CN101406834A - Method for preparing silver and titanic oxide nano compound material at low temperature - Google Patents
Method for preparing silver and titanic oxide nano compound material at low temperature Download PDFInfo
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- CN101406834A CN101406834A CNA2008101222244A CN200810122224A CN101406834A CN 101406834 A CN101406834 A CN 101406834A CN A2008101222244 A CNA2008101222244 A CN A2008101222244A CN 200810122224 A CN200810122224 A CN 200810122224A CN 101406834 A CN101406834 A CN 101406834A
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Abstract
The invention discloses a method for preparing a silver and titanium dioxide nano-composite at low temperature. The method comprises the following steps: (1) a titanium compound is dissolved in an organic solvent, so as to obtain an A solution; (2) the A solution is dripped into water gradually and stirred to form stable sol, so as to obtain a B solution; (3) a silver compound and diethanolameine are dissolved in the organic solvent, so as to obtain a C solution; and (4) the C solution and the B solution are mixed, aged and dried. The method has the advantages that the method is simple, needs no special device or high temperature condition, and can obtain the silver and titanium dioxide nano-composite at low temperature. In the prepared silver and titanium dioxide nano-composite, the size of silver particles is between 5 and 40 nanometers, and the size of titanium dioxide particles is between 4 and 6 nanometers. The composite has excellent properties in photocatalysis, deodorization and sterilization.
Description
Technical field
The present invention relates to the method that a kind of low temperature prepares silver and titanic oxide nano compound material.
Background technology
Metal-oxide semiconductor (MOS) titanium dioxide (TiO
2) be semiconductor material with wide forbidden band, energy gap is about 3.2～3.41eV, and is transparent in 0.35～12 mum wavelength interval, the refractive index height, and have characteristic of mechanical property height, stable chemical performance or the like.TiO at the ultraviolet light wave band
2Has photocatalysis characteristic, at numerous photochemical catalyst (TiO
2, ZnO, Fe
2O
3, CdS etc.) in, TiO
2Nontoxic with it, catalytic activity is high, good stability, characteristics such as cheap and easy to get are subject to people's attention.Metal energy and TiO
2Constitute composite photo-catalyst, metal is at metal/TiO
2Effect in the composite is the ultra-voltage that separates and reduce reduction reaction (reduction of proton, the reduction of dissolved oxygen) that helps light induced electron and hole, improves the activity of photochemical catalyst greatly, precious metals ag doped Ti O
2Be current TiO
2A focus in the study on the modification.There are some researches show, at TiO
2An amount of Ag of middle adding forms nanometer Ag/TiO
2Composite can significantly improve its photo-catalysis capability.
But obtain the Ag/TiO of crystalline state
2Composite in the preparation process of material, must pass through the heat treatment that is not less than 350 ℃.High-temperature heat treatment has limited Ag/TiO
2The application of composite on environment that can not experience high-temperature heat treatment and matrix.So, if can under low temperature even normal temperature, prepare Ag/TiO
2Composite all has important meaning for photocatalysis performance or other performance of the titanium dioxide of the compound silver of research.
Summary of the invention
The purpose of this invention is to provide the method that a kind of low temperature prepares silver and titanic oxide nano compound material.This
The low temperature of invention prepares the method for silver and titanic oxide nano compound material, and step is as follows:
1) titanium compound is dissolved in the organic solvent, gets A liquid, the mol ratio of organic solvent and titanium compound is greater than 2;
2) A liquid is dropwise splashed in the water, the mol ratio of water and titanium compound is greater than 20, and the pH value of regulator solution stirs up to forming stable sols to less than 7, gets B liquid;
3) compound and the diethanol amine with silver is 1 in molar ratio: 1-10 is dissolved in the organic solvent, gets C liquid, and the mol ratio of the compound of organic solvent and silver is greater than 6, and the compound of silver and the mol ratio of titanium compound are 0.001-0.3;
4) C liquid is mixed with B liquid, 50-200 ℃ of drying, obtain silver and titanic oxide nano compound material after the ageing.
The compound of above-mentioned titanium can be butyl titanate, titanium chloride or isopropyl titanate.Said organic solvent can be one or more in ethanol, propyl alcohol, ethylene glycol, propane diols, oxolane, acetone and the butanols.The compound of said silver can be silver nitrate or silver chlorate.
Beneficial effect of the present invention is:
Preparation method of the present invention is simple, need not special device and hot conditions, can obtain silver and titanic oxide nano compound material under cryogenic conditions.In the silver and titanic oxide nano compound material that makes, silver-colored particle size 5-40 nanometer, the titanium dioxide granule size is about the 4-6 nanometer.This composite has excellent photocatalysis, deodorizing, bactericidal property.
