CN101318128A - Method of preparing anatase structured highlight catalytic active nano-TiO2 - Google Patents
Method of preparing anatase structured highlight catalytic active nano-TiO2 Download PDFInfo
- Publication number
- CN101318128A CN101318128A CNA2008100539295A CN200810053929A CN101318128A CN 101318128 A CN101318128 A CN 101318128A CN A2008100539295 A CNA2008100539295 A CN A2008100539295A CN 200810053929 A CN200810053929 A CN 200810053929A CN 101318128 A CN101318128 A CN 101318128A
- Authority
- CN
- China
- Prior art keywords
- solution
- ratio
- catalytic active
- preparation
- active nano
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Abstract
The invention discloses a preparation method for a high photo-catalytic activity nano-TiO2 with anatase structure, which comprises the following steps: (1) weighing organic titanium compounds or titanium inorganic salt which is dissolved in glacial acetic acid to prepare the mixed solution and dissolving the mixed solution in anhydrous alcohol to obtain solution 1; (2) selecting two or three templates, dissolving the templates in the anhydrous alcohol to obtain solution 2; (3) mixing the solution 1 and solution 2, adding distilled water, stirring, obtaining settled solution, standing for 2-5 days, forming gel and drying; (4) calcining the dried matter to remove the templates and obtaining the high photo-catalytic activity nano-TiO2 with anatase structure. The high photo-catalytic activity nano-TiO2 with anatase structure prepared by the method of the invention has smaller grain diameter smaller, larger specific surface and higher photo-catalytic activity than P-25, which can be widely used in the fields such as photocatalysis and sensitized solar batteries.
Description
Technical field
The present invention relates to belong to solar cell, photochemical catalyst field.Particularly relate to a kind of preparation of nanomaterials.
Background technology
Nano-TiO
2Advantage is widely used in fields such as photocatalysis, solar cell so that its photocatalytic activity height, chemical property be stable, nontoxic etc. as important semi-conducting material.The nanometer titanic oxide material of anatase and rutile structure is present widely used nano material, and wherein the anatase nano titanium oxide has highlight catalytic active, is used for the photochemical catalyst of catalyze and degrade organic pollutants or transmission solar energy system.
The method that prepare at present nano titanium oxide is a lot, and that uses always has sol-gel process, hydro-thermal method, a solvent-thermal method etc.Wherein template plays an important role in the nano-oxide of preparation different table area and degree of crystallinity, and we utilize the agent of single mode plate also to prepare the nano-TiO with premium properties
2Yet for single mode version agent preparation process, its control level dullness can not be taken into account control crystal morphology and structure and make the nano material of preparation have high degree of crystallinity and big specific area simultaneously.At present less about the report of the titanic oxide material of preparation highlight catalytic active, United States Patent (USP) 20080045410 has been reported a kind of method that phosphorus prepares highlight catalytic active nano titanium dioxide of mixing, obtain the highlight catalytic active material by mixing phosphorus, and 750 ℃ of following calcinings 16 hours of process need, preparation process condition is had relatively high expectations.
The most frequently used commercialization nano titanium oxide is P-25 at present, and P-25 is the mixed crystal of rutile and anatase, and crystal grain is 20nm more greatly, and specific area is less, is 50m
2G
-1, have certain limitation during with photocatalyst.
Summary of the invention
The objective of the invention is to overcome deficiency of the prior art, a kind of anatase structured highlight catalytic active nano TiO is provided
2The preparation method.
Technical scheme of the present invention is summarized as follows:
A kind of anatase structured highlight catalytic active nano TiO
2The preparation method, comprise the steps:
(1) being that inorganic salts that 1: 2~4 ratio takes by weighing titanium organic compound or titanium are dissolved in glacial acetic acid and make mixed liquor in mass ratio, is that 1: 0.8~1.5 ratio is dissolved in described mixed liquor in the absolute ethyl alcohol according to volume ratio, obtains solution 1;
(2) be that 1: 1~6 or 1: 1~5: 1~4 ratio is chosen two kinds or three kinds of template agent in molar ratio, be dissolved in absolute ethyl alcohol, the mass ratio of described template agent and described absolute ethyl alcohol is 1: 5~15, obtains solution 2, and described template agent is polymer class, ammonium class or amine;
(3) be that 1: 0.5~2 ratio is mixed solution 1 and solution 2 by volume, add 1/30~1/20 distilled water of solution 1 and solution 2 mixeding liquid volumes, stirred 10~48 hours, obtain settled solution, left standstill 2~5 days at 60~120 ℃, form gel, 50~90 ℃ of dryings 12~48 hours;
(4) dry thing is removed the template agent in 1~5 hour in 350~600 ℃ of calcinings, obtain the white solid powder, promptly anatase structured highlight catalytic active nano TiO
2
Described titanium organic compound is butyl titanate, metatitanic acid four isopropyl alcohol esters, tetramethoxy titanium, purity titanium tetraethoxide or four titanium propanolates.
