CN1934954A - Method for preparing nano Ag/TiO2 composite material - Google Patents

Method for preparing nano Ag/TiO2 composite material Download PDF

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CN1934954A
CN1934954A CNA2006101047119A CN200610104711A CN1934954A CN 1934954 A CN1934954 A CN 1934954A CN A2006101047119 A CNA2006101047119 A CN A2006101047119A CN 200610104711 A CN200610104711 A CN 200610104711A CN 1934954 A CN1934954 A CN 1934954A
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solution
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ammonia
deionized water
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CN100442983C (en
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杨辉
张�林
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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Abstract

The present invention relates to a preparation method of nano Ag/TiO2 composite material. Said method includes the following steps: firstly, dissolving AgNO3 in ammonia solution to obtain AgNO3 ammonia solution; dissolving Ti(SO4)2 in deionized water to obtain Ti(SO4)2 solution; adding the AgNO3 ammonia solution into the Ti(SO4)2 solution to obtain white colloidal solution; heating said colloidal solution to 90-100 deg.C, keeping constant temperature for 2h, standing still for 12-24 h at 50-60 deg.C, vacuum filtering and washing by using deionized water to remove SO42-ions, drying at 90 deg.C for 20-24h, grinding to obtain powder body, treating at 500-600 deg.C for 2h, cooling so as to obtain the invented product.

Description

A kind of nanometer Ag/TiO 2The preparation method of composite
Technical field
The present invention relates to a kind of nano-TiO 2The preparation method of composite is specifically related to a kind of nanometer Ag/TiO 2The preparation method of composite.
Background technology
The TiO of anatase phase 2It is material with photocatalysis characteristic, it utilizes the ultraviolet light in sunshine, the fluorescent lamp to make excitaton source and have antimicrobial effect, action effect is lasting, and have purify air, dispose of sewage, from photocatalytic effects such as cleanings, the prerequisite of its realization is exciting of ultraviolet light, so, in the occasion that does not have ultraviolet light to exist, even the TiO of anatase phase 2Also do not have antibiotic effect, in order to address this problem, the metal ion that normally will have antibacterial action is written into wherein.That antibiotic property is best in metal ion is Ag +, it has characteristics such as broad-spectrum antibacterial property is good, germicidal efficiency is high, be difficult for developing immunity to drugs, Ag +Also has activation TiO 2The effect of catalytic activity, broadening TiO 2To ultraviolet absorption region, therefore, nano silver-carrying composite titania material (Ag/TiO 2) be desirable anti-biotic material, moreover, this material is expected to the process that catalysis photodissociation water becomes hydrogen and oxygen, and its preparation is one of focus of present people's research.
The preparation method of nano silver-carrying composite titania material mainly contains: solid-phase synthesis, continuous acid-hydrolysis method and acid hydrolysis secondary precipitation, photo-reduction sedimentation, sol-gal process, microwave drying etc. (referring to: Liu Qingju, Zhang Jin, Zhu Zhongqi etc.Carry silver-colored TiO 2The preparation and property research of inorganic antiseptic.Functional material.2005.3 (36): 474～476; Ma Dengfeng, Peng Bing, Chai Liyuan etc.The Study on Preparation of Ag-carried nanometer titanium dioxide antimicrobial powder.Fine-chemical intermediate.2006.2,36 (1): 63～66; Huang Yueyuan, Mi Yu, Guo Renmin etc.TiO 2The research of base composite nano germicide.Chemical Engineering.2004.8,32 (4): 46～48; Huang Yueyuan, Mi Yu, Guo Renmin etc.TiO 2/ Ag nano anti-biotic material.Northwest University's journal (natural science edition) 2003.10,33 (5): 566～571; Liu Xuefeng is