CN103086426A - Preparation method of titanium dioxide aerogel - Google Patents
Preparation method of titanium dioxide aerogel Download PDFInfo
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- CN103086426A CN103086426A CN2013100128513A CN201310012851A CN103086426A CN 103086426 A CN103086426 A CN 103086426A CN 2013100128513 A CN2013100128513 A CN 2013100128513A CN 201310012851 A CN201310012851 A CN 201310012851A CN 103086426 A CN103086426 A CN 103086426A
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Abstract
The invention discloses a preparation method of titanium dioxide aerogel. The method comprises the following steps of: (1) firstly dissolving butyl titanate in ethanol, adding a surface active agent in the mixture, and magnetically stirring the resulting solution to obtain a mixed solution A; (2) dissolving a chelating agent in a mixed solution of the ethanol and water, and uniformly stirring the resulting solution to obtain a mixed solution B; (3) adding the mixed solution B into the mixed solution A, adding a drying control chemical additive in the mixed solution, stirring and standing the resulting solution, to obtain the titanium dioxide gel; (4) orderly aging, soaking and washing the titanium dioxide gel; (5) drying the product obtained in the step 4; and (6) thermally treating the dried product obtained from the step 5 at the temperature of 200-300 DEG C for 3-5 hours to obtain the final titanium dioxide aerogel. By virtue of the method, the titanium dioxide aerogel with a relatively large specific area, relatively low density, and uniform pore size distribution can be prepared.
Description
Technical field
The invention belongs to inorganic materials preparation and sol-gel method technical field, be specifically related to a kind of method of titania aerogel for preparing take butyl (tetra) titanate as the presoma constant pressure and dry.
Background technology
TiO
2Aerogel is that the size of its inner void and essentially consist particle all is in nanometer scale by nanoparticle or the high-polymer molecular coalescent and porous three-dimensional network solid material that consists of mutually, and specific surface area is at 50～1600m
2/ g, porosity is up to 80% ~ 99.8%, and even aperture distribution, and light transmission is also better.With TiO
2Powder is different with film, TiO
2Aerogel is transparent or semitransparent shape solid, and is higher to the percent of pass of light.UV-light is sweep gas gel particle fully almost, excited gas gel top layer and inner TiO
2, discharge hole and electronics.Consist of in addition TiO
2The basic granules of aerogel is very little, is in the quantum size scope, and when UV-irradiation excited, the hole of its Surface Creation and electronics were difficult for compound, thereby has greatly improved photocatalytic activity.And it is the mesoporous material with high-specific surface area, and pollutent outside surface within it adsorbs simultaneously and degrades, and efficient is enhanced.
At present, about the existing relevant report of preparation titania aerogel.But mainly use the supercritical drying drying method, its condition is harsh, cost is higher, complex process, danger are larger.Therefore the research of safe, easy, cheap constant pressure and dry method is imperative.
Be in the patents such as CN 101288835A, CN 102671586A at publication number, introduced take titanium tetrachloride as the titanium source and take service water glass or silicic acid as the silicon source, constant pressure and dry is prepared TiO
2-SiO
2Composite aerogel.But with TiO
2Be main body, and add the preparation research that tensio-active agent carries out the aerogel of surface modification and but have no report.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation method of titania aerogel, adopts the method can prepare that specific surface area is large, density is lower, the titania aerogel of even aperture distribution.