The inorganic salts of described titanium are TiCl
3, TiCl
4, TiO (NO
3)
2, TiOSO
4Or H
2TiF
6
Described polymer class is polyethylene glycol, polyethylene glycol-glycerine-polyethylene glycol triblock polymer or epoxy ethane-epoxy propane-oxirane triblock copolymer.
Described ammonium class is softex kw, cetyl ammonium bromide, TMAH, tetraethyl ammonium hydroxide, TPAOH or TBAH.
Described amine is triethylene diamine, n-propylamine, triethanolamine, diethanol amine, ethylenediamine or diethylamine.
Anatase structured highlight catalytic active nano TiO with method preparation of the present invention
2Its particle diameter is less than P-25, and specific area has the photocatalytic activity higher than P-25 greater than P-25, can be widely used in fields such as photocatalysis, sensitization solar battery.
Description of drawings
Fig. 1 is the device schematic diagram of sample survey photocatalytic activity;
Fig. 2 is the anatase structured highlight catalytic active nano TiO of the embodiment of the invention 1 to embodiment 3 preparation
2TiO with the conventional means preparation
2, and the photocatalytic activity comparison diagram of commercial product nano titanium oxide;
Fig. 3 is the anatase structured highlight catalytic active nano TiO of embodiment 1 to embodiment 3 preparation
2X-ray diffraction pattern;
Fig. 4 is the anatase structured highlight catalytic active nano TiO of embodiment 1 to 3 preparation
2TEM figure.Wherein A, B, C are respectively and prepare sample when polyethylene glycol and softex kw mol ratio are 1: 4,1: 6,1: 2.
The specific embodiment
The present invention is further illustrated below in conjunction with specific embodiment.
Embodiment 1:
(1) 7ml butyl titanate (TEOT), 4.6ml glacial acetic acid are added in the four-hole boiling flask, the absolute ethyl alcohol that adds 10ml is simultaneously made solvent, stirs the pale yellow solution 1 that makes clarification;
(2) take by weighing polyethylene glycol (PEG4000) and softex kw (CTAB) as double template, its mol ratio was respectively 1: 4; Add 15ml anhydrous ethanol solvent (mass ratio of template agent and absolute ethyl alcohol is 1: 10), stirring obtains solution 2 after making template agent dissolving;
(3) solution 2 is mixed with solution 1 in the four-hole boiling flask, the water of adding 1.44ml, entire reaction is carried out under room temperature, after the stirring 10h clarification, solution is transferred to crystallizing kettle and is placed insulating box, leaves standstill 3d under 60 ℃, forms gel, and drying is 24 hours under 80 ℃;
(4) with drying spy 450 ℃ of roasting 3h of temperature adjustment in Muffle furnace, grind at last and obtain powdery white solid.
Measure the character of this powder and be shown in table 1.
Embodiment 2:
According to obtaining titania powder with embodiment 1 described same procedure, just template agent polyethylene glycol (PEG4000) changes 1: 6 into the mol ratio of softex kw (CTAB).
Measure the character of this powder and be shown in table 1.
Embodiment 3:
According to obtaining titanium dioxide granule with embodiment 1 described same procedure, just template agent polyethylene glycol (PEG4000) changes 1: 2 into the mol ratio of softex kw (CTAB).
Measure the character of this powder and be shown in table 1.
Comparative Examples 1:
According to obtaining titania powder, only be to use 0.9112g single mode plate agent cetyl ammonium bromide with embodiment 1 described same procedure.
Measure the character of this powder and be shown in table 1.
Comparative Examples 2:
According to obtaining titanium dioxide granule, only be to use 0.8g single mode plate agent Macrogol 4000 with embodiment 1 described same procedure.
Measure the character of this powder and be shown in table 1.
Comparative Examples 3:
According to obtaining titanium dioxide granule, just do not add any template agent with embodiment 1 described same procedure.
Measure the character of this powder and be shown in table 1.
Table 1
|
|
|
Comparative Examples 1 | Comparative Examples 2 | Comparative Examples 3 | |
Color | White | White | White | White | White | White |
Crystalline phase | Anatase | Anatase | Anatase | Anatase | Anatase | Anatase |
Shape | Spherical | Spherical | Spherical | Spherical | Spherical | Spherical |
Specific area (m 2/g) | 111.3 | 120.7 | 100.8 | 93 | 86 | 43 |
Average grain diameter (nm) | 8.74 | 8.36 | 9.33 | 25.31 | 35.2 | 47.6 |
Chemical stability | Stable | Stable | Stable | Stable | Stable | Stable |
The photocatalysis test:
Contrast the commercial stronger titania powder of catalytic capability commonly used, the photo-catalysis capability of the titania powder that measurement is obtained to Comparative Examples 3 conditions by embodiment 1 to embodiment 3 and Comparative Examples 1, the photocatalytic activity of the nano material that relatively commercial product P-25 and this method prepare.
