CN107973599A - Titanium deoxid film preparation method based on sol-gal process - Google Patents
Titanium deoxid film preparation method based on sol-gal process Download PDFInfo
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- CN107973599A CN107973599A CN201610919965.XA CN201610919965A CN107973599A CN 107973599 A CN107973599 A CN 107973599A CN 201610919965 A CN201610919965 A CN 201610919965A CN 107973599 A CN107973599 A CN 107973599A
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- solution
- sol
- preparation
- titanium deoxid
- deoxid film
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- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 20
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 19
- 239000010936 titanium Substances 0.000 title claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000001354 calcination Methods 0.000 claims abstract description 13
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000001802 infusion Methods 0.000 claims abstract description 5
- 238000000926 separation method Methods 0.000 claims abstract description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 14
- 230000032683 aging Effects 0.000 claims description 4
- 230000029087 digestion Effects 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims 1
- 238000009776 industrial production Methods 0.000 abstract description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 7
- 229960000583 acetic acid Drugs 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- -1 Hydroxyl radical free radical Chemical class 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010931 ester hydrolysis Methods 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/62222—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining ceramic coatings
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/624—Sol-gel processing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- B01J35/39—
-
- B01J35/59—
Abstract
The invention discloses a kind of titanium deoxid film preparation method based on sol-gal process, the preparation method includes：Butyl titanate, be dissolved in absolute ethyl alcohol by S1, obtains the first solution；S2, mix water with absolute ethyl alcohol, obtains the second solution；S3, instill the first solution in the second solution dropwise, and stirs fully to react, and makes collosol and gel, and be aged at room temperature；TiO 2 sol in S4, separation solution；S5, using lifting infusion process, by TiO 2 sol, titanium deoxid film is made in the film on carrier, calcining.Titanium deoxid film preparation process is simple and convenient in the present invention, can effectively avoid in colloidal sol preparation process and fails caused by butyl titanate hydrolyzes, and success rate is high, can large-scale application in industrial production.
Description
Technical field
It is thin more particularly to a kind of titanium dioxide based on sol-gal process the present invention relates to semiconductor film technique field
Membrane preparation method.
Background technology
With expanding economy, water pollution situation is serious all the more, and photocatalysis technology is at waste water developed in recent years
Reason technology.Photochemical catalyst is the material for causing catalytic reaction under light irradiation, and by light-catalyzed reaction, generation has Strong oxdiative ability
Hydroxyl radical free radical and super oxonium ion, come decomposing organic pollutant matter of degrading.
Titanium dioxide (TiO2) it is a kind of most extensive semiconductor light-catalyst, it is widely used in photocatalysis field.
But TiO2Greater band gap, can only show photochemical activity in ultra-violet (UV) band of the wavelength less than 378nm, while its photoelectron and hole hold
Easily occur it is compound, so as to reduce photocatalysis efficiency.
TiO2Film can be prepared by sol-gel process, need that TiO 2 sol is made by sol-gel process first,
The use of lifting dipping membrane formation is a kind of preparation method of common titanium deoxid film.In the preparation of titania gel,
Butyl titanate is often added into absolute ethyl alcohol, adding glacial acetic acid makes its hydrolysis, and stirring obtains the stable sol of pale yellow transparent.But
Since butyl titanate is unstable, it is extremely easy in decomposition after being contacted with the water in air, forms milky turbid, cannot get pale yellow transparent
Colloidal sol, therefore this method there is certain defect, and failure is tended in actual operating process.
Therefore, in view of the above-mentioned problems, being necessary to propose a kind of titanium deoxid film preparation method based on sol-gal process.
The content of the invention
In view of this, the present invention provides a kind of titanium deoxid film preparation method based on sol-gal process.
In order to realize foregoing invention purpose, the present invention provides a kind of titanium deoxid film preparation side based on sol-gal process
Method, the preparation method include：
Butyl titanate, be dissolved in absolute ethyl alcohol by S1, obtains the first solution；
S2, mix water with absolute ethyl alcohol, obtains the second solution；
S3, instill the first solution in the second solution dropwise, and stirs fully to react, and makes collosol and gel, and in room
The lower ageing of temperature；
TiO 2 sol in S4, separation solution；
S5, using lifting infusion process, by TiO 2 sol, titanium deoxid film is made in the film on carrier, calcining.