For solving above-mentioned technical barrier, the invention provides a kind of preparation method of titania aerogel, comprise the following steps:
1), under room temperature, first butyl (tetra) titanate is dissolved in ethanol, then add the tensio-active agent magnetic agitation, obtain mixed liquor A;
2), under room temperature, sequestrant is dissolved in the mixed solution of second alcohol and water, uniform stirring obtains mixed liquid B;
3), under room temperature, mixed liquid B is added in mixed liquor A, add again afterwards drying control chemical additive, after stirring 10 ~ 60 min, standing 5 ~ 50 min obtain titania gel;
Described butyl (tetra) titanate: tensio-active agent: sequestrant: the mol ratio=1:0.0005 of drying control chemical additive ~ 0.006(is preferably 0.003 ~ 0.005): 0.3 ~ 2.4:0.2 ~ 1.0;
4), the titania gel of step 3) gained is placed in the temperature ageing 0.5 ~ 4d(days of 40 ~ 70 ℃), then use ethanol in 55 ~ 65 ℃ of washings 1 ~ 3 time, each 8 ~ 16h; Use again the finishing agent solution in 55 ~ 65 ℃ of immersions 1 ~ 3 time, each 22 ~ 26h; Use at last low surface tension solvent in 55 ~ 65 ℃ of immersions 1 ~ 3 time, each 22 ~ 26h;
5), with the gains of step 4) prior to 50 ~ 65 ℃ of drying 22 ~ 26h; Be warming up to again 70 ~ 85 ℃, insulation 3 ~ 6h; Be warming up at last 100 ~ 120 ℃, insulation 3 ~ 6h;
6), with the dry thing of step 5) gained in 200 ~ 300 ℃ of thermal treatment 3 ~ 5h, obtain titania aerogel.
Improvement as the preparation method of titania aerogel of the present invention: tensio-active agent is cetomacrogol 1000, Macrogol 2000, triblock copolymer F127, triblock copolymer F108 or triblock copolymer P123.
Further improvement as the preparation method of titania aerogel of the present invention: sequestrant is acetic acid, citric acid, vinylformic acid, oxalic acid, methyl ethyl diketone or quadrol.
Further improvement as the preparation method of titania aerogel of the present invention: drying control chemical additive is methane amide, DMF or glycerol.
Further improvement as the preparation method of titania aerogel of the present invention: the finishing agent solution is that volumetric concentration is that ethanolic soln, the volumetric concentration of 5% ~ 50% tetraethoxy is that the ethanolic soln of 5% ~ 50% trimethylchlorosilane or volumetric concentration are the ethanolic soln of 5% ~ 50% methyltrimethoxy silane.
Further improvement as the preparation method of titania aerogel of the present invention: low surface tension solvent is ethanol, normal hexane, Virahol or acetone.
Further improvement as the preparation method of titania aerogel of the present invention: step 3), mixed liquid B adds in mixed liquor A in the mode that drips, and the rate of addition of mixed liquid B is 5 ~ 10ml/min.
Further improvement as the preparation method of titania aerogel of the present invention: ethanol and step 2 that step 1) is used) the ethanol sum of using and the mol ratio of butyl (tetra) titanate are that 22 ~ 26:1(is preferably 24:1);
Step 2) water of using and the mol ratio of butyl (tetra) titanate are that 5 ~ 7:1(is preferably 6:1).
Further improvement as the preparation method of titania aerogel of the present invention: in step 1), the time of magnetic agitation is 10 ~ 20min, step 2) in time of uniform stirring be 10 ~ 20min.
In the present invention, room temperature generally refers to 10 ~ 30 ℃.
In the present invention, ethanol all refers to dehydrated alcohol.
The present invention is take titanium dioxide as main body, adds the tensio-active agent surface modification, and normal pressure prepares the method for titania aerogel.
In the present invention, adding tensio-active agent is for gel being carried out modification, improve homogeneity, size and the frame strength in duct, and caving in that when reducing because of drying, surface tension causes broken.This is main inventive point of the present invention place.
In the present invention, adding the sequestrant such as acetic acid is in order to reduce the hydrolysis rate of butyl (tetra) titanate, helps to be stablized, structure uniformly.
In the present invention, the drying control chemical additives such as methane amide can make the pore size distribution of gel narrow, the stability when improving drying.