Fig. 1 is the device schematic diagram of sample survey photocatalytic activity, (among the figure, uviol lamp-1, quartz plate-2, quartz reactor-3, agitator-4) utilize batch (-type) heterogeneous reaction device, its material is to ultraviolet light transmittance quartz glass preferably, stir with dull and stereotyped magnetic stirring apparatus, add small magnetic needle in quartz reactor, stirring mixes reaction.With 3I
-→ I
3 -+ 2e
-Be reaction model, by measuring I
-The I that oxidation generates
3 -Concentration is estimated the activity of catalysis material, detailed process: the KI solution of configuration 0.2mol/L, each 10ml solution that takes out, add the 10mg sample, under the uviol lamp of 28W, 365nm, carry out light-catalyzed reaction, shine 3,6 respectively, 9min, take out 0.5ml then and dilute 10 times, measure with ultraviolet-uisible spectrophotometer, be scattered in I by the research catalyst
-Generate I behind the solution
3 -Speed estimate photocatalytic activity.
Fig. 2 is the anatase structured highlight catalytic active nano TiO of the embodiment of the invention 1 to embodiment 3 preparation
2TiO with the conventional means preparation
2, and the photocatalytic activity comparison diagram of commercial product nano titanium oxide; The time that carry out for photocatalysis the bottom, a, b, c are respectively the product of embodiment 1 to embodiment 3 preparation, and f represents commercial product P-25, and d, e, h are the photocatalytic activity figure of Comparative Examples 1 to Comparative Examples 3 preparation samples.
As can be seen from Figure 2, its photocatalytic activity of sample of different PEG and CTAB mol ratio preparation all is higher than commercialization titanium dioxide product P-25, and the photocatalytic activity of gained sample is the highest when template agent PEG and CTAB mol ratio are 1: 4; The product photocatalytic activity height for preparing when in addition, the sample ratio that uses hybrid template to make uses single mode plate PEG and CTAB respectively.At the photocatalytic activity of preparation sample, there is optimum value in the mol ratio of PEG and CTAB, and its photocatalytic activity of preparing product will be higher than the product for preparing when not adding the template agent when adding the template agent.
Fig. 3 is the x-ray diffraction pattern of the titania powder of embodiment 1 to embodiment 3 preparation.
In Fig. 3, the longitudinal axis is represented relative intensity and transverse axis is represented x-ray diffraction angle θ.Can determine that from figure the titania powder that derives from embodiment 1 to embodiment 3 is made up of highly purified anatase phase crystal.
The TEM figure of the titania powder that Fig. 4 obtains for embodiment 1 to embodiment 3, this photo shows that the grain diameter of the sample of preparation all is lower than 10nm.Plant discovery at Fig. 4, add the dispersion effect difference of the product of different mixed templates preparations, also there is difference in degree of scatter between its granular size and the particle.
As calculated the following anatase structured highlight catalytic active nano TiO of preparation of mixed templates of different proportionings
2Specific area be respectively 111.3m
2/ g, 120.7m
2/ g, 100.8m
2/ g is respectively 8.74nm, 8.36nm, 9.33nm through measuring particle grain size, and character is better than present widely used commercial product P-25.With 3I
-→ I
3 -+ 2e
-Be the model testing nano-TiO
2The photocatalytic activity of particle, the result can find that the photocatalytic activity of preparing product under the different templates agent conditions of mixture ratios is higher than commercial product P-25 as shown in Figure 1, this product also can be applied to other condition, as photocatalytic degradation phenol, rhodamine B etc., and other organic pollution.
Crystal structure, pattern and specific area are measured by the following method.
Crystal structure
The Japan Rigaku D/max 2500v/pc of company type X-ray diffractometer, the Cu target, tube voltage 40kV, tube current 30mA, sweep speed is 0.02 °/sec, sweep limits 0-90 °.
Crystal morphology and particle size
The Tecnai G2 F20 field transmission electron microscope that the Holland Philips produces, the pattern of observation sample and granular size;
Specific area
The N of the ASAP 2020M of U.S. Micromeritics company nitrogen absorption specific surface and voidage analysis-e/or determining sample
2Isothermal adsorption-desorption curve.