As a further improvement on the present invention, in first solution, the volume ratio of butyl titanate and absolute ethyl alcohol is 1:
100~1:20.
As a further improvement on the present invention, in second solution, the volume ratio of water and absolute ethyl alcohol is 1:2~2:1.
As a further improvement on the present invention, acetic acid is further included in first solution, for adjusting the pH of the first solution
Value is between 4~6.
As a further improvement on the present invention, the digestion time in the step S3 is 10~40h.
As a further improvement on the present invention, the calcining heat in the step S5 is 300~500 DEG C, calcination time 2
~4h.
Compared with prior art, the beneficial effects of the invention are as follows：
Titanium deoxid film preparation process is simple and convenient in the present invention, can effectively avoid in colloidal sol preparation process due to metatitanic acid
Fail caused by butyl ester hydrolysis, success rate is high, can large-scale application in industrial production.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is attached drawing needed in technology description to be briefly described, it should be apparent that, drawings in the following description are only this
Some embodiments described in invention, for those of ordinary skill in the art, without creative efforts,
Other attached drawings can also be obtained according to these attached drawings.
Fig. 1 is the flow diagram of the titanium deoxid film preparation method based on sol-gal process in the present invention.
Embodiment
The technical solution in the embodiment of the present invention will be described in detail below, it is clear that described embodiment is only
Only it is part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, ordinary skill
Personnel's all other embodiments obtained on the premise of creative work is not made, belong to the model that the present invention protects
Enclose.
Join shown in Fig. 1, a kind of titanium deoxid film preparation method based on sol-gal process in the present invention, including：
Butyl titanate, be dissolved in absolute ethyl alcohol by S1, obtains the first solution；
S2, mix water with absolute ethyl alcohol, obtains the second solution；
S3, instill the first solution in the second solution dropwise, and stirs fully to react, and makes collosol and gel, and in room
The lower ageing of temperature；
TiO 2 sol in S4, separation solution；
S5, using lifting infusion process, by TiO 2 sol, titanium deoxid film is made in the film on carrier, calcining.
Preferably, in the first solution, the volume ratio of butyl titanate and absolute ethyl alcohol is 1:100~1:20.
Preferably, in the second solution, the volume ratio of water and absolute ethyl alcohol is 1:2~2:1.
Preferably, acetic acid is further included in the first solution, for adjusting the pH value of the first solution between 4~6.
Preferably, the digestion time in step S3 is 10~40h.
Preferably, the calcining heat in step S5 is 300~500 DEG C, and calcination time is 2~4h.
In the specific embodiment of the present invention, a kind of titanium deoxid film preparation method based on sol-gal process, tool
Body includes：
Butyl titanate, be dissolved in absolute ethyl alcohol by S1, and the volume ratio of butyl titanate and absolute ethyl alcohol is 1:40, obtain
One solution, meanwhile, acetic acid is added, for adjusting the pH value of the first solution between 4~6；
S2, mix water with absolute ethyl alcohol, and the volume ratio of water and absolute ethyl alcohol is 1:1, obtain the second solution；
S3, instill the first solution in the second solution dropwise, and stirs fully to react, and makes collosol and gel, and in room
The lower ageing 20h of temperature；
TiO 2 sol in S4, separation solution；
S5, using lifting infusion process by TiO 2 sol the film on carrier, calcining (calcining heat be 300~500
DEG C, calcination time is 2~4h) titanium deoxid film is made.
As can be seen from the above technical solutions, titanium deoxid film preparation process is simple and convenient in the present invention, can effectively keep away
Exempt from caused by butyl titanate hydrolyzes to fail in colloidal sol preparation process, success rate is high, can large-scale application in industrial production
In.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Profit requires rather than described above limits, it is intended that all in the implication and scope of the equivalency of claim by falling
Change is included in the present invention.Any reference numeral in claim should not be considered as to the involved claim of limitation.