The present invention is that the contriver is through conscientiously research, long-term experiment obtain.The present invention improves the duct by adding tensio-active agent, utilizes sol-gel technique and constant pressure and dry to prepare sample.Reaction conditions is gentle, and is lower to equipment requirements, when having improved properties of sample, reduced danger and preparation cost.
The titania aerogel specific surface area of the present invention's preparation is 300-500m
2/ g, density is 0.2-0.6g/cm
3, pore size distribution is in nanometer scale, and even structure is stable, can be widely used in the fields such as catalysis, environmental protection.
In sum, the present invention is take butyl (tetra) titanate as raw material, in conjunction with sol-gel technique, by adding tensio-active agent etc., utilizes that the constant pressure and dry technology prepares that specific surface area is large, density is lower, even aperture distribution, constitutionally stable titania aerogel.
Embodiment
The preparation method of embodiment 1, a kind of titania aerogel, carry out following steps successively:
One, preparation titania gel:
At first prepare burden:
Butyl (tetra) titanate: ethanol: water: tensio-active agent: sequestrant: the mol ratio=1:24:6:0.005:1.8:0.6 of drying control chemical additive;
Remarks explanations: above-mentioned ethanol refers to step 1) and step 2) the consumption sum of ethanol.
Select Macrogol 2000 as tensio-active agent, acetic acid is as sequestrant, methane amide is as drying control chemical additive, and the ethanolic soln of tetraethoxy (volume fraction of tetraethoxy is 20%) is as coating materials, and ethanol is low surface tension solvent;
Carry out successively following steps:
1), under room temperature, with butyl (tetra) titanate be dissolved in part ethanol (consumption only needs to guarantee at least the butyl (tetra) titanate dissolving is got final product, be for example above-mentioned ethanol total amount 1/2), Macrogol 2000 is added, magnetic agitation 15min obtains mixed liquor A;
2), under room temperature, in the solution that the water-soluble and remaining ethanol of acetic acid is formed, stir 15min, obtain mixed liquid B;
3), under room temperature, mixed liquid B is dropwise added (rate of addition is 6ml/min) in mixed liquor A, add afterwards methane amide, stir 30 min, standing 15 min of room temperature obtain titania gel;
Two, titania gel is carried out following processing again:
4), titania gel is placed in the temperature ageing 2d of 40 ℃, then with ethanol in 60 ℃ of washings 2 times, the consumption of the each washing of each 12h(must guarantee that titania gel is submerged); Use the ethanolic soln of tetraethoxy in 60 ℃ of immersions 2 times, each each consumption of 24h(must guarantee that titania gel is submerged again); Use at last ethanol in 60 ℃ of immersions 2 times, each each consumption of 24h(must guarantee that titania gel is submerged);
5), with the gains of step 4) first at 60 ℃ of dry 24h, then be warming up to 80 ℃, insulation 4h is warming up to 110 ℃ at last, insulation 4h;
6), with the dry thing of step 5) gained in 250 ℃ of thermal treatment 4h, obtain titania aerogel.
The titania aerogel specific surface area of the present invention's preparation is 496m
2/ g, density is 0.45g/cm
3, mean pore size is 8.6nm, even structure is stable.
The preparation method of embodiment 2, a kind of titania aerogel, carry out following steps successively:
One, preparation titania gel:
At first prepare burden:
Butyl (tetra) titanate: ethanol: water: tensio-active agent: sequestrant: the mol ratio=1:24:6:0.003:0.5:0.8 of drying control chemical additive;
Remarks explanations: above-mentioned ethanol refers to step 1) and step 2) the consumption sum of ethanol.