A kind of anatase structured highlight catalytic active nano TiO
2The preparation method, comprise the steps:
(1) being that 1: 3 ratio takes by weighing butyl titanate and is dissolved in glacial acetic acid and makes mixed liquor in mass ratio, is that 1: 1 ratio is dissolved in described mixed liquor in the absolute ethyl alcohol according to volume ratio, obtains solution 1;
(2) be that 1: 1 ratio is chosen polyethylene glycol-glycerine-polyethylene glycol triblock polymer and cetyl ammonium bromide as the template agent in molar ratio, be dissolved in absolute ethyl alcohol, the mass ratio of template agent and absolute ethyl alcohol is 1: 5, obtains solution 2;
(3) be that 1: 1 ratio is mixed solution 1 and solution 2 by volume, add 1/30 distilled water of solution 1 and solution 2 mixeding liquid volumes, stirred 24 hours, obtain settled solution, left standstill 3 days at 80 ℃, the formation gel was 50 ℃ of dryings 48 hours;
(4) dry thing is removed the template agent in 2 hours in 450 ℃ of calcinings, obtain the white solid powder, promptly anatase structured highlight catalytic active nano TiO
2
Embodiment 5
A kind of anatase structured highlight catalytic active nano TiO
2The preparation method, comprise the steps:
(1) being that 1: 2 ratio takes by weighing metatitanic acid four isopropyl alcohol esters and is dissolved in glacial acetic acid and makes mixed liquor in mass ratio, is that 1: 0.8 ratio is dissolved in described mixed liquor in the absolute ethyl alcohol according to volume ratio, obtains solution 1;
(2) be that 1: 6 ratio is chosen epoxy ethane-epoxy propane-oxirane triblock copolymer and triethylene diamine is the template agent in molar ratio, be dissolved in absolute ethyl alcohol, the mass ratio of template agent and absolute ethyl alcohol is 1: 5, obtains solution 2;
(3) be that 1: 0.5 ratio is mixed solution 1 and solution 2 by volume, add 1/20 distilled water of solution 1 and solution 2 mixeding liquid volumes, stirred 10 hours, obtain settled solution, left standstill 2 days at 120 ℃, the formation gel was 90 ℃ of dryings 12 hours;
(4) dry thing is removed the template agent in 3 hours in 400 ℃ of calcinings, obtain the white solid powder, promptly anatase structured highlight catalytic active nano TiO
2
A kind of anatase structured highlight catalytic active nano TiO
2The preparation method, comprise the steps:
(1) being that 1: 4 ratio takes by weighing the tetramethoxy titanium and is dissolved in glacial acetic acid and makes mixed liquor in mass ratio, is that 1: 0.8 ratio is dissolved in mixed liquor in the absolute ethyl alcohol according to volume ratio, obtains solution 1;
(2) be that 1: 4 ratio is chosen Macrogol 6000 and TMAH is the template agent in molar ratio, be dissolved in absolute ethyl alcohol, the mass ratio of template agent and absolute ethyl alcohol is 1: 15, obtains solution 2;
(3) be that 1: 2 ratio is mixed solution 1 and solution 2 by volume, add 1/25 distilled water of solution 1 and solution 2 mixeding liquid volumes, stirred 48 hours, obtain settled solution, left standstill 5 days at 60 ℃, the formation gel was 60 ℃ of dryings 40 hours;
(4) dry thing is removed the template agent in 2 hours in 400 ℃ of calcinings, obtain the white solid powder, promptly anatase structured highlight catalytic active nano TiO
2
Embodiment 7
A kind of anatase structured highlight catalytic active nano TiO
2The preparation method, comprise the steps:
(1) being that 1: 3 ratio takes by weighing purity titanium tetraethoxide and is dissolved in glacial acetic acid and makes mixed liquor in mass ratio, is that 1: 0.8~1.5 ratio is dissolved in described mixed liquor in the absolute ethyl alcohol according to volume ratio, obtains solution 1;
(2) be that 1: 3 ratio is chosen polyethylene glycol-glycerine-polyethylene glycol triblock polymer and n-propylamine is the template agent in molar ratio, be dissolved in absolute ethyl alcohol, the mass ratio of template agent and absolute ethyl alcohol is 1: 10, obtains solution 2;
(3) be that 1: 1 ratio is mixed solution 1 and solution 2 by volume, add 1/30 distilled water of solution 1 and solution 2 mixeding liquid volumes, stirred 36 hours, obtain settled solution, left standstill 4 days at 70 ℃, the formation gel was 70 ℃ of dryings 36 hours;
(4) dry thing is removed the template agent in 2 hours in 550 ℃ of calcinings, obtain the white solid powder, promptly anatase structured highlight catalytic active nano TiO
2
A kind of anatase structured highlight catalytic active nano TiO
2The preparation method, comprise the steps:
