CN1438061A - Method for preparing porous ceramic material with titanium dioxide optical catalytic nano-coating for purifying air and water - Google Patents
Method for preparing porous ceramic material with titanium dioxide optical catalytic nano-coating for purifying air and water Download PDFInfo
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- CN1438061A CN1438061A CN 03118762 CN03118762A CN1438061A CN 1438061 A CN1438061 A CN 1438061A CN 03118762 CN03118762 CN 03118762 CN 03118762 A CN03118762 A CN 03118762A CN 1438061 A CN1438061 A CN 1438061A
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Abstract
The method for preparing titanium dioxide photocatalysis nano coating porous ceramic material for cleaning air and water includes: porous ceramic material preparation (pore size is 50-500 micrometers), preparing titanium dioxide sol and preparing high-activity TiO2 germicidal film. Said product can be used for filtration and sterilization of water and adding trace elements beneficial to health of human body, and at the same time can be used for filtration and sterilization of air.
Description
Technical field
The present invention relates to a kind of in porous ceramics the deposition of titanium oxide film, acquisition is used to purify air and the preparation method of the optically catalytic TiO 2 nano coating porous ceramic film material of water, promptly uses Prepared by Sol Gel Method optically catalytic TiO 2 nano coating porous ceramic film material preparation method.
Background technology
Along with the development of society and the raising of people's quality of life, more and more be subjected to the attention of countries in the world at aspects such as the purification of air, water treatments.The development of industrial technology has improved people's quality of life on the one hand, also environment has been caused certain pollution on the other hand, and particularly to the pollution of water and air, the quality of improving human drinking water and breathe air has unusual meaning to health.
For now, also do not have the highly effective device of a cover can carry out the cleaning and the sterilization of water and air, and can add the part trace element that human body needs.Ecological environment material nd technology of preparing and new material technology of preparing can be combined, by titanium dioxide coating photocatalytic nanometer coating in porous ceramics, be prepared into have filtration, sterilization and the device that adds trace element, be necessary to satisfy the needs that the human lives improves day by day.
Pore size by the porous ceramics in the modifier can carry out the filtration of different impurities, reasonably select the preparation material of porous ceramics, can reach the increase effect of trace elements, can make simultaneously that water and air is almost unresisted to be passed through, by being coated in the TiO2 film that has sterilizing function under the UV-irradiation, reach the purpose of sterilization, also be with a wide range of applications in industrial aspect.
Summary of the invention
The purpose of this invention is to provide a kind of simple, effective, various and suitable modern production in enormous quantities be used to purify air and the preparation method of the optically catalytic TiO 2 nano coating porous ceramic film material of water.
The object of the present invention is achieved like this: a kind ofly being used to purify air and the method for the optically catalytic TiO 2 nano coating porous ceramics modulator material of water, is the plated film matrix with the porous ceramics, comprises the steps:
(1) porous ceramics preparation;
(2) TiO 2 sol preparation;
(3) porous ceramics is adopted dip-coating method or spray-on process plated film with TiO 2 sol, carry out drying with clean hot-air then and handle;
(4) porous ceramics behind the plated film is carried out crystallization and thermal treatment;
(5) porous ceramics that plated film and crystallization and thermal treatment are crossed carries out acid treatment, washes then, uses clean hot-air drying at last, promptly makes to can be used for purifying air and the optically catalytic TiO 2 nano coating porous ceramic film material of water.
Described porous ceramics is the porous ceramics of size between 50~500 μ m in hole.
Described porous ceramics adopts the dip-coating method plated film with TiO 2 sol, and the speed that sinks to of its dipping is 20~40cm/min, time of staying 30s~30min, and pull rate is 15~35cm~min.Be no less than 30min drying time after immersion plating was finished.
The programming rate that porous ceramics behind the above-mentioned plated film carries out crystallization and thermal treatment is 10~20 ℃/min, and temperature retention time is 80~120min, and cooling rate is 10~15 ℃/min.
The used acid of above-mentioned acid treatment is any or several composite acids in sulfuric acid, sulfurous acid, hydrochloric acid, the acetate.The concentration of acid is 0.003~2M during acid treatment, soak time 5~100min, 0~60 ℃ of the temperature of acid.
Described porous ceramics prepares by following method step:
(1) being raw material with alumina powder, silica powder, carbon dust, calcium oxide powder, microcrystalline glass powder, is bond with aqueous solution of silica gel, the b propanol aqueous solution, mix according to known method in the ratio of setting, and extrusion modling, pressure is 3~6Mpa;
(2) with molding blank under 80~100 ℃ of temperature, dry 30~60min is raised to 1200 ℃ of sintering 〉=2h with 5~10 ℃/min programming rate then and gets final product.