coated with an inscription ancient type of banner hoisted on a featherdecked mast.The development of rare earth loaded type nano titanium dioxide anti-bacterial agent.Modern chemical industry.2005.7,145～147; Liu Xuefeng, Zhang Li is coated with an inscription ancient type of banner hoisted on a featherdecked mast.Nano Ce/TiO 2The preparation of inorganic antiseptic and performance evaluation thereof.The process engineering journal.2004.6,4 (3): 256～260; Han Qing profit 1, gold is revitalized, Huang Hongyan.Microwave drying prepares Ag/TiO 2The photocatalytic activity experimental study.Environmental protection science.2005.10,31 (131): 6～12; Zhang Fuxiang, Zhang Xiu, Chen Jixin etc.Ag/TiO 2The preparation of composite nano-catalyst and sign and photocatalytic activity thereof.The catalysis journal.2003.11,24 (11): 887～880; Zhao Gaoling, Han Gaorong.The Prepared by Sol Gel Method of Nano silver grain P titania coextruded film and the research of optical property thereof.Materials Science and Engineering.2001,19 (1): 21～25; What advances, Chen Xingbi, Yang Chuanren.TiO 2(Ag) preparation of Nano semiconductor film and photocatalysis performance thereof.Electronic component and material.1999,2:13～17; Wang Zhiqun.Compound silver series inorganic germifuge.The number of applying for a patent: 98111623.X; A kind of dichloride in anatase type TiO 2Composite inorganic antimicrobial agent and preparation method thereof.The number of applying for a patent: 200410081239.2), the basic preparation process of these methods was divided into for two steps: being written into of the preparation of nano-titanium dioxide powder and silver ion.The a large amount of acid of hydrolytic process consumption in the preparation also need be dissolved metatitanic acid down at 125 ℃ to continuous hydrolysis process, and the operational process of craft complexity is wayward, the production cost height.
Summary of the invention
The objective of the invention is to overcome the shortcoming of above-mentioned prior art, provide a kind of preparation technology simple, easy to operate, pollute few, and have strong antibiotic property, do not having the ultraviolet ray excited nanometer Ag/TiO that still has antibiotic property down 2The preparation method of composite.
For achieving the above object, the preparation method that the present invention adopts is: at first being 25% ammoniacal liquor and deionized water with mass concentration is mixed and made into ammonia spirit by 1: 1 volume ratio, then with AgNO 3Be dissolved in and make the AgNO that concentration is 0.001～0.01mol/L in the ammonia spirit 3Ammonia solution; Secondly with Ti (SO 4) 2Be dissolved in the deionized water, being mixed with concentration is the Ti (SO of 0.02～0.2mol/L 4) 2Solution; Under 40～60 ℃ of stirrings, press AgNO 3Ammonia solution and Ti (SO 4) 2Solution is that 1: 1～1: 1.5 volume ratio is with AgNO 3Ammonia solution stream is added to Ti (SO 4) 2In the solution or with Ti (SO 4) 2Flow of solution is added to AgNO 3In the ammonia solution, obtain the white size liquid solution; Continue to stir and gained colloidal solution is warming up to 90～100 ℃, constant temperature 2 hours leaves standstill 12～24h with colloidal solution in 50～60 ℃ again; Vacuum filtration is also removed SO through deionized water washing 4 2-Behind the ion, behind 90 ℃ of drying 20～24h, be ground to powder; Above-mentioned gained powder in 500～600 ℃ of processing 2h, is got final product with the stove cooling.
The present invention is simple to operate, does not need the acid hydrolysis process, and consumption acids not pollutes for a short time, with low cost, is easy to suitability for industrialized production; The gained material is the nano silver-carrying composite titania material, particle size 4～5nm, and main crystal consists of Detitanium-ore-type TiO 2, have photocatalysis, because Ag +Existence, its catalytic activity is higher; There is not the ultraviolet ray excited strong bactericidal action that still has down.