(1) being that 1: 2.5 ratio takes by weighing four titanium propanolates and is dissolved in glacial acetic acid and makes mixed liquor in mass ratio, is that 1: 1.5 ratio is dissolved in described mixed liquor in the absolute ethyl alcohol according to volume ratio, obtains solution 1;
(2) be in molar ratio 1: 1: 1 ratio to choose Macrogol 6000, tetraethyl ammonium hydroxide and triethanolamine be the template agent, be dissolved in absolute ethyl alcohol, the mass ratio of template agent and absolute ethyl alcohol is 1: 12, obtains solution 2;
(3) be that 1: 0.5 ratio is mixed solution 1 and solution 2 by volume, add 1/20 distilled water of solution 1 and solution 2 mixeding liquid volumes, stirred 12 hours, obtain settled solution, left standstill 3 days at 90 ℃, the formation gel was 80 ℃ of dryings 24 hours;
(4) dry thing is removed the template agent in 2 hours in 500 ℃ of calcinings, obtain the white solid powder, promptly anatase structured highlight catalytic active nano TiO
2
Embodiment 9
A kind of anatase structured highlight catalytic active nano TiO
2The preparation method, comprise the steps:
(1) be that 1: 3.5 ratio takes by weighing TiCl in mass ratio
3Being dissolved in glacial acetic acid and making mixed liquor, is that 1: 0.8~1.5 ratio is dissolved in described mixed liquor in the absolute ethyl alcohol according to volume ratio, obtains solution 1;
(2) be in molar ratio 1: 1: 2 ratio to choose Macrogol 4000, TPAOH and ethylenediamine be the template agent, be dissolved in absolute ethyl alcohol, the mass ratio of template agent and absolute ethyl alcohol is 1: 12, obtains solution 2;
(3) be that 1: 2 ratio is mixed solution 1 and solution 2 by volume, add 1/25 distilled water of solution 1 and solution 2 mixeding liquid volumes, stirred 18 hours, obtain settled solution, left standstill 4 days at 100 ℃, the formation gel was 90 ℃ of dryings 15 hours;
(4) dry thing is removed the template agent in 3 hours in 450 ℃ of calcinings, obtain the white solid powder, promptly anatase structured highlight catalytic active nano TiO
2
A kind of anatase structured highlight catalytic active nano TiO
2The preparation method, comprise the steps:
(1) be that 1: 3 ratio takes by weighing TiCl in mass ratio
4Being dissolved in glacial acetic acid and making mixed liquor, is that 1: 0.9 ratio is dissolved in described mixed liquor in the absolute ethyl alcohol according to volume ratio, obtains solution 1;
(2) be in molar ratio 1: 5: 1 ratio to choose Macrogol 4000, TBAH and diethanol amine be the template agent, be dissolved in absolute ethyl alcohol, the mass ratio of template agent and absolute ethyl alcohol is 1: 7, obtains solution 2;
(3) be that 1: 1 ratio is mixed solution 1 and solution 2 by volume, add 1/30 distilled water of solution 1 and solution 2 mixeding liquid volumes, stirred 24 hours, obtain settled solution, left standstill 3 days at 110 ℃, the formation gel was 85 ℃ of dryings 16 hours;
(4) dry thing is removed the template agent in 4 hours in 400 ℃ of calcinings, obtain the white solid powder, promptly anatase structured highlight catalytic active nano TiO
2
Embodiment 11
A kind of anatase structured highlight catalytic active nano TiO
2The preparation method, comprise the steps:
(1) be that 1: 3 ratio takes by weighing TiO (NO in mass ratio
3)
2Being dissolved in glacial acetic acid and making mixed liquor, is that 1: 1.5 ratio is dissolved in described mixed liquor in the absolute ethyl alcohol according to volume ratio, obtains solution 1;
(2) be that 1: 5: 4 ratio epoxy ethane-epoxy propane-oxirane triblock copolymer, TBAH and diethylamine is the template agent in molar ratio, be dissolved in absolute ethyl alcohol, the mass ratio of template agent and absolute ethyl alcohol is 1: 6, obtains solution 2;
(3) be that 1: 0.5 ratio is mixed solution 1 and solution 2 by volume, add 1/20 distilled water of solution 1 and solution 2 mixeding liquid volumes, stirred 36 hours, obtain settled solution, left standstill 4 days at 90 ℃, the formation gel was 70 ℃ of dryings 20 hours;
(4) dry thing is removed the template agent in 1 hour in 600 ℃ of calcinings, obtain the white solid powder, promptly anatase structured highlight catalytic active nano TiO
2
Embodiment 12
A kind of anatase structured highlight catalytic active nano TiO
2The preparation method, comprise the steps:
(1) be that 1: 3 ratio takes by weighing H in mass ratio
2TiF
6Being dissolved in glacial acetic acid and making mixed liquor, is that 1: 1 ratio is dissolved in mixed liquor in the absolute ethyl alcohol according to volume ratio, obtains solution 1;