Above-mentioned TiO 2 sol is prepared by the titanate hydrolysis, titanate is one or both combinations in positive metatitanic acid fourth fat, isopropyl titanate and the metatitanic acid second fat, the concentration of titanate is 0.001~1M, and solvent for use is one or more the combination in ethanol, isopropyl alcohol, propyl alcohol or the water.Added the complexing stabilizing agent in the TiO 2 sol, the complexing stabilizing agent is one or both the combination in triethanolamine, diethanol amine, acetate acetone, the diethylene glycol, its addition be in the colloidal sol titanium dioxide quality 0.05~10%.
The specific embodiment
The porous ceramics piece preparation method:
With ceramic raw material alumina powder, silica powder, carbon dust, calcium oxide powder, microcrystalline glass powder and bond aqueous solution of silica gel and the b propanol aqueous solution, fully mix in the ratio of setting, be squeezed into required sheet afterwards, squeeze pressure is generally 3~6Mpa (can carry out processing before the sintering in case of necessity according to required form, sintering more afterwards), mould is generally to adopt steel material.After this base substrate of extrusion modling is rising to 1200 ℃ with 5~10 ℃ of per minutes at 80~100 ℃ of drying 30~60min, keeps 2 hours in this temperature, makes it final size within desired scope.
The method for preparing the Photoactive titania film at porous ceramic surface is as follows: with the titanium alkoxide is the titanium source, the titanium alkoxide is dissolved in organic solvent such as the absolute ethyl alcohol under constantly stirring, add acetylacetone,2,4-pentanedione or other anticatalysts simultaneously, hydrolysis rate with control titanium alkoxide, stir after 2 hours, the mixture that adds alcohol and water again, allow alkoxide with suitable speed hydrolysis, (mean molecule quantity is 2000 and 4000 to the last polyethylene glycol that the adding difference is measured in above-mentioned colloidal sol, be expressed as 2000PEG and 4000PEG respectively), stir 30min, stablized, evenly, as clear as crystal yellowish orange colloidal sol.Leave standstill after 2 hours and promptly can be used for plated film.In order to allow ceramic matrix and titanium deoxid film form firm chemical bond, used ceramic matrix must clean up.Plated film can adopt dip-coating method plated film or spray-on process plated film, and earlier 100 ℃ of dryings 5~10 minutes, then 500~700 ℃ of heat treatments 1 hour, the film cool to room temperature was promptly finished the operation at the porous ceramic surface plated film to the gained gel film.
Embodiment 1
With isopropyl titanate [Ti (OC
3H
7)
4, CP] and be primary raw material, measure isopropyl titanate and absolute ethyl alcohol with graduated cylinder, the absolute ethyl alcohol amount is dissolved in isopropyl titanate in the absolute ethyl alcohol more than isopropyl titanate (volume), stirs simultaneously, makes isopropyl titanate/ethanolic solution; Then add the acetylacetone,2,4-pentanedione anticatalyst,, prevent local T iO to delay the intense hydrolysis of butyl titanate
2Separating out of precipitation; To be mixed evenly after, dropwise splashing into volume ratio again is H
2O: C
2H
5OH=1: 10 ethanol water, 1h is stirred in continuation, and (mean molecule quantity is 2000 to the last polyethylene glycol that the adding difference is measured in above-mentioned colloidal sol, be expressed as 2000PEG), thereby obtain stable, even, as clear as crystal light yellow colloidal sol, leave standstill 2h after, can be used for preparing TiO
2Film, wherein the chemical composition mol ratio of precursor sol liquid is Ti (OC
4H
9)
4: C
2H
5OH: H
2O: (CH
3CO)
2CH
2=1: 26.5: 1: 1; Polyethylene glycol is TiO in the colloidal sol
2Quality 25%.Used ceramic matrix is clean aluminium oxide ceramics.Its film plating process is for immersing the ceramic substrate of cleaning in the above-mentioned colloidal sol for preparing, leave standstill 10 seconds after, with 4mms
-1Pull rate lift vertically upward, then substrate is put into 100 ℃ dry 10 minutes of drying box, at last substrate is placed 600 ℃ muffle furnace heat treatment 2h, take out and promptly obtain TiO
2Film.Repeat aforesaid operations, can obtain the film of different-thickness.TiO in above-mentioned ceramic matrix surface preparation
2Film is a porous, has bigger specific area, helps the raising of photocatalytic activity.
