CN1733846A - Method for preparing peroxo-titanic acid photocatalytic coating agent - Google Patents
Method for preparing peroxo-titanic acid photocatalytic coating agent Download PDFInfo
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- CN1733846A CN1733846A CN 200410020302 CN200410020302A CN1733846A CN 1733846 A CN1733846 A CN 1733846A CN 200410020302 CN200410020302 CN 200410020302 CN 200410020302 A CN200410020302 A CN 200410020302A CN 1733846 A CN1733846 A CN 1733846A
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Abstract
The invention discloses a method for peroxy titanic acid with visible-light activity for supported photocatalyst. Wherein, preparing clear solution with given concentration by TiSO4 to drip with diluted ammonia into deionized water with given pH value as basic solution; mixing and holding given pH value to form precursor deposition of titanium oxide; continuing to mix for some time; taking solid-liquid separation to the suspending liquid to clean for 3-5 times, dripping some H2O2 peptizer to deposite and obtain the product. The film coating can crystallize and form anatase phase at 150Deg. The membrane layer particle is 10-20 nano sphere or ~20X~100 nano column.
Description
Technical field
The present invention relates to a kind of preparation method of coating agent of photocatalysis, relate to the method that a kind of precipitationpeptization legal system of utilizing inorganic salt is equipped with the pertitanic acid coating agent of photocatalysis in particular.
Background technology
Usually the loading type titanium oxide base photocatalyst of using generally is that powder coheres method or adopts sol-gel technique to load on the base material; Alkoxide that the cost of material that the latter uses is valuable and general inorganic salt contain a large amount of organic solvents or complexing agent, and the acidity of colloidal sol are stronger, and metal base is restricted; Prepared cohere coating and dissolved glue film all needs higher thermal treatment temp, organic thermolysis contaminate environment, and raw materials cost is improved, application art is complicated.Applied titanium oxide base photocatalyst is arranged at present, contain a large amount of organic solvent classes, need higher thermal treatment temp, organism volatilization contaminate environment, efficient is low, cost is high; And be strongly-acid or stronger acidity, but the base material range of load is little, influences the application of photocatalyst.
Summary of the invention
The present invention is in order to overcome weak point of the prior art, provides that a kind of preparation cost is low, application art is simple, and product has visible light activity, loading type photocatalytic titanium oxide with the method that applies agent.
The present invention is achieved by following technical proposals: earlier with TiOSO
4NH
2O makes clear solution, gets appropriate amount of deionized water (water furnishing certain pH 7～9) and does end liquid, with 0.1～0.5mol/L TiOSO
4Settled solution and 3mol/L ammoniacal liquor (NH
3H
2O) two kinds of common titration of solution are in end liquid, and constantly stirring mixes the precipitin reaction thing simultaneously, and the rate of addition of controlling both is to keep pH between 7～9, and the precipitation suspension that obtains after titration is finished continues to stir ageing～30min.Solid-liquid separation is removed NH with the white precipitate that obtains with deionized water wash then
4 +And SO
4 2-, and repeated washing 3～5 times.With washing finish, precipitation behind the suction filtration is diluted to certain concentration (is generally 0.05mol/L～0.2mol/L), become white precipitate suspension; Select 30% H
2O
2Solution is pressed certain mol proportion (Ti as peptizing agent
4+: H
2O
2=1: 4～6) it is dripped in this suspension, constantly stir to react fully simultaneously and carry out, this moment, reactant became yellow; Peptizing agent adds the back and continue to stir 60～90min, standing and reacting liquid～24h, can obtain the finished product-light yellow, near the neutral clear solution as coating agent of photocatalysis.This coating agent can utilize metal or anti-150 ℃ non-metallic material to make base material, and the loaded photocatalyst of making promptly has visible light activity through 150 ℃ subzero treatment.
The beneficial effect of the technology of the present invention is, prepared coating agent of photocatalysis does not contain organic solvent based, and thermal treatment temp is low, and cost reduces; Apply agent near neutral, multiple base material is had good sticking power, have visible light activity.