(2) be in molar ratio 1: 1: 4 ratio to choose Macrogol 6000, TBAH and diethylamine be the template agent, be dissolved in absolute ethyl alcohol, the mass ratio of template agent and absolute ethyl alcohol is 1: 14, obtains solution 2;
(3) be that 1: 0.6 ratio is mixed solution 1 and solution 2 by volume, add 1/25 distilled water of solution 1 and solution 2 mixeding liquid volumes, stirred 40 hours, obtain settled solution, left standstill 3 days at 80 ℃, the formation gel was 60 ℃ of dryings 36 hours;
(4) dry thing is removed the template agent in 5 hours in 350 ℃ of calcinings, obtain the white solid powder, promptly anatase structured highlight catalytic active nano TiO
2
Claims (6)
1. anatase structured highlight catalytic active nano TiO
2The preparation method, its feature comprises the steps:
(1) being that inorganic salts that 1: 2~4 ratio takes by weighing titanium organic compound or titanium are dissolved in glacial acetic acid and make mixed liquor in mass ratio, is that 1: 0.8~1.5 ratio is dissolved in described mixed liquor in the absolute ethyl alcohol according to volume ratio, obtains solution 1;
(2) be that 1: 1~6 or 1: 1~5: 1~4 ratio is chosen two kinds or three kinds of template agent in molar ratio, be dissolved in absolute ethyl alcohol, the mass ratio of described template agent and described absolute ethyl alcohol is 1: 5~15, obtains solution 2, and described template agent is polymer class, ammonium class or amine;
(3) be that 1: 0.5~2 ratio is mixed solution 1 and solution 2 by volume, add 1/30~1/20 distilled water of solution 1 and solution 2 mixeding liquid volumes, stirred 10~48 hours, obtain settled solution, left standstill 2~5 days at 60~120 ℃, form gel, 50~90 ℃ of dryings 12~48 hours;
(4) dry thing is removed the template agent in 1~5 hour in 350~600 ℃ of calcinings, obtain the white solid powder, promptly anatase structured highlight catalytic active nano TiO
2
2. a kind of anatase structured highlight catalytic active nano TiO according to claim 1
2The preparation method, it is characterized in that described titanium organic compound is butyl titanate, metatitanic acid four isopropyl alcohol esters, tetramethoxy titanium, purity titanium tetraethoxide or four titanium propanolates.
3. a kind of anatase structured highlight catalytic active nano TiO according to claim 1
2The preparation method, the inorganic salts that it is characterized in that described titanium are TiCl
3, TiCl
4, TiO (NO
3)
2, TiOSO
4Or H
2TiF
6
4. a kind of anatase structured highlight catalytic active nano TiO according to claim 1
2The preparation method, it is characterized in that described polymer class is polyethylene glycol, polyethylene glycol-glycerine-polyethylene glycol triblock polymer or epoxy ethane-epoxy propane-oxirane triblock copolymer.
5. a kind of anatase structured highlight catalytic active nano TiO according to claim 1
2The preparation method, it is characterized in that described ammonium class is softex kw, cetyl ammonium bromide, TMAH, tetraethyl ammonium hydroxide, TPAOH or TBAH.
6. a kind of anatase structured highlight catalytic active nano TiO according to claim 1
2The preparation method, it is characterized in that described amine is triethylene diamine, n-propylamine, triethanolamine, diethanol amine, ethylenediamine or diethylamine.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CNA2008100539295A CN101318128A (en) | 2008-07-23 | 2008-07-23 | Method of preparing anatase structured highlight catalytic active nano-TiO2 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CNA2008100539295A CN101318128A (en) | 2008-07-23 | 2008-07-23 | Method of preparing anatase structured highlight catalytic active nano-TiO2 |
Publications (1)
Publication Number | Publication Date |
---|---|
CN101318128A true CN101318128A (en) | 2008-12-10 |
Family
ID=40178546
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CNA2008100539295A Pending CN101318128A (en) | 2008-07-23 | 2008-07-23 | Method of preparing anatase structured highlight catalytic active nano-TiO2 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN101318128A (en) |
Cited By (19)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101920194A (en) * | 2010-06-10 | 2010-12-22 | 南开大学 | Effective method for improving photocatalysis efficiency of nano TiO2 catalyst |
CN102198393A (en) * | 2011-04-02 | 2011-09-28 | 重庆大学 | Method for preparing mixed crystal nanometer titanium dioxide suspension from double precursors |
CN103771505A (en) * | 2012-10-24 | 2014-05-07 | 中国石油化工股份有限公司 | Synthetic method of titanium dioxide self-assembled particles |