Select triblock copolymer F127 as tensio-active agent, methyl ethyl diketone is as sequestrant, N, dinethylformamide is as drying control chemical additive, the ethanolic soln of trimethylchlorosilane (volume fraction of trimethylchlorosilane is 10%) is as coating materials, and normal hexane is low surface tension solvent;
Carry out successively following steps:
1), under room temperature, with butyl (tetra) titanate be dissolved in part ethanol (consumption only needs to guarantee at least the butyl (tetra) titanate dissolving is got final product, be for example above-mentioned ethanol total amount 1/2), then add triblock copolymer F127, magnetic agitation 20min obtains mixed liquor A;
2), under room temperature, in the solution that the water-soluble and remaining ethanol of methyl ethyl diketone is formed, stir 20min, obtain mixed liquid B;
3), under room temperature, mixed liquid B is dropwise added (rate of addition is 5ml/min) in mixed liquor A, add afterwards DMF, stir 20 min, standing 25 min obtain titania gel;
Two, titania gel is carried out following processing again:
4), titania gel is placed in the temperature ageing 3d of 45 ℃, then with ethanol in 60 ℃ of washings 2 times, each 12h; Use again the ethanolic soln of trimethylchlorosilane in 60 ℃ of immersions 3 times, each 24h; Use at last normal hexane in 60 ℃ of immersions 3 times, each 24h;
5), with the gains of step 4) first at 50 ℃ of dry 24h, then be warming up to 70 ℃, insulation 4h is warming up to 100 ℃ at last, insulation 4h;
6), with the dry thing of step 5) gained in 250 ℃ of thermal treatment 4h, obtain titania aerogel.
The titania aerogel specific surface area of the present invention's preparation is 445m
2/ g, density is 0.26g/cm
3, mean pore size is 11.2nm, even structure is stable.
The preparation method of embodiment 3, a kind of titania aerogel, carry out following steps successively:
One, preparation titania gel:
At first prepare burden:
Butyl (tetra) titanate: ethanol: water: tensio-active agent: sequestrant: the mol ratio=1:24:6 of drying control chemical additive; 0.003:1.0:0.5;
Remarks explanations: above-mentioned ethanol refers to step 1) and step 2) the consumption sum of ethanol.
Select triblock copolymer P123 as tensio-active agent, citric acid is as sequestrant, glycerol is as drying control chemical additive, the ethanolic soln of methyltrimethoxy silane (volume fraction of methyltrimethoxy silane is 15%) is as coating materials, and Virahol is low surface tension solvent;
Carry out successively following steps:
1), under room temperature, with triblock copolymer P123 be dissolved in part ethanol (consumption only needs to guarantee at least the butyl (tetra) titanate dissolving is got final product, be for example above-mentioned ethanol total amount 1/2), triblock copolymer P123 is added, magnetic agitation 20min obtains mixed liquor A;
2), under room temperature, in the solution that the water-soluble and remaining ethanol of citric acid is formed, stir 20min, obtain mixed liquid B;
3), under room temperature, mixed liquid B is dropwise added (rate of addition is 7.5ml/min) in mixed liquor A, add afterwards glycerol, stir 40 min, standing 38 min obtain titania gel;
Two, titania gel is carried out following processing again:
4), titania gel is placed in the temperature ageing 3d of 60 ℃, then with ethanol in 60 ℃ of washings 3 times, each 12h; Use again the ethanolic soln of methyltrimethoxy silane in 60 ℃ of immersions 3 times, each 24h; Use at last Virahol in 60 ℃ of immersions 3 times, each 24h;
5), with the gains of step 4) first at 60 ℃ of dry 24h, then be warming up to 75 ℃, insulation 6h is warming up to 100 ℃ at last, insulation 6h;
6), with the dry thing of step 5) gained in 300 ℃ of thermal treatment 5h, obtain titania aerogel.
The titania aerogel specific surface area of the present invention's preparation is 434m
2/ g, density is 0.39g/cm
3, mean pore size is 15.4nm, even structure is stable.
The preparation method of embodiment 4, a kind of titania aerogel, carry out following steps successively:
One, preparation titania gel:
At first prepare burden:
Butyl (tetra) titanate: ethanol: water: tensio-active agent: sequestrant: the mol ratio=1:24:6:0.003:1.8:0.3 of drying control chemical additive;
Remarks explanations: above-mentioned ethanol refers to step 1) and step 2) the consumption sum of ethanol.