The present invention applies agent near neutral, the 150 ℃ of crystallizableization formation anatase octahedrite phases of making on base material of filming; Optional metal of base material or anti-150 ℃ non-metallic material; Have visible light activity, the rete particle be the 10-20 nanometer spherical or～20 *～100 nanometer columns.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1:
Take by weighing the 34.6g (Ti that contains 0.1mol
4+) TiOSO
4NH
2O adds the 200ml deionized water solution, leaves standstill 8h and dissolves fully to raw material and carry out suction filtration and remove impurity and become settled solution.Get the 500ml beaker, add 200ml deionized water furnishing pH 8, with TiOSO
4Settled solution and 3mol/L ammoniacal liquor divide titration in beaker jointly, constantly stir reactant mixed, the pH that keeps reaction solution in the reaction process is about 8, the white precipitate that obtains after titration is finished stirs ageing 25min.Solid-liquid separation is used decompress filter then, and the white precipitate that obtains is removed NH with deionized water wash
4 +And SO
4 2-, and repeated washing 3 times.With washing finish, precipitation behind the suction filtration is diluted to 0.1mol/L, becomes white precipitate suspension; Select 30% H
2O
2Solution drips it in this suspension as peptizing agent 50ml, constantly stirs to react fully simultaneously and carries out, and this moment, reactant became yellow; Peptizing agent adds the back and continue to stir 60min, standing and reacting liquid 24h, can obtain the finished product-light yellow, near the neutral clear solution as coating agent of photocatalysis.This coating agent can utilize metal or anti-150 ℃ non-metallic material to make base material, and the loaded photocatalyst of making promptly has visible light activity through 150 ℃ subzero treatment.
Embodiment 2:
Take by weighing the 128.4g (Ti that contains 0.4mol
4+) TiOSO
4NH
2O adds the 200ml deionized water solution, leaves standstill 10h and dissolves fully to raw material and carry out suction filtration and remove impurity and become settled solution.Get the 500ml beaker, add 200ml deionized water furnishing pH 7.5, with TiOSO
4Settled solution and 3mol/L ammoniacal liquor divide titration in beaker jointly, constantly stir reactant mixed, the pH that keeps reaction solution in the reaction process is 7.5, the white precipitate that obtains after titration is finished stirs ageing 30min.Solid-liquid separation is used centrifugation then, and the white precipitate that obtains is removed NH with deionized water wash
4 +And SO
4 2-, and repeated washing 4 times.With washing finish, precipitation behind the suction filtration is diluted to 0.05mol/L, becomes white precipitate suspension; Select 30% H
2O
2Solution drips it in this suspension as peptizing agent 170ml, constantly stirs to react fully simultaneously and carries out, and this moment, reactant became yellow; Peptizing agent adds the back and continue to stir 80min, standing and reacting liquid 20h, can obtain the finished product-light yellow, near the neutral clear solution as coating agent of photocatalysis.This coating agent can utilize metal or anti-150 ℃ non-metallic material to make base material, and the loaded photocatalyst of making promptly has visible light activity through 150 ℃ subzero treatment.
Embodiment 3:
At first in beaker, add the TiOSO of 103.8 grams
4NH
2O (the Ti that contains 0.3mol according to purity
4+), add the 200ml deionized water solution, leave standstill 12h and dissolve fully to raw material, again this solution is carried out suction filtration and remove impurity and become settled solution.Get appropriate amount of deionized water, the certain pH of furnishing does end liquid 9, with above-mentioned TiOSO
4Settled solution and 3mol/L ammoniacal liquor (NH
3H
2O) two kinds of common titration of solution are in end liquid, and constantly stirring mixes the precipitin reaction thing simultaneously, and the rate of addition of controlling both is to keep pH 9, and the precipitation suspension that obtains after titration is finished continues to stir ageing 30min.Solid-liquid separation is used decompress filter then, and the white precipitate that obtains is removed NH with deionized water wash
4 +And SO
4 2-, and repeated washing 5 times.With washing finish, precipitation behind the suction filtration is diluted to concentration 0.2mol/L, becomes white precipitate suspension; Select 30% H
2O
2Solution 150ml drips it in this suspension as peptizing agent, constantly stirs to react fully simultaneously and carries out, and this moment, reactant became yellow; Peptizing agent adds the back and continue to stir 90min, standing and reacting liquid 24h, can obtain the finished product-light yellow, near the neutral clear solution as coating agent of photocatalysis.This coating agent can utilize metal or anti-150 ℃ non-metallic material to make base material, and the loaded photocatalyst of making promptly has visible light activity through 150 ℃ subzero treatment.
Claims (2)
1. a method for preparing the pertitanic acid coating agent of photocatalysis is characterized in that, comprises the steps:
A. earlier with TiOSO
4NH
2O makes the Ti that contains 0.1～0.5mol
4+Clear solution;
B. get an amount of pH and do end liquid, TiOSO at 7～9 deionized waters
4Settled solution and 3mol/L ammoniacal liquor (NH
3H
2O) two kinds of common titration of solution are in end liquid, constantly stir simultaneously the precipitin reaction thing is mixed, and the rate of addition of controlling both to be keeping pH between 7～9,
C. the precipitation suspension that obtains after titration is finished continues to stir ageing 20～30min,
D. solid-liquid separation is then removed NH with the white precipitate that obtains with deionized water wash
4 +And SO
4 2-, and repeated washing 3～5 times,
E. washing is finished, the dilution of the precipitation behind suction filtration 0.05mol/L～0.2mol/L, become white precipitate suspension;
F. select 30%H
2O
2Solution is as peptizing agent, in molar ratio Ti
4+: H
2O
2Drip it in above-mentioned suspension in at=1: 4～6, constantly stirs to react fully simultaneously and carry out, and this moment, reactant became yellow;
G. peptizing agent adds the back and continue to stir 60～90min, and standing and reacting liquid 20～24h can obtain the finished product: light yellow, near the neutral clear solution as coating agent of photocatalysis.