Moreover, it will be appreciated that although the present specification is described in terms of embodiments, not each embodiment is only wrapped
Containing an independent technical solution, this narrating mode of specification is only that those skilled in the art should for clarity
Using specification as an entirety, the technical solution in each embodiment can also be closed through appropriate, and forming those skilled in the art can
With the other embodiment of understanding.
Claims (6)
1. a kind of titanium deoxid film preparation method based on sol-gal process, it is characterised in that the preparation method includes：
Butyl titanate, be dissolved in absolute ethyl alcohol by S1, obtains the first solution；
S2, mix water with absolute ethyl alcohol, obtains the second solution；
S3, instill the first solution in the second solution dropwise, and stirs fully to react, and makes collosol and gel, and at room temperature
Ageing；
TiO 2 sol in S4, separation solution；
S5, using lifting infusion process, by TiO 2 sol, titanium deoxid film is made in the film on carrier, calcining.
2. preparation method according to claim 1, it is characterised in that in first solution, butyl titanate and anhydrous second
The volume ratio of alcohol is 1:100~1:20.
3. preparation method according to claim 1, it is characterised in that in second solution, the body of water and absolute ethyl alcohol
Product is than being 1:2~2:1.
4. preparation method according to claim 1, it is characterised in that acetic acid is further included in first solution, for adjusting
The pH value of the first solution is saved between 4~6.
5. preparation method according to claim 1, it is characterised in that the digestion time in the step S3 is 10~40h.
6. preparation method according to claim 1, it is characterised in that the calcining heat in the step S5 is 300~500
DEG C, calcination time is 2~4h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610919965.XA CN107973599A (en) | 2016-10-21 | 2016-10-21 | Titanium deoxid film preparation method based on sol-gal process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610919965.XA CN107973599A (en) | 2016-10-21 | 2016-10-21 | Titanium deoxid film preparation method based on sol-gal process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107973599A true CN107973599A (en) | 2018-05-01 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610919965.XA Pending CN107973599A (en) | 2016-10-21 | 2016-10-21 | Titanium deoxid film preparation method based on sol-gal process |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112694122A (en) * | 2020-12-14 | 2021-04-23 | 浙江大学温州研究院 | Preparation method of granular titanium dioxide sol |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1724476A (en) * | 2005-07-05 | 2006-01-25 | 南京大学 | Preparation method of TiO2 photocatalyst for loading on ceramic surface |
| CN101053829A (en) * | 2007-05-29 | 2007-10-17 | 景德镇陶瓷学院 | Method for preparing porous titanium dioxide photocatalysis film with non-hydrolyzed sol-gel method |
| CN101444725A (en) * | 2008-12-26 | 2009-06-03 | 上海师范大学 | Method for preparing load type titanium dioxide photocatalytic film |
| CN104587994A (en) * | 2015-01-07 | 2015-05-06 | 四川师范大学 | Preparation method of TiO2 film |
-
2016
- 2016-10-21 CN CN201610919965.XA patent/CN107973599A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1724476A (en) * | 2005-07-05 | 2006-01-25 | 南京大学 | Preparation method of TiO2 photocatalyst for loading on ceramic surface |
| CN101053829A (en) * | 2007-05-29 | 2007-10-17 | 景德镇陶瓷学院 | Method for preparing porous titanium dioxide photocatalysis film with non-hydrolyzed sol-gel method |
| CN101444725A (en) * | 2008-12-26 | 2009-06-03 | 上海师范大学 | Method for preparing load type titanium dioxide photocatalytic film |
| CN104587994A (en) * | 2015-01-07 | 2015-05-06 | 四川师范大学 | Preparation method of TiO2 film |
Non-Patent Citations (1)
| Title |
|---|
| 王黎明: ""高分散纳米TiO2的低温制备、生长控制及在棉制品上的应用"", 《中国博士学位论文全文数据库工程科技I辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112694122A (en) * | 2020-12-14 | 2021-04-23 | 浙江大学温州研究院 | Preparation method of granular titanium dioxide sol |
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