pore-size distribution.With relative pressure (P/P
0) be that 0.994 nitrogen adsorption volume is determined pore volume and average pore size.Utilization transmission electron microscope (TEM) and high-resolution-ration transmission electric-lens (HRTEM) are observed the size and dimension of the crystal grain of mesoporous titanium dioxide powder.Observe the required sample of TEM and be at first under ultrasound condition TiO
2Powder is distributed in the absolute ethyl alcohol, then dispersant liquid drop is added to prepare on carbon film-copper composite web.
Hydrothermal surface fluorination method of the present invention is the preparation of suitable other high activity materials also.
Further specify the present invention below in conjunction with drawings and Examples.
Description of drawings
Fig. 1 is at different R
FThe TiO for preparing under the condition
2The XRD figure of sample
Fig. 2 R
F=0 and R
F=0.5 o'clock TiO
2Nitrogen adsorption-the desorption isotherm of sample
Fig. 3 R
F=0 and R
F=0.5 o'clock TiO
2The pore size distribution curve of sample
Fig. 4 R
F=0.5 TiO
2The TEM of sample
Fig. 5 R
F=0.5 TiO
2The HRTEM of sample
The different R of Fig. 6
FTiO
2The comparison of sample speed constant
R wherein
FAtomic ratio for fluorine and titanium.
The specific embodiment
Receive brilliant TiO in order to prepare
2Powder, butyl titanate are used as the titanium source.The detailed experiments process is as follows: the distilled water of at first getting 120 milliliters places 200 milliliters polytetrafluoroethyllining lining, toward wherein adding 0.29-0.57 gram ammonium acid fluoride and constantly stirring it is dissolved fully.Then 6.8 milliliters of butyl titanates are dissolved in 30 milliliters the ethanol and fully mix, at ambient temperature, this solution is dropwise added in the aqueous solution of ammonium acid fluoride and constantly stir.It is hydrolysis that butyl titanate is met water, produces precipitation.After the sealing, reactor is heated to 150 ℃, and under this temperature, kept 10 hours.Behind the reactor cool to room temperature, collect white product and successively with deionized water and ethanol washing, then with powder in drying box in 80 ℃ of dryings 2 hours.At last desciccate is ground to form fine powder with agate mortar, promptly get required surface fluorination TiO
2Powder sample.
Characterize the phase structure of prepared sample with XRD.The TiO that under different temperatures, prepares
2The XRD figure of sample is shown in Fig. 1 and table 1 with relevant physical property.Titanium dioxide (the R that as can be seen from Figure 1 prepares in the pure water
F=0) is mainly the anatase phase, contains a spot of brockite phase simultaneously.What be positioned at 2 θ=30.7 ° is unimodal promptly corresponding to the diffraction maximum of titanium dioxide brockite phase (121) face.Add NH
4HF
2The prepared TiO that goes out in back
2Do not have the brockite phase, this is because NH
4HF
2Suppressed the formation of brockite.Further observe and find, along with R
FRaising, the XRD peak of anatase phase strengthens gradually, the width of diffraction maximum also narrows down gradually, shows TiO
2Growing up and the raising of degree of crystallinity of crystal grain.TiO
2The degree of crystallinity of nano particle is calculated by the relative intensity of anatase (101) face diffraction maximum and is got.Table 1 has been listed different R
FFollowing TiO
2The average grain size of sample and anatase be relative crystallinity mutually.As can be seen from the table, average grain size and anatase mutually relative crystallinity along with R
FRaising and improve.
Fig. 2 has provided R
F=0 and R
FNitrogen adsorption-the desorption isotherm of=0.5 o'clock titanium dioxide sample.The nitrogen adsorption-desorption thermoisopleth of all titanium dioxide is the IV type, is to have a hysteresis winding between the 0.5-0.8 at relative pressure, and loopback type is the H2 type, is generally ink bottle hole (small for mouth and large for cavity).
Fig. 3 has provided R
F=0 and R
FPrepared the pore size distribution curve of sample correspondence at=0.5 o'clock.By the pore size distribution curve that the nitrogen desorption isotherm obtains narrower (3.0-8.0nm), the peak bore dia is about 5.4nm by BJH (Barrett-Joyner-Halenda) method.These mesoporous reunions that come from primary particle.Narrow pore size distribution shows the TiO of the method preparation
2Particle has the pore-size distribution of homogeneous.
Fig. 4 has provided R
FThe TiO of preparation in=0.5 o'clock
2The TEM of sample.As can be seen from the figure TiO
2The crystalline substance of receiving is aggregating state, and contains the meso-hole structure of disordered state.The average-size of the primary granule of estimating from the TEM photo is approximately 11 ± 2nm, with the grain size value (11.2nm) very identical (as shown in table 1) that adopts the Scherrer equation to calculate from XRD figure.