2. the method for preparing the pertitanic acid coating agent of photocatalysis according to claim 1 is characterized in that, described coating agent can utilize metal or anti-150 ℃ non-metallic material to make base material, the loaded photocatalyst of making.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100203021A CN1319642C (en) | 2004-08-11 | 2004-08-11 | Method for preparing peroxo-titanic acid photocatalytic coating agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100203021A CN1319642C (en) | 2004-08-11 | 2004-08-11 | Method for preparing peroxo-titanic acid photocatalytic coating agent |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1733846A true CN1733846A (en) | 2006-02-15 |
| CN1319642C CN1319642C (en) | 2007-06-06 |
Family
ID=36076475
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2004100203021A Expired - Fee Related CN1319642C (en) | 2004-08-11 | 2004-08-11 | Method for preparing peroxo-titanic acid photocatalytic coating agent |
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|---|---|
| CN (1) | CN1319642C (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101559979B (en) * | 2009-05-22 | 2011-04-27 | 东华大学 | Method for preparing extrafine anatase titanium dioxide nano rods |
| CN103769067A (en) * | 2013-04-15 | 2014-05-07 | 盖剑明 | Method for preparing titanium dioxide photocatalytic sol by using inorganic salt |
| CN104056610A (en) * | 2014-06-09 | 2014-09-24 | 上海荣芝蓝环保科技发展有限公司 | Method for preparing nanometer titanium dioxide photocatalyst sol |
| CN106185832A (en) * | 2016-06-30 | 2016-12-07 | 攀枝花学院 | A kind of stably-doped peroxo titanic acid sol and preparation method thereof |
| CN109336172A (en) * | 2018-10-30 | 2019-02-15 | 攀枝花学院 | The method for preparing photocatalysis nano-titanium dioxide as raw material using metatitanic acid |
| CN111151233A (en) * | 2019-12-31 | 2020-05-15 | 陕西科技大学 | Oxygen-deficient TiO2Normal temperature and pressure water phase preparation method |
| CN112961551A (en) * | 2021-03-03 | 2021-06-15 | 华中师范大学 | Titanium dioxide catalytic air purification coating and preparation method and application thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4312299B2 (en) * | 1999-05-27 | 2009-08-12 | 日揮触媒化成株式会社 | Method for producing titanium oxide fine particles containing brookite-type crystals |
| CN1194813C (en) * | 2003-03-06 | 2005-03-30 | 天津大学 | Method of preparing SnO2 cladded Tio2 nano particle photocatalyst |
-
2004
- 2004-08-11 CN CNB2004100203021A patent/CN1319642C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101559979B (en) * | 2009-05-22 | 2011-04-27 | 东华大学 | Method for preparing extrafine anatase titanium dioxide nano rods |
| CN103769067A (en) * | 2013-04-15 | 2014-05-07 | 盖剑明 | Method for preparing titanium dioxide photocatalytic sol by using inorganic salt |
| CN104056610A (en) * | 2014-06-09 | 2014-09-24 | 上海荣芝蓝环保科技发展有限公司 | Method for preparing nanometer titanium dioxide photocatalyst sol |
| CN106185832A (en) * | 2016-06-30 | 2016-12-07 | 攀枝花学院 | A kind of stably-doped peroxo titanic acid sol and preparation method thereof |
| CN109336172A (en) * | 2018-10-30 | 2019-02-15 | 攀枝花学院 | The method for preparing photocatalysis nano-titanium dioxide as raw material using metatitanic acid |
| CN111151233A (en) * | 2019-12-31 | 2020-05-15 | 陕西科技大学 | Oxygen-deficient TiO2Normal temperature and pressure water phase preparation method |
| CN111151233B (en) * | 2019-12-31 | 2022-07-08 | 陕西科技大学 | Oxygen-deficient TiO2Normal temperature and pressure water phase preparation method |
| CN112961551A (en) * | 2021-03-03 | 2021-06-15 | 华中师范大学 | Titanium dioxide catalytic air purification coating and preparation method and application thereof |
| CN112961551B (en) * | 2021-03-03 | 2022-04-05 | 华中师范大学 | Titanium dioxide catalytic air purification coating and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1319642C (en) | 2007-06-06 |
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