CN103769066A (en) * | 2012-10-18 | 2014-05-07 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of titanium dioxide photocatalyst |
CN104445404A (en) * | 2014-11-07 | 2015-03-25 | 南京大学昆山创新研究院 | Preparation method of monodisperse Nb2O microspheres |
CN105618022A (en) * | 2016-01-12 | 2016-06-01 | 遵义医学院 | Preparation method of high-activity mesoporous hydrated titanium oxide powder |
CN105833919A (en) * | 2016-04-25 | 2016-08-10 | 张哲夫 | Composite visible-light response catalyst Ag2CO3/TiO2/M-ZIF-8 and application thereof |
CN106170338A (en) * | 2014-01-27 | 2016-11-30 | 道达尔公司 | As the TiO2 material of absorbent in visible spectrum and production method thereof |
CN106972170A (en) * | 2017-05-27 | 2017-07-21 | 河北省科学院能源研究所 | A kind of lithium titanate electrode material with composite pore structural and preparation method thereof |
CN107185557A (en) * | 2017-06-02 | 2017-09-22 | 西北师范大学 | A kind of preparation method of titanium dioxide supported palladium zinc cadmium sulphur photochemical catalyst |
CN107899562A (en) * | 2017-11-24 | 2018-04-13 | 武汉理工大学 | A kind of preparation method of flower-shaped hierarchy titanium dioxide gas-phase photocatalysis material |
CN109046303A (en) * | 2018-08-28 | 2018-12-21 | 燕山大学 | The preparation method of hydrophily anatase phase titanium dioxide nano-photocatalyst |
CN109319833A (en) * | 2018-10-11 | 2019-02-12 | 武汉工程大学 | A kind of preparation method of anatase titanium dioxide mesoporous nanoparticle tinaniun dioxide |
WO2019051734A1 (en) * | 2017-09-14 | 2019-03-21 | 季春柳 | Method for preparing tio2 capillary monolithic column |
CN110681380A (en) * | 2019-10-22 | 2020-01-14 | 吉林师范大学 | Preparation of high-efficiency hydrogen production catalyst Au-HSTiO by liquid phase reduction2Method (2) |
CN110694620A (en) * | 2019-10-22 | 2020-01-17 | 吉林师范大学 | Ag-HSTiO2Preparation method of composite structure catalyst |
CN112044432A (en) * | 2020-09-07 | 2020-12-08 | 南京大学 | Rapid preparation method of titanium dioxide supported gold nanoparticles at normal temperature |
CN113893664A (en) * | 2021-09-23 | 2022-01-07 | 同曦集团有限公司 | High-activity composite formaldehyde removing finishing agent |
CN115650288A (en) * | 2022-12-27 | 2023-01-31 | 北京为康环保科技有限公司 | Oxygen vacancy type titanium dioxide and preparation method and application thereof |
-
2008
- 2008-07-23 CN CNA2008100539295A patent/CN101318128A/en active Pending
Cited By (27)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101920194A (en) * | 2010-06-10 | 2010-12-22 | 南开大学 | Effective method for improving photocatalysis efficiency of nano TiO2 catalyst |
CN102198393A (en) * | 2011-04-02 | 2011-09-28 | 重庆大学 | Method for preparing mixed crystal nanometer titanium dioxide suspension from double precursors |
CN102198393B (en) * | 2011-04-02 | 2012-09-26 | 重庆大学 | Method for preparing mixed crystal nanometer titanium dioxide suspension from double precursors |
CN103769066A (en) * | 2012-10-18 | 2014-05-07 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of titanium dioxide photocatalyst |
CN103771505B (en) * | 2012-10-24 | 2015-08-12 | 中国石油化工股份有限公司 | A kind of synthetic method of titanium dioxide self-assembly particle |
CN103771505A (en) * | 2012-10-24 | 2014-05-07 | 中国石油化工股份有限公司 | Synthetic method of titanium dioxide self-assembled particles |
CN106170338A (en) * | 2014-01-27 | 2016-11-30 | 道达尔公司 | As the TiO2 material of absorbent in visible spectrum and production method thereof |
CN104445404A (en) * | 2014-11-07 | 2015-03-25 | 南京大学昆山创新研究院 | Preparation method of monodisperse Nb2O microspheres |
CN104445404B (en) * | 2014-11-07 | 2017-03-22 | 南京大学昆山创新研究院 | Preparation method of monodisperse Nb2O microspheres |
CN105618022B (en) * | 2016-01-12 | 2018-09-18 | 遵义医学院 | A kind of mesoporous hydrous titanium oxide raw powder's production technology of high activity |
CN105618022A (en) * | 2016-01-12 | 2016-06-01 | 遵义医学院 | Preparation method of high-activity mesoporous hydrated titanium oxide powder |
CN105833919A (en) * | 2016-04-25 | 2016-08-10 | 张哲夫 | Composite visible-light response catalyst Ag2CO3/TiO2/M-ZIF-8 and application thereof |
CN106972170A (en) * | 2017-05-27 | 2017-07-21 | 河北省科学院能源研究所 | A kind of lithium titanate electrode material with composite pore structural and preparation method thereof |
CN107185557A (en) * | 2017-06-02 | 2017-09-22 | 西北师范大学 | A kind of preparation method of titanium dioxide supported palladium zinc cadmium sulphur photochemical catalyst |
CN107185557B (en) * | 2017-06-02 | 2019-09-03 | 西北师范大学 | A kind of preparation method of titanium dioxide supported palladium-zinc cadmium sulphur photochemical catalyst |
WO2019051734A1 (en) * | 2017-09-14 | 2019-03-21 | 季春柳 | Method for preparing tio2 capillary monolithic column |