Fig. 5 has provided R
FThe TiO of preparation in=0.5 o'clock
2The HRTEM photo of sample.As can be seen from the figure lattice fringe clearly shows the height of specimen crystallization.The spacing of lattice fringe is 0.35nm, with anatase TiO mutually
2(101) spacing of crystal face matches.
Fig. 6 has provided R under UV-irradiation
FTo prepared TiO
2The influence of the apparent reaction rate constant of powder and with the photocatalytic activity of P25 relatively.What prepare in the pure water does not fluoridize TiO
2Have photocatalytic activity preferably, this is because it has bigger specific area and little crystallite dimension.And all TiO after fluoridizing
2Have than not fluoridizing the activity higher with P25.Along with R
FIncrease, fluoridize TiO
2Crystallization strengthens, and its photocatalytic activity significantly improves.Work as R
F=0.5 o'clock, k reached maximum, was 17.35 * 10
-3Min
-1And its light-catalyzed reaction speed constant of the P25 with good photocatalytic activity of generally acknowledging is 5.64 * 10
-3Min
-1R
FFluoridized TiO at=0.5 o'clock
2Photocatalytic activity be 3.01 times of P25, this is because it has the specific area bigger than P25, less crystallite dimension and meso-hole structure etc.Generally speaking, the specific area of P25 and grain size are respectively 50m
2g
-1And 30nm.Along with R
FFurther increase, the k value then obviously reduces.
Embodiment 2:
In order to check of the influence of hydro-thermal time to the sample photocatalytic activity, 50 ℃ of hydrothermal temperature stuck-at-s, except that the hydro-thermal asynchronism(-nization), other reaction condition as: the amounts of butyl titanate, absolute ethyl alcohol, ammonium acid fluoride and water etc. are all identical with embodiment 1.The result shows that the sample that prepared at 0.5-1 hour is owing to its impalpable structure, and it does not have photocatalytic activity basically.Along with the prolongation of hydro-thermal time, the photocatalytic activity of sample improves gradually.Be increased to 8 hours when the hydro-thermal time, the photocatalytic activity of sample obviously increases and is higher than P25, and this may be because the former has bigger specific area, higher pore volume and littler crystallite dimension.The photocatalytic activity of the sample of preparation in 10 hours is the highest.Though this sample has less specific area than the sample of preparation in 5 hours, it has bigger crystallite dimension and the degree of crystallinity of Geng Gao.Usually degree of crystallinity is high more, that is to say that defective is few more mutually with body on the surface, causes the recombination probability in light induced electron and hole to reduce increase with photocatalytic activity.Continue to prolong the hydro-thermal time by 15-24 hour, then photocatalytic activity begins to reduce, and this is possible be because the increase of crystallite dimension causes specific area and pore volume sharply to reduce.Can reason out according to above result and to have more high-crystallinity and the more TiO of large pore volume
2Particle more helps light-catalysed application.In the present embodiment, 5-24 hour hydro-thermal time all can be realized the raising to photocatalytic activity, and the best hydro-thermal time was advisable with 8-12 hour.
Embodiment 3:
In order to check the influence of hydrothermal temperature to the sample photocatalytic activity, except that hydro-thermal temperature difference, other reaction conditions as: the amounts of hydro-thermal time (10 hours), butyl titanate, absolute ethyl alcohol, ammonium acid fluoride and water etc. are all identical with embodiment 1.The result shows that when hydrothermal temperature was lower than 100 ℃, prepared sample was amorphous state substantially, and photocatalytic activity is very low.Along with the raising of temperature, the photocatalytic activity of titanium dioxide also improves gradually, and this is because higher temperature more helps growing up of crystal grain.When temperature rose to 140-160 ℃, the photocatalytic activity of prepared titanium dioxide reached peak.Continue rising temperature to 200 ℃, the activity of sample begins to reduce, this be sharply descend by specific area due to.Therefore, to prepare the best hydrothermal temperature of high-activity titanium deoxide be 140-160 ℃ to this method.
Embodiment 4:
For the influence of the amount of checking butyl titanate to the sample photocatalytic activity, except that the amount difference of butyl titanate, other reaction condition as: the amounts (120 milliliters) of reaction temperature (150 ℃), reaction time (10 hours), water etc. are all identical with embodiment 1.The result shows, when the amount of butyl titanate during in 5-10 milliliter scope, prepared titanium dioxide sample all has higher photocatalytic activity.The amount of finding best butyl titanate in the experiment is the 6-7 milliliter.