Claims (10)
1, a kind ofly being used to purify air and the method for the optically catalytic TiO 2 nano coating porous ceramics modulator material of water, is the plated film matrix with the porous ceramics, it is characterized in that step is as follows:
(1) porous ceramics preparation;
(2) TiO 2 sol preparation;
(3) porous ceramics is adopted dip-coating method or spray-on process plated film with TiO 2 sol, carry out drying with clean hot-air then and handle;
(4) porous ceramics behind the plated film is carried out crystallization and thermal treatment;
(5) porous ceramics that plated film and crystallization and thermal treatment are crossed carries out acid treatment, washes then, uses clean hot-air drying at last, promptly makes to can be used for purifying air and the optically catalytic TiO 2 nano coating porous ceramics of water.
2, by the described method of claim 1, it is characterized in that described porous ceramics is the porous ceramics of size between 50~500 μ m in hole.
3, by the described method of claim 1, it is characterized in that described porous ceramics adopts the dip-coating method plated film with TiO 2 sol, the speed that sinks to of its dipping is 20~40cm/min, time of staying 30s~30min, pull rate is 15~35cm/min.
4, by the described method of claim 1, it is characterized in that the drying after the described immersion plating, be no less than 30min its drying time.
5, by the described method of claim 1, it is characterized in that the programming rate that described porous ceramics carries out crystallization and thermal treatment is 10~20 ℃/min, temperature retention time is 80~120min, cooling rate is 10~15 ℃/min.
6,, it is characterized in that the used acid of described acid treatment is any or several composite acids in sulfuric acid, sulfurous acid, hydrochloric acid, the acetate by the described method of claim 1.
7, by the described method of claim 1, the concentration of acid is 0.003~2M when it is characterized in that acid treatment, soak time 5~100min, 0~60 ℃ of the temperature of acid.
8, the preparation method of the described porous ceramics of claim 1 is characterized in that preparation process is::
(1) being raw material with alumina powder, silica powder, carbon dust, calcium oxide powder, microcrystalline glass powder, is bond with aqueous solution of silica gel, the b propanol aqueous solution, mixes extrusion modling according to known method in the ratio of setting;
(2) with (1) molding blank in 80~100 ℃ of temperature, dry 30~60min is raised to 1200 ℃ of sintering 〉=2h with 5~10 ℃/min programming rate then and gets final product.
9, the preparation method of the described TiO 2 sol of claim 1, it is characterized in that preparing by the titanate hydrolysis, titanate is one or both combinations in positive metatitanic acid fourth fat, isopropyl titanate and the metatitanic acid second fat, the concentration of titanate is 0.001~1M, and solvent for use is one or more the combination in ethanol, isopropyl alcohol, propyl alcohol or the water.
10, by the described method of claim 9, it is characterized in that having added in the TiO 2 sol complexing stabilizing agent, the complexing stabilizing agent is one or both the combination in triethanolamine, diethanol amine, acetate acetone, the diethylene glycol, its addition be in the colloidal sol titanium dioxide quality 0.05~10%.