Description of drawings
Fig. 1 is the X ray diffracting spectrum of silver and titanic oxide nano compound material.
Fig. 2 is the transmission electron microscope photo of silver and titanic oxide nano compound material.
The specific embodiment
Further specify the present invention below in conjunction with instantiation.
Embodiment 1
1) butyl titanate is dissolved in the ethanol, the mol ratio of butyl titanate and ethanol is 1: 6, obtains A liquid;
2) A liquid is dropwise splashed in the water, the mol ratio of water and butyl titanate is 40, with the pH value to 3 of nitric acid regulator solution, stirs up to forming stable sols, gets B liquid;
3) diethanol amine with silver nitrate and equivalent is dissolved in the ethanol, gets C liquid, and the mol ratio of ethanol and silver nitrate is 12, and the mol ratio of silver nitrate and butyl titanate is 0.1;
4) C liquid is mixed with B liquid, 50 ℃ of dryings, obtain silver and titanic oxide nano compound material after the ageing.
The silver that makes and the X ray diffracting spectrum of titanic oxide nano compound material as shown in Figure 1, titanium dioxide is made up of anatase and brockite, silver exists with the zeroth order silver of face-centred cubic structure.The silver and the transmission electron microscope photo of titanic oxide nano compound material as shown in Figure 2, the particle size of titanium dioxide is about 5 nanometers, the size 10-20 nanometer of silver-colored particle.
Embodiment 2
1) isopropyl titanate is dissolved in the ethylene glycol, the mol ratio of isopropyl titanate and ethylene glycol is 1: 5, obtains A liquid;
2) A liquid is dropwise splashed in the water, the mol ratio of water and isopropyl titanate is 100, with the pH value to 2 of nitric acid regulator solution, stirs up to forming stable sols, gets B liquid;
3) be to be dissolved in ethylene glycol at 1: 4 in molar ratio with silver nitrate and diethanol amine, C liquid, the mol ratio of ethylene glycol and silver nitrate is 10, the mol ratio of silver nitrate and isopropyl titanate is 0.001;
4) C liquid is mixed with B liquid, 100 ℃ of dryings, obtain silver and titanic oxide nano compound material after the ageing.
The size of prepared titanium dioxide crystal is about 6 nanometers, the size 4-10 nanometer of silver-colored particle.
Embodiment 3
1) titanium chloride is dissolved in the propyl alcohol, the mol ratio of titanium chloride and propyl alcohol is 1: 10, obtains A liquid;
2) A liquid is dropwise splashed in the water, the mol ratio of water and titanium chloride is 200, with the pH value to 4 of hydrochloric acid conditioning solution, stirs up to forming stable sols, gets B liquid;
3) be to be dissolved in propyl alcohol at 1: 8 in molar ratio with silver chlorate and diethanol amine, C liquid, the mol ratio of propyl alcohol and silver chlorate is 20, the mol ratio of silver chlorate and titanium chloride is 0.3;
4) C liquid is mixed with B liquid, 150 ℃ of dryings, obtain silver and titanic oxide nano compound material after the ageing.
The size of prepared titanium dioxide crystal is about 4 nanometers, the size 15-40 nanometer of silver-colored particle.
Claims (4)
1. a low temperature prepares the method for silver and titanic oxide nano compound material, it is characterized in that may further comprise the steps:
1) titanium compound is dissolved in the organic solvent, gets A liquid, the mol ratio of organic solvent and titanium compound is greater than 2;
2) A liquid is dropwise splashed in the water, the mol ratio of water and titanium compound is greater than 20, and the pH value of regulator solution stirs up to forming stable sols to less than 7, gets B liquid;
3) compound and the diethanol amine with silver is 1 in molar ratio: 1-10 is dissolved in the organic solvent, gets C liquid, and the mol ratio of the compound of organic solvent and silver is greater than 6, and the compound of silver and the mol ratio of titanium compound are 0.001-0.3;
4) C liquid is mixed with B liquid, 50-200 ℃ of drying, obtain silver and titanic oxide nano compound material after the ageing.
2. low temperature according to claim 1 prepares the method for silver and titanic oxide nano compound material, and the compound that it is characterized in that said titanium is butyl titanate, titanium chloride or isopropyl titanate.
3. low temperature according to claim 1 prepares the method for silver and titanic oxide nano compound material, it is characterized in that said organic solvent is one or more in ethanol, propyl alcohol, ethylene glycol, propane diols, oxolane, acetone and the butanols.