Embodiment
Embodiment 1, and at first being 25% ammoniacal liquor and deionized water with mass concentration is mixed and made into ammonia spirit by 1: 1 volume ratio, then with AgNO 3Be dissolved in and make the AgNO that concentration is 0.001mol/L in the ammonia spirit 3Ammonia solution; Secondly with Ti (SO 4) 2Be dissolved in the deionized water, being mixed with concentration is the Ti (SO of 0.02mol/L 4) 2Solution; Under 60 ℃ of stirrings, press AgNO 3Ammonia solution and Ti (SO 4) 2Solution is that 1: 1 volume ratio is with AgNO 3Ammonia solution stream is added to Ti (SO 4) 2In the solution or with Ti (SO 4) 2Flow of solution is added to AgNO 3In the ammonia solution, obtain the white size liquid solution; Continue to stir and gained colloidal solution is warming up to 90 ℃, constant temperature 2 hours leaves standstill 24h with colloidal solution in 50 ℃ again; Vacuum filtration is also removed SO through deionized water washing 4 2-Behind the ion, behind 90 ℃ of dry 24h, be ground to powder; Above-mentioned gained powder in 600 ℃ of processing 2h, with the stove cooling, is obtained nanometer Ag/TiO 2, wherein main crystal composition is Detitanium-ore-type TiO 2
Embodiment 2, and at first being 25% ammoniacal liquor and deionized water with mass concentration is mixed and made into ammonia spirit by 1: 1 volume ratio, then with AgNO 3Be dissolved in and make the AgNO that concentration is 0.003mol/L in the ammonia spirit 3Ammonia solution; Secondly with Ti (SO 4) 2Be dissolved in the deionized water, being mixed with concentration is the Ti (SO of 0.05mol/L 4) 2Solution; Under 45 ℃ of stirrings, press AgNO 3Ammonia solution and Ti (SO 4) 2Solution is that 1: 1.5 volume ratio is with AgNO 3Ammonia solution stream is added to Ti (SO 4) 2In the solution or with Ti (SO 4) 2Flow of solution is added to AgNO 3In the ammonia solution, obtain the white size liquid solution; Continue to stir and gained colloidal solution is warming up to 98 ℃, constant temperature 2 hours leaves standstill 18h with colloidal solution in 55 ℃ again; Vacuum filtration is also removed SO through deionized water washing 4 2-Behind the ion, behind 90 ℃ of dry 22h, be ground to powder; Above-mentioned gained powder in 500 ℃ of processing 2h, with the stove cooling, is obtained nanometer Ag/TiO 2, wherein main crystal composition is Detitanium-ore-type TiO 2
Embodiment 3, and at first being 25% ammoniacal liquor and deionized water with mass concentration is mixed and made into ammonia spirit by 1: 1 volume ratio, then with AgNO 3Be dissolved in and make the AgNO that concentration is 0.006mol/L in the ammonia spirit 3Ammonia solution; Secondly with Ti (SO 4) 2Be dissolved in the deionized water, being mixed with concentration is the Ti (SO of 0.1mol/L 4) 2Solution; Under 55 ℃ of stirrings, press AgNO 3Ammonia solution and Ti (SO 4) 2Solution is that 1: 1.2 volume ratio is with AgNO 3Ammonia solution stream is added to Ti (SO 4) 2In the solution or with Ti (SO 4) 2Flow of solution is added to AgNO 3In the ammonia solution, obtain the white size liquid solution; Continue to stir and gained colloidal solution is warming up to 93 ℃, constant temperature 2 hours leaves standstill 15h with colloidal solution in 58 ℃ again; Vacuum filtration is also removed SO through deionized water washing 4 2-Behind the ion, behind 90 ℃ of dry 21h, be ground to powder; Above-mentioned gained powder in 550 ℃ of processing 2h, with the stove cooling, is obtained nanometer Ag/TiO 2, wherein main crystal composition is Detitanium-ore-type TiO 2
Embodiment 4, and at first being 25% ammoniacal liquor and deionized water with mass concentration is mixed and made into ammonia spirit by 1: 1 volume ratio, then with AgNO 3Be dissolved in and make the AgNO that concentration is 0.008mol/L in the ammonia spirit 3Ammonia solution; Secondly with Ti (SO 4) 2Be dissolved in the deionized water, being mixed with concentration is the Ti (SO of 0.16mol/L 4) 2Solution; Under 40 ℃ of stirrings, press AgNO 3Ammonia solution and Ti (SO 4) 2Solution is that 1: 1.4 volume ratio is with AgNO 3Ammonia solution stream is added to Ti (SO 4) 2In the solution or with Ti (SO 4) 2Flow of solution is added to AgNO 3In the ammonia solution, obtain the white size liquid solution; Continue to stir and gained colloidal solution is warming up to 95 ℃, constant temperature 2 hours leaves standstill 22h with colloidal solution in 53 ℃ again; Vacuum filtration is also removed SO through deionized water washing 4 2-Behind the ion, behind 90 ℃ of dry 23h, be ground to powder; Above-mentioned gained powder in 570 ℃ of processing 2h, with the stove cooling, is obtained nanometer Ag/TiO 2, wherein main crystal composition is Detitanium-ore-type TiO 2