Select triblock copolymer F108 as tensio-active agent, acetic acid is as sequestrant, methane amide is as drying control chemical additive, and the ethanolic soln of tetraethoxy (volume fraction of tetraethoxy is 25%) is as coating materials, and normal hexane is low surface tension solvent;
Carry out successively following steps:
1), under room temperature, with butyl (tetra) titanate be dissolved in part ethanol (consumption only needs to guarantee at least the butyl (tetra) titanate dissolving is got final product, be for example above-mentioned ethanol total amount 1/2), triblock copolymer F108 is added, magnetic agitation 15min obtains mixed liquor A;
2), under room temperature, in the solution that the water-soluble and remaining ethanol of acetic acid is formed, stir 15min, obtain mixed liquid B;
3), under room temperature, mixed liquid B is dropwise added (rate of addition is 9ml/min) in mixed liquor A, add afterwards methane amide, stir 20 min, standing 42 min obtain titania gel;
Two, titania gel is carried out following processing again:
4), titania gel is placed in the temperature ageing 2d of 40 ℃, then with ethanol in 60 ℃ of washings 2 times, each 12h; Use again the ethanolic soln of tetraethoxy in 60 ℃ of immersions 3 times, each 24h; Use at last normal hexane in 60 ℃ of immersions 3 times, each 24h;
5), with the gains of step 4) first at 60 ℃ of dry 24h, then be warming up to 80 ℃, insulation 4h is warming up to 100 ℃ at last, insulation 4h;
6), with the dry thing of step 5) gained in 250 ℃ of thermal treatment 4h, obtain titania aerogel.
The titania aerogel specific surface area of the present invention's preparation is 397m
2/ g, density is 0.48g/cm
3, mean pore size is 14.1nm, even structure is stable.
The use of " Macrogol 2000 " in Comparative Examples 1-1, cancellation embodiment 1, all the other are equal to embodiment 1.
The titania aerogel specific surface area of gained is 254m
2/ g, density is 0.82g/cm
3, mean pore size is 3.2nm, and is broken serious.
Comparative Examples 1-2, " Macrogol 2000 " in embodiment 1 made into " Macrogol 4000 ", all the other are equal to embodiment 1.
The titania aerogel specific surface area of gained is 322m
2/ g, density is 0.69g/cm
3, mean pore size is 21.3nm, fragmentation is more serious.
Comparative Examples 1-3, " Macrogol 2000 " in embodiment 1 made into " poly(oxyethylene glycol) 400 ", all the other are equal to embodiment 1.
The titania aerogel specific surface area of gained is 307m
2/ g, density is 0.71g/cm
3, mean pore size is 5.9nm, fragmentation is more serious.
Comparative Examples 1-4, " butyl (tetra) titanate: the mol ratio=1:0.005 of tensio-active agent " in embodiment 1 made into " butyl (tetra) titanate: the mol ratio=1:0.01 of tensio-active agent "; All the other are equal to embodiment 1.
The titania aerogel specific surface area of gained is 408m
2/ g, density is 0.59g/cm
3, mean pore size is 14.2nm, and is easily broken.
Comparative Examples 2 ~ Comparative Examples 5,
With the tensio-active agent in embodiment 2 make respectively " triblock copolymer F108 ", " triblock copolymer P123 ", " triblock copolymer F68 ", " triblock copolymer P105 " into by " triblock copolymer F127 ", all the other are equal to embodiment 2.
Performance data such as the following table 1 of the titania aerogel of final gained:
Table 1
| Specific surface area (m 2/g） | Density (g/cm 3） | Aperture (nm) | Structure | |
| Comparative Examples 2 | 456 | 0.24 | 10.8 | Uniform and stable |
| Comparative Examples 3 | 432 | 0.29 | 8.7 | Uniform and stable |
| Comparative Examples 4 | 358 | 0.40 | 4.6 | Easily broken |
| Comparative Examples 5 | 337 | 0.43 | 4.4 | Easily broken |
At last, it is also to be noted that, what more than enumerate is only several specific embodiments of the present invention.Obviously, the invention is not restricted to above embodiment, many distortion can also be arranged.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention all should be thought protection scope of the present invention.