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CN1312050C (en) * | 2004-10-28 | 2007-04-25 | 上海交通大学 | Method for light catalytic degrading carbamate pesticide in water |
CN1319634C (en) * | 2005-07-30 | 2007-06-06 | 大连理工大学 | Titanium dioxide nanometer pipe composite separating membrane, its preparation and use thereof |
CN100428984C (en) * | 2006-11-17 | 2008-10-29 | 大连理工大学 | Composite separating membrane of Si-doped TiO2 nanotube and its preparing method and application |
CN100439282C (en) * | 2006-06-14 | 2008-12-03 | 山东理工大学 | Prepn process of multifunctional honeycomb ceramic filter element |
CN100588447C (en) * | 2008-04-28 | 2010-02-10 | 苏州纳米技术与纳米仿生研究所 | Titania nanotube/pipe/high-efficiency glass fiber filter in situ synthesis supporting method |
CN102294167A (en) * | 2007-04-19 | 2011-12-28 | 雅高思先进科技有限公司 | A method and apparatus for fluid purification |
CN101565329B (en) * | 2009-05-27 | 2012-07-04 | 福州大学 | Method for producing photocatalysis ceramics with adjustable surface gloss |
CN103482960A (en) * | 2013-09-06 | 2014-01-01 | 鞍山仕普瑞科技有限公司 | Light-activated high-activity nanometer ceramic chip with multidimensional structure and preparation method thereof |
CN103586090A (en) * | 2013-01-07 | 2014-02-19 | 刘绍川 | Preparation method for air and water purification material |
CN104117347A (en) * | 2013-04-28 | 2014-10-29 | 浙江高明玻璃有限公司 | Preparation method of modified nano-titanium dioxide film |
CN104436860A (en) * | 2014-12-31 | 2015-03-25 | 安徽省元琛环保科技有限公司 | Copper fiber filter screen for load photocatalyst and manufacturing method thereof |
CN105439350A (en) * | 2015-12-08 | 2016-03-30 | 黄荣贵 | Breathing gas and drinking water shared purifying device |
CN105439340A (en) * | 2015-12-08 | 2016-03-30 | 黄荣贵 | External respiratory air and drinking water alternate purification method |
CN105540961A (en) * | 2015-12-08 | 2016-05-04 | 黄荣贵 | Method for co-purifying external breathing air and drinking water |
CN107841670A (en) * | 2017-11-02 | 2018-03-27 | 裴寿益 | A kind of ceramics and its manufacture method |
CN107986327A (en) * | 2017-12-18 | 2018-05-04 | 苏州中科纳福材料科技有限公司 | The preparation method of titanium dioxide nano-film |
CN109482241A (en) * | 2018-12-07 | 2019-03-19 | 怀化学院 | TiO2/ MOF-5 photochemical catalyst and preparation method thereof |
CN113185328A (en) * | 2020-01-14 | 2021-07-30 | 顾明 | Production process of nano microcrystalline film photocatalytic ceramic |
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2003
- 2003-03-11 CN CN 03118762 patent/CN1206015C/en not_active Expired - Fee Related
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CN1312050C (en) * | 2004-10-28 | 2007-04-25 | 上海交通大学 | Method for light catalytic degrading carbamate pesticide in water |
CN1319634C (en) * | 2005-07-30 | 2007-06-06 | 大连理工大学 | Titanium dioxide nanometer pipe composite separating membrane, its preparation and use thereof |
CN100439282C (en) * | 2006-06-14 | 2008-12-03 | 山东理工大学 | Prepn process of multifunctional honeycomb ceramic filter element |
CN100428984C (en) * | 2006-11-17 | 2008-10-29 | 大连理工大学 | Composite separating membrane of Si-doped TiO2 nanotube and its preparing method and application |
CN102294167A (en) * | 2007-04-19 | 2011-12-28 | 雅高思先进科技有限公司 | A method and apparatus for fluid purification |
CN102294167B (en) * | 2007-04-19 | 2014-04-02 | 雅高思先进科技有限公司 | A method and apparatus for fluid purification |
CN100588447C (en) * | 2008-04-28 | 2010-02-10 | 苏州纳米技术与纳米仿生研究所 | Titania nanotube/pipe/high-efficiency glass fiber filter in situ synthesis supporting method |
CN101565329B (en) * | 2009-05-27 | 2012-07-04 | 福州大学 | Method for producing photocatalysis ceramics with adjustable surface gloss |
CN103586090A (en) * | 2013-01-07 | 2014-02-19 | 刘绍川 | Preparation method for air and water purification material |
CN104117347A (en) * | 2013-04-28 | 2014-10-29 | 浙江高明玻璃有限公司 | Preparation method of modified nano-titanium dioxide film |
CN103482960A (en) * | 2013-09-06 | 2014-01-01 | 鞍山仕普瑞科技有限公司 | Light-activated high-activity nanometer ceramic chip with multidimensional structure and preparation method thereof |
CN103482960B (en) * | 2013-09-06 | 2015-03-04 | 鞍山奇典生态科技研究所有限公司 | Light-activated high-activity nanometer ceramic chip with multidimensional structure and preparation method thereof |
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CN107986327B (en) * | 2017-12-18 | 2019-11-15 | 苏州中科纳福材料科技有限公司 | The preparation method of titanium dioxide nano-film |
CN109482241A (en) * | 2018-12-07 | 2019-03-19 | 怀化学院 | TiO2/ MOF-5 photochemical catalyst and preparation method thereof |
CN109482241B (en) * | 2018-12-07 | 2021-08-17 | 怀化学院 | TiO2/MOF-5 photocatalyst and preparation method thereof |
CN113185328A (en) * | 2020-01-14 | 2021-07-30 | 顾明 | Production process of nano microcrystalline film photocatalytic ceramic |
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