Embodiment 5, and at first being 25% ammoniacal liquor and deionized water with mass concentration is mixed and made into ammonia spirit by 1: 1 volume ratio, then with AgNO 3Be dissolved in and make the AgNO that concentration is 0.01mol/L in the ammonia spirit 3Ammonia solution; Secondly with Ti (SO 4) 2Be dissolved in the deionized water, being mixed with concentration is the Ti (SO of 0.2mol/L 4) 2Solution; Under 50 ℃ of stirrings, press AgNO 3Ammonia solution and Ti (SO 4) 2Solution is that 1: 1.1 volume ratio is with AgNO 3Ammonia solution stream is added to Ti (SO 4) 2In the solution or with Ti (SO 4) 2Flow of solution is added to AgNO 3In the ammonia solution, obtain the white size liquid solution; Continue to stir and gained colloidal solution is warming up to 100 ℃, constant temperature 2 hours leaves standstill 12h with colloidal solution in 60 ℃ again; Vacuum filtration is also removed SO through deionized water washing 4 2-Behind the ion, behind 90 ℃ of dry 20h, be ground to powder; Above-mentioned gained powder in 520 ℃ of processing 2h, with the stove cooling, is obtained nanometer Ag/TiO 2, wherein main crystal composition is Detitanium-ore-type TiO 2
The present invention passes through AgNO 3Ammonia solution provides the precipitating reagent of precipitated titanium ion simultaneously for composite provides silver, is to realize synthetic key substance of a step; Under stirring condition the mixing of two kinds of solution guaranteed uniformity, the degree of supersaturation when having controlled precipitation and the growth of crystal; Being warmed up to 90～100 ℃ after the mixing is the pH value that volatilization removes ammonia, reduction solution with stirring main purpose, makes Ag +Enter into TiO by ion exchange or absorption 2In the crystal; Leave standstill and to make crystal more complete; Powder is to obtain the TiO of Detitanium-ore-type in 500～600 ℃ of processing intents 2Crystal.The present invention adopts Ti (SO 4) 2As raw material, the nano-TiO used with present solid-phase synthesis, continuous acid-hydrolysis method etc. 2Or metatitanic acid compares, and its low price can make production cost greatly reduce, owing to there is not the acid hydrolysis process not only can reduce cost but also can reduce acid pollution.Product of the present invention namely can be used as strong antiseptic and is applied to a plurality of fields, and the while is used for the production field of environmental protection and clear energy sources etc. as strong catalysis material.

Claims (6)

1, a kind of nanometer Ag/TiO 2The preparation method of composite is characterized in that:
1) at first being 25% ammoniacal liquor and deionized water with mass concentration is mixed and made into ammonia spirit by 1: 1 volume ratio, then with AgNO 3Be dissolved in and make the AgNO that concentration is 0.001～0.01mol/L in the ammonia spirit 3Ammonia solution;
2) secondly with Ti (SO 4) 2Be dissolved in the deionized water, being mixed with concentration is the Ti (SO of 0.02～0.2mol/L 4) 2Solution;
3) under 40～60 ℃ of stirrings, press AgNO 3Ammonia solution and Ti (SO 4) 2Solution is that 1: 1～1: 1.5 volume ratio is with AgNO 3Ammonia solution stream is added to Ti (SO 4) 2In the solution or with Ti (SO 4) 2Flow of solution is added to AgNO 3In the ammonia solution, obtain the white size liquid solution;
4) continue to stir and gained colloidal solution is warming up to 90～100 ℃, constant temperature 2 hours leaves standstill 12～24h with colloidal solution in 50～60 ℃ again;
5) vacuum filtration and remove SO through deionized water washing 4 2-Behind the ion, behind 90 ℃ of drying 20～24h, it is ground is powder;
6) above-mentioned gained powder is handled 2h in 500～600 ℃, get final product with the stove cooling.