The different R of table 1
FTo TiO
2The influence of the physical property of sample
| R F | Phase composition | Specific surface (m 2/g) | Pore volume (cm 3/g) | Average pore size (nm) | Porosity (%) | Crystallite dimension (nm) |
| 0 | A，B | 196.6 | 0.28 | 5.7 | 50.9 | 8.1(1.00) |
| 0.25 | A | 126.6 | 0.19 | 5.8 | 41.3 | 10.9(1.35) |
| 0.5 | A | 122.0 | 0.19 | 6.1 | 41.3 | 11.2(1.38 |
| 1 | A | 120.9 | 0.18 | 6.2 | 40.0 | 11.5(1.42) |
A represents the anatase phase in the table 1, and B represents the brockite phase; The BET surface area is by the linear segment (P/P of adsorption isotherm
0=0.05-0.3) calculate; Pore volume (total pore volume) is from P/P
0=0.994 N
2Adsorption volume obtains; Average pore size is with desorption isotherm and the estimation of Barrett-Joyner-Halenda (BJH) method; Porosity is estimated by pore volume; TiO
2Average grain size calculate with the Scherrer equation by XRD; Relative crystallinity: the relative intensity (being shown in the bracket) of anatase phase (101) crystal face diffraction maximum.
Claims (6)
1, a kind of hydrothermal surface fluorination method for preparing the highlight catalytic active nano titania powder is characterized in that method step is followed successively by:
1st, the configuration ammonium acid fluoride aqueous solution and butyl titanate ethanolic solution, solution allocation is: 0.01-1 gram ammonium acid fluoride adds 150 ml waters; 12 milliliters of butyl titanates add in 1040 milliliters of ethanol;
2nd, the ethanolic solution of the butyl titanate that is disposed dropwise joins in the ammonium acid fluoride aqueous solution under magnetic agitation;
3rd, this mixed solution is transferred in 200 milliliters of water heating kettles, 80% volume of water heating kettle is filled, cover water heating kettle completely, at 100-200 ℃ of hydro-thermal reaction 5-24 hour;
4th, the white solid of gained precipitation is collected water and ethanol washing successively, then in vacuum drying chamber in 30-100 ℃ dry 1-3 hour down, promptly make the highlight catalytic active nano titania powder.
2, the hydrothermal surface fluorination method of preparation highlight catalytic active nano titania powder as claimed in claim 1 is characterized in that: the described ammonium acid fluoride aqueous solution adds the configuration of 120 ml waters by 0.29-0.57 gram ammonium acid fluoride.
3, the hydrothermal surface fluorination method of preparation highlight catalytic active nano titania powder as claimed in claim 1 is characterized in that: described butyl titanate ethanolic solution adds 30 milliliters of ethanol configurations by butyl titanate 5-10 milliliter.
4, as the hydrothermal surface fluorination method of described each preparation highlight catalytic active nano titania powder of claim 1-3, it is characterized in that: described hydrothermal temperature is 140-160 ℃.
5, as the hydrothermal surface fluorination method of described each preparation highlight catalytic active nano titania powder of claim 1-3, it is characterized in that: the described hydro-thermal reaction time is 8-12 hour.
6, as the hydrothermal surface fluorination method of described each preparation highlight catalytic active nano titania powder of claim 1-3, it is characterized in that: the 4th step in vacuum drying chamber in 80 ℃ of dryings 2 hours.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109046302A (en) * | 2018-08-27 | 2018-12-21 | 合肥工业大学 | A kind of porous petal-like anatase TiO2Nano-crystal film and preparation method thereof |
| CN110026173A (en) * | 2019-04-28 | 2019-07-19 | 苏州科技大学 | Nano-ZnO/TiO2Composite photo-catalyst and its preparation method and application |
| CN111072114A (en) * | 2018-10-18 | 2020-04-28 | 南京化学工业园环保产业协同创新有限公司 | Nano circulating water treatment agent with biological activity |
| CN111710873A (en) * | 2020-06-23 | 2020-09-25 | 深圳市德立新材料科技有限公司 | Method for preparing ultrathin lithium battery copper foil through photocatalytic deposition |
-
2009
- 2009-04-08 CN CN200910061468A patent/CN101524642A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109046302A (en) * | 2018-08-27 | 2018-12-21 | 合肥工业大学 | A kind of porous petal-like anatase TiO2Nano-crystal film and preparation method thereof |
| CN109046302B (en) * | 2018-08-27 | 2021-12-07 | 合肥工业大学 | Porous petal-shaped anatase TiO2Nanocrystalline thin film and preparation method thereof |
| CN111072114A (en) * | 2018-10-18 | 2020-04-28 | 南京化学工业园环保产业协同创新有限公司 | Nano circulating water treatment agent with biological activity |
| CN110026173A (en) * | 2019-04-28 | 2019-07-19 | 苏州科技大学 | Nano-ZnO/TiO2Composite photo-catalyst and its preparation method and application |
| CN111710873A (en) * | 2020-06-23 | 2020-09-25 | 深圳市德立新材料科技有限公司 | Method for preparing ultrathin lithium battery copper foil through photocatalytic deposition |
| CN111710873B (en) * | 2020-06-23 | 2021-09-17 | 深圳市德立新材料科技有限公司 | Method for preparing ultrathin lithium battery copper foil through photocatalytic deposition |
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