CN107899562B (en) * | 2017-11-24 | 2020-08-04 | 武汉理工大学 | Preparation method of flower-shaped hierarchical titanium dioxide gas-phase photocatalytic material |
CN107899562A (en) * | 2017-11-24 | 2018-04-13 | 武汉理工大学 | A kind of preparation method of flower-shaped hierarchy titanium dioxide gas-phase photocatalysis material |
CN109046303A (en) * | 2018-08-28 | 2018-12-21 | 燕山大学 | The preparation method of hydrophily anatase phase titanium dioxide nano-photocatalyst |
CN109319833B (en) * | 2018-10-11 | 2021-03-30 | 武汉工程大学 | Preparation method of anatase type mesoporous nano titanium dioxide |
CN109319833A (en) * | 2018-10-11 | 2019-02-12 | 武汉工程大学 | A kind of preparation method of anatase titanium dioxide mesoporous nanoparticle tinaniun dioxide |
CN110694620A (en) * | 2019-10-22 | 2020-01-17 | 吉林师范大学 | Ag-HSTiO2Preparation method of composite structure catalyst |
CN110681380A (en) * | 2019-10-22 | 2020-01-14 | 吉林师范大学 | Preparation of high-efficiency hydrogen production catalyst Au-HSTiO by liquid phase reduction2Method (2) |
CN112044432A (en) * | 2020-09-07 | 2020-12-08 | 南京大学 | Rapid preparation method of titanium dioxide supported gold nanoparticles at normal temperature |
CN112044432B (en) * | 2020-09-07 | 2021-12-17 | 南京大学 | Rapid preparation method of titanium dioxide supported gold nanoparticles at normal temperature |
CN113893664A (en) * | 2021-09-23 | 2022-01-07 | 同曦集团有限公司 | High-activity composite formaldehyde removing finishing agent |
CN115650288A (en) * | 2022-12-27 | 2023-01-31 | 北京为康环保科技有限公司 | Oxygen vacancy type titanium dioxide and preparation method and application thereof |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN101318128A (en) | Method of preparing anatase structured highlight catalytic active nano-TiO2 | |
KR100374478B1 (en) | Method for Preparing an Anatase Typed-Titanium Dioxide Photocatalyst and Photocatalyst Produced by the same | |
CN102523735B (en) | Silica-stabilized ultrafine anatase titania, vanadia catalysts, and methods of production thereof | |
CN102180515B (en) | Preparation method for nano titanium dioxide with high visible light catalytic activity and water dispersion thereof | |
CN101357329A (en) | Preparation method of vanadium-doped nano titanic oxide catalyst | |
CN1325381C (en) | Method for preparing medium pore molecular sieve of titanium dioxide | |
US8226911B2 (en) | Methods of producing titanium dioxide nanoparticles | |
CN101456585A (en) | In situ self-transition preparation method of urea-modified high photocatalytic activity titanic oxide hollow microsphere | |
CN103691415B (en) | High-crystallinity, rule the titania-silica nano-complex of meso-hole structure, preparation method and applications | |
CN109499620A (en) | TiO2The preparation method of/ZIF-8 composite photo-catalyst | |
US9382124B2 (en) | Synthesis method for ETS-10 titanosilicate molecular sieve | |
CN109482243A (en) | TiO2The preparation method of/MOF-5 composite photo-catalyst | |
Carlucci et al. | Selective synthesis of TiO 2 nanocrystals with morphology control with the microwave-solvothermal method | |
CN109482241A (en) | TiO2/ MOF-5 photochemical catalyst and preparation method thereof | |
US20200306728A1 (en) | Titanium dioxide sol, method for preparation thereof and products obtained therefrom | |
CN106012018A (en) | Preparation method for bismuth vanadate mesoporous single crystal | |
CN103464130B (en) | A kind of method preparing the adjustable titanium dioxide mesoporous material in aperture | |
Zhang et al. | Preparation and application of poly (zwitterionic ionic liquid) to enhance the photocatalytic activity of TiO 2 | |
Goswami et al. | Synthesis, characterization and photocatalytic reactions of phosphated mesoporous titania | |
CN101830501B (en) | Method for preparing soluble anatase titanium dioxide | |
CN105836796A (en) | Preparation method of bell-type core-shell structured nano-TiO2(at)void(at)SiO2 powder | |
CN103214033B (en) | The preparation method of the controlled spherical mesoporous titanium dioxide of size | |
CN103112896B (en) | Method for preparing octahedral nano bismuth vanadate photocatalyst by microwave process | |
CN102367180B (en) | Method for preparing high-pore order degree nano mesoporous TiO2 material with low-priced industrial titanium source | |
CN104909403B (en) | A kind of preparation method and applications of titanium dioxide nanoplate |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
C12 | Rejection of a patent application after its publication | ||
RJ01 | Rejection of invention patent application after publication |
Open date: 20081210 |