Claims (9)
1. the preparation method of titania aerogel is characterized in that comprising the following steps:
1), under room temperature, first butyl (tetra) titanate is dissolved in ethanol, then add the tensio-active agent magnetic agitation, obtain mixed liquor A;
2), under room temperature, sequestrant is dissolved in the mixed solution of second alcohol and water, uniform stirring obtains mixed liquid B;
3), under room temperature, mixed liquid B is added in mixed liquor A, add again afterwards drying control chemical additive, after stirring 10 ~ 60 min, standing 5 ~ 50 min obtain titania gel;
Described butyl (tetra) titanate: tensio-active agent: sequestrant: the mol ratio=1:0.0005 of drying control chemical additive ~ 0.006:0.3 ~ 2.4:0.2 ~ 1.0;
4), the titania gel of step 3) gained is placed in the temperature ageing 0.5 ~ 4d of 40 ~ 70 ℃, then use ethanol in 55 ~ 65 ℃ the washing 1 ~ 3 time, each 8 ~ 16h; Use again the finishing agent solution in 55 ~ 65 ℃ of immersions 1 ~ 3 time, each 22 ~ 26h; Use at last low surface tension solvent in 55 ~ 65 ℃ of immersions 1 ~ 3 time, each 22 ~ 26h;
5), with the gains of step 4) prior to 50 ~ 65 ℃ of drying 22 ~ 26h; Be warming up to again 70 ~ 85 ℃, insulation 3 ~ 6h; Be warming up at last 100 ~ 120 ℃, insulation 3 ~ 6h;
6), with the dry thing of step 5) gained in 200 ~ 300 ℃ of thermal treatment 3 ~ 5h, obtain titania aerogel.
2. the preparation method of titania aerogel according to claim 1, it is characterized in that: described tensio-active agent is cetomacrogol 1000, Macrogol 2000, triblock copolymer F127, triblock copolymer F108 or triblock copolymer P123.
3. the preparation method of titania aerogel according to claim 2, it is characterized in that: described sequestrant is acetic acid, citric acid, vinylformic acid, oxalic acid, methyl ethyl diketone or quadrol.
4. the preparation method of titania aerogel according to claim 3, it is characterized in that: described drying control chemical additive is methane amide, DMF or glycerol.
5. the preparation method of titania aerogel according to claim 4 is characterized in that: described finishing agent solution is that volumetric concentration is that ethanolic soln, the volumetric concentration of 5% ~ 50% tetraethoxy is that the ethanolic soln of 5% ~ 50% trimethylchlorosilane or volumetric concentration are the ethanolic soln of 5% ~ 50% methyltrimethoxy silane.
6. the preparation method of titania aerogel according to claim 5, it is characterized in that: described low surface tension solvent is ethanol, normal hexane, Virahol or acetone.
7. the preparation method of titania aerogel according to claim 6 is characterized in that: described step 3), and mixed liquid B adds in mixed liquor A in the mode that drips, and the rate of addition of mixed liquid B is 5 ~ 10ml/min.
8. the preparation method of titania aerogel according to claim 7 is characterized in that:
Ethanol and step 2 that described step 1) is used) the ethanol sum of using and the mol ratio of butyl (tetra) titanate be 22 ~ 26:1;
Step 2) water of using and the mol ratio of butyl (tetra) titanate are 5 ~ 7:1.
9. the preparation method of titania aerogel according to claim 8, it is characterized in that: in described step 1), the time of magnetic agitation is 10 ~ 20min, step 2) in time of uniform stirring be 10 ~ 20min.
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