4. low temperature according to claim 1 prepares the method for silver and titanic oxide nano compound material, and the compound that it is characterized in that said silver is silver nitrate or silver chlorate.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2008101222244A CN101406834B (en) | 2008-11-04 | 2008-11-04 | Method for preparing silver and titanic oxide nano compound material at low temperature |
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| CN2008101222244A CN101406834B (en) | 2008-11-04 | 2008-11-04 | Method for preparing silver and titanic oxide nano compound material at low temperature |
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| CN101406834A true CN101406834A (en) | 2009-04-15 |
| CN101406834B CN101406834B (en) | 2010-07-07 |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101613556B (en) * | 2009-07-16 | 2011-09-14 | 浙江大学 | Preparation method of titanium silver-based antimildew and antibacterial emulsion paint interior wall paint |
| CN102513103A (en) * | 2011-11-14 | 2012-06-27 | 浙江大学 | Preparation method of surfactant for photo-reduction method of Ag/TiO2 nano heterogenous junction by virtue of induction |
| CN103240084A (en) * | 2013-05-10 | 2013-08-14 | 天津大学 | Titanium dioxide-silver nano-composite material and synthetic method thereof |
| CN104722296A (en) * | 2015-04-02 | 2015-06-24 | 东北林业大学 | Method for preparing Ag-TiO2 compound photocatalyst at low temperature |
| CN106679307A (en) * | 2016-12-28 | 2017-05-17 | 青岛海尔股份有限公司 | Panel, refrigerator with sterilization inner container and manufacturing method for sterilization inner container |
| CN107774286A (en) * | 2017-09-29 | 2018-03-09 | 郑州爱可安环保技术有限公司 | A kind of method of low temperature preparation composite photo-catalyst |
| WO2018121509A1 (en) * | 2016-12-30 | 2018-07-05 | 苏州律点信息科技有限公司 | Formaldehyde adsorbing building coating |
| CN113786831A (en) * | 2021-09-10 | 2021-12-14 | 上海电力大学 | Amorphous TiO2Ag/composite nano-particle and preparation method and application thereof |
| CN113970582A (en) * | 2021-10-18 | 2022-01-25 | 嘉兴学院 | Whole-course mild preparation method of flexible ammonia gas sensor and ammonia gas sensor |
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2008
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101613556B (en) * | 2009-07-16 | 2011-09-14 | 浙江大学 | Preparation method of titanium silver-based antimildew and antibacterial emulsion paint interior wall paint |
| CN102513103A (en) * | 2011-11-14 | 2012-06-27 | 浙江大学 | Preparation method of surfactant for photo-reduction method of Ag/TiO2 nano heterogenous junction by virtue of induction |
| CN102513103B (en) * | 2011-11-14 | 2013-11-13 | 浙江大学 | Preparation method of surfactant for photo-reduction method of Ag/TiO2 nano heterogenous junction by virtue of induction |
| CN103240084A (en) * | 2013-05-10 | 2013-08-14 | 天津大学 | Titanium dioxide-silver nano-composite material and synthetic method thereof |
| CN104722296A (en) * | 2015-04-02 | 2015-06-24 | 东北林业大学 | Method for preparing Ag-TiO2 compound photocatalyst at low temperature |
| CN106679307A (en) * | 2016-12-28 | 2017-05-17 | 青岛海尔股份有限公司 | Panel, refrigerator with sterilization inner container and manufacturing method for sterilization inner container |
| CN106679307B (en) * | 2016-12-28 | 2019-05-31 | 青岛海尔股份有限公司 | A kind of plate, the refrigerator with sterilization liner and the production method for sterilizing liner |
| WO2018121509A1 (en) * | 2016-12-30 | 2018-07-05 | 苏州律点信息科技有限公司 | Formaldehyde adsorbing building coating |
| CN107774286A (en) * | 2017-09-29 | 2018-03-09 | 郑州爱可安环保技术有限公司 | A kind of method of low temperature preparation composite photo-catalyst |
| CN113786831A (en) * | 2021-09-10 | 2021-12-14 | 上海电力大学 | Amorphous TiO2Ag/composite nano-particle and preparation method and application thereof |
| CN113970582A (en) * | 2021-10-18 | 2022-01-25 | 嘉兴学院 | Whole-course mild preparation method of flexible ammonia gas sensor and ammonia gas sensor |
| CN113970582B (en) * | 2021-10-18 | 2023-07-21 | 嘉兴学院 | Whole-course mild preparation method of flexible ammonia sensor and ammonia sensor |
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| Publication number | Publication date |
|---|---|
| CN101406834B (en) | 2010-07-07 |
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Application publication date: 20090415 Assignee: Weihai Blue Star Glass Group Co., Ltd. Assignor: Zhejiang University Contract record no.: 2013330000090 Denomination of invention: Method for preparing silver and titanic oxide nano compound material at low temperature Granted publication date: 20100707 License type: Common License Record date: 20130422 |
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