2, nanometer Ag/TiO according to claim 1 2The composite manufacture method is characterized in that: at first being 25% ammoniacal liquor and deionized water with mass concentration is mixed and made into ammonia spirit by 1: 1 volume ratio, then with AgNO 3Be dissolved in and make the AgNO that concentration is 0.001mol/L in the ammonia spirit 3Ammonia solution; Secondly with Ti (SO 4) 2Be dissolved in the deionized water, being mixed with concentration is the Ti (SO of 0.02mol/L 4) 2Solution; Under 60 ℃ of stirrings, press AgNO 3Ammonia solution and Ti (SO 4) 2Solution is that 1: 1 volume ratio is with AgNO 3Ammonia solution stream is added to Ti (SO 4) 2In the solution or with Ti (SO 4) 2Flow of solution is added to AgNO 3In the ammonia solution, obtain the white size liquid solution; Continue to stir and gained colloidal solution is warming up to 90 ℃, constant temperature 2 hours leaves standstill 24h with colloidal solution in 50 ℃ again; Vacuum filtration is also removed SO through deionized water washing 4 2-Behind the ion, behind 90 ℃ of dry 24h, be ground to powder; Above-mentioned gained powder in 600 ℃ of processing 2h, is got final product with the stove cooling.
3, nanometer Ag/TiO according to claim 1 2The composite manufacture method is characterized in that: at first being 25% ammoniacal liquor and deionized water with mass concentration is mixed and made into ammonia spirit by 1: 1 volume ratio, then with AgNO 3Be dissolved in and make the AgNO that concentration is 0.003mol/L in the ammonia spirit 3Ammonia solution; Secondly with Ti (SO 4) 2Be dissolved in the deionized water, being mixed with concentration is the Ti (SO of 0.05mol/L 4) 2Solution; Under 45 ℃ of stirrings, press AgNO 3Ammonia solution and Ti (SO 4) 2Solution is that 1: 1.5 volume ratio is with AgNO 3Ammonia solution stream is added to Ti (SO 4) 2In the solution or with Ti (SO 4) 2Flow of solution is added to AgNO 3In the ammonia solution, obtain the white size liquid solution; Continue to stir and gained colloidal solution is warming up to 98 ℃, constant temperature 2 hours leaves standstill 18h with colloidal solution in 55 ℃ again; Vacuum filtration is also removed SO through deionized water washing 4 2-Behind the ion, behind 90 ℃ of dry 22h, be ground to powder; Above-mentioned gained powder in 500 ℃ of processing 2h, is got final product with the stove cooling.
4, nanometer Ag/TiO according to claim 1 2The composite manufacture method is characterized in that: at first being 25% ammoniacal liquor and deionized water with mass concentration is mixed and made into ammonia spirit by 1: 1 volume ratio, then with AgNO 3Be dissolved in and make the AgNO that concentration is 0.006mol/L in the ammonia spirit 3Ammonia solution; Secondly with Ti (SO 4) 2Be dissolved in the deionized water, being mixed with concentration is the Ti (SO of 0.1mol/L 4) 2Solution; Under 55 ℃ of stirrings, press AgNO 3Ammonia solution and Ti (SO 4) 2Solution is that 1: 1.2 volume ratio is with AgNO 3Ammonia solution stream is added to Ti (SO 4) 2In the solution or with Ti (SO 4) 2Flow of solution is added to AgNO 3In the ammonia solution, obtain the white size liquid solution; Continue to stir and gained colloidal solution is warming up to 93 ℃, constant temperature 2 hours leaves standstill 15h with colloidal solution in 58 ℃ again; Vacuum filtration is also removed SO through deionized water washing 4 2-Behind the ion, behind 90 ℃ of dry 21h, be ground to powder; Above-mentioned gained powder in 550 ℃ of processing 2h, is got final product with the stove cooling.
5, nanometer Ag/TiO according to claim 1 2The composite manufacture method is characterized in that: at first being 25% ammoniacal liquor and deionized water with mass concentration is mixed and made into ammonia spirit by 1: 1 volume ratio, then with AgNO 3Be dissolved in and make the AgNO that concentration is 0.008mol/L in the ammonia spirit 3Ammonia solution; Secondly with Ti (SO 4) 2Be dissolved in the deionized water, being mixed with concentration is the Ti (SO of 0.16mol/L 4) 2Solution; Under 40 ℃ of stirrings, press AgNO 3Ammonia solution and Ti (SO 4) 2Solution is that 1: 1.4 volume ratio is with AgNO 3Ammonia solution stream is added to Ti (SO 4) 2In the solution or with Ti (SO 4) 2Flow of solution is added to AgNO 3In the ammonia solution, obtain the white size liquid solution; Continue to stir and gained colloidal solution is warming up to 95 ℃, constant temperature 2 hours leaves standstill 22h with colloidal solution in 53 ℃ again; Vacuum filtration is also removed SO through deionized water washing 4 2-Behind the ion, behind 90 ℃ of dry 23h, be ground to powder; Above-mentioned gained powder in 570 ℃ of processing 2h, is got final product with the stove cooling.
6, nanometer Ag/TiO according to claim 1 2The composite manufacture method is characterized in that: at first being 25% ammoniacal liquor and deionized water with mass concentration is mixed and made into ammonia spirit by 1: 1 volume ratio, then with AgNO 3Be dissolved in and make the AgNO that concentration is 0.01mol/L in the ammonia spirit 3Ammonia solution; Secondly with Ti (SO 4) 2Be dissolved in the deionized water, being mixed with concentration is the Ti (SO of 0.2mol/L 4) 2Solution; Under 50 ℃ of stirrings, press AgNO 3Ammonia solution and Ti (SO 4) 2Solution is that 1: 1.1 volume ratio is with AgNO 3Ammonia solution stream is added to Ti (SO 4) 2In the solution or with Ti (SO 4) 2Flow of solution is added to AgNO 3In the ammonia solution, obtain the white size liquid solution; Continue to stir and gained colloidal solution is warming up to 100 ℃, constant temperature 2 hours leaves standstill 12h with colloidal solution in 60 ℃ again; Vacuum filtration is also removed SO through deionized water washing 4 2-Behind the ion, behind 90 ℃ of dry 20h, be ground to powder; Above-mentioned gained powder in 520 ℃ of processing 2h, is got final product with the stove cooling.
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CN101623659B (en) * 2009-08-07 2010-12-01 陕西科技大学 Preparation method for titanium dioxide photocatalyst doped with metal ion
CN101972653A (en) * 2010-10-27 2011-02-16 陕西科技大学 Method for preparing anatase nano Ag/TiO2 composite material
WO2011054153A1 (en) * 2009-11-06 2011-05-12 詹振强 Preparation of silver ion
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CN110180557A (en) * 2019-06-12 2019-08-30 巢湖学院 A kind of Ag2S/TiO2The preparation method and applications of composite photo-catalyst
CN111807712A (en) * 2020-07-23 2020-10-23 长虹美菱股份有限公司 Self-cleaning glass panel of refrigerator and preparation process thereof
CN113509813A (en) * 2021-07-08 2021-10-19 广西柳州中和高新技术有限公司 Ag@Fe3O4@C/TiO2Synthesis method and application of nano material
CN113509813B (en) * 2021-07-08 2022-07-26 广西柳州中和高新技术有限公司 Ag@Fe 3 O 4 @C/TiO 2 Synthesis method and application of nano material

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