CN105191981A - Preparation method for copper-doped nanometer titania with photo-catalysis antibacterial property - Google Patents
Preparation method for copper-doped nanometer titania with photo-catalysis antibacterial property Download PDFInfo
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- CN105191981A CN105191981A CN201510651518.6A CN201510651518A CN105191981A CN 105191981 A CN105191981 A CN 105191981A CN 201510651518 A CN201510651518 A CN 201510651518A CN 105191981 A CN105191981 A CN 105191981A
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Abstract
The invention discloses a preparation method for copper-doped nanometer titania with photo-catalysis antibacterial property. The preparation method comprises the following steps: taking 28.602ml of butyl titanate and 22.1ml of triethanolamine and uniformly mixing the solutions, adding 105.34ml of deionized water, forming a 0.5mol/L Ti<4+> solution, adding 15ml of prepared copper salt solution, causing the mole percent of Cu<2+> to Ti<4+> to be 0.2% and uniformly stirring; adding 150ml of prepared 0.12mol/L sodium hydroxide solution into the solution and uniformly stirring; putting the reaction liquid into a heat-resisting bottle and aging for 22-26 hours at 90-110 DEG C; split-charging the formed colloid with high viscidity into a polytetrafluoroethylene-lined high pressure kettle and aging for 70-74 hours at 130-150 DEG C; repeatedly centrifugally washing the reaction liquid after aging in a 10000-12000r/min centrifugal machine till the reaction liquid is neutral; freezing and drying a sample in a vacuum freeze drying machine; and grinding the prepared nanometer titania micro-powder. According to the preparation method provided by the invention, the photo-catalysis antibacterial effect of the titania is effectively promoted; the titania has higher antibacterial property under both sunlight and dark conditions; the preparation method is simple and feasible; and the cost is low.
Description
Technical field
The present invention relates to a kind of method preparing nano titanium oxide, specifically a kind of preparation method with photocatalysis bacteriostasis property Copper-cladding Aluminum Bar nano titanium oxide.
Background technology
Nano material refers to that particle size is the ultrafine dust of nanometer scale, and because its size is little, specific surface area is large, surface atom number is many, surface energy and surface tension sharply increase with the decline of particle diameter and have the new features such as light, heat, electricity, magnetic that quantum size effect, small-size effect, skin effect and macro quanta tunnel effect etc. are different from Conventional solid.TiO
2for inorganic constituents, nontoxic, tasteless, nonirritant, heat endurance and good heat resistance and do not burn.Nano-TiO
2be a kind of novel inorganic material, particle diameter is 10-50nm, is equivalent to 1/10 of ordinary titanium powder particle diameter.Have the characteristic of the aspects such as very strong absorption UV resistance, preferably heat endurance, chemical stability and excellent optics, electricity and mechanics, in recent ten years, it as a kind of New Inorganic Antibacterial Agents development rapidly.Also a lot of to its research both at home and abroad.Start at every field application TiO both at home and abroad
2antibacterial and absorb ultraviolet performance, present many companies be devoted to apply TiO
2develop environment-friendly products, comprise self-cleaning fabric, pottery etc.As antibacterial agent, nano-TiO
2there is following feature: 1. prompt effect is good; 2. be a kind of antibacterial agent of semipermanent maintenance antibacterial effect; 3. good safety is had.But also there are some technical problems 1, photo-generate electron-hole is high to recombination rate.2, the energy gap due to titanium dioxide is large, so its light absorption is only confined near ultraviolet band, to the availability of sunshine only about 1%.3, there are some basic center and also have hydrophily in titanium dioxide surface, can greatly reduce light-catalyzed reaction speed.4, titanium dioxide spectrum response range is narrow.5, photocatalytic activity and granularity have very large relation, and granularity is less, and photocatalytic activity is higher, but too smallly secondary aggregation can occur.Secondly now general technology needs in technique to carry out high-temperature calcination, and the power consumption of this process is serious, and can produce a large amount of discarded heat-energy losses, temperature-fall period is slow.
Summary of the invention
The object of the present invention is to provide a kind of preparation method with photocatalysis bacteriostasis property Copper-cladding Aluminum Bar nano titanium oxide, to solve the problem proposed in above-mentioned background technology.
For achieving the above object, the invention provides following technical scheme:
There is a preparation method for photocatalysis bacteriostasis property Copper-cladding Aluminum Bar nano titanium oxide, comprise the steps:
1) get butyl titanate 28.602ml to mix with triethanolamine 22.1ml solution, add deionized water 105.34ml, form the Ti of 0.5mol/L
4+solution, adds the copper salt solution 15ml configured, makes Cu
2+shared Ti
4+mol ratio is 0.2%, stirs;
2) in solution, adding the 150ml concentration prepared is 0.12mol/L sodium hydroxide solution, stirs;
3) reactant liquor is placed in screw-topped heat-resisting bottle, in 90-110 DEG C of ageing 22-26h;
4) colloid of the high viscosity of formation is divided the autoclave being filled to teflon lined, in 130-150 DEG C of ageing 70-74h;
5) reactant liquor after ageing, in 10000-12000r/min centrifuge, carries out repeatedly centrifuge washing, and washing is to neutral;
6) sample carries out freeze drying in vacuum freeze drier machine;
7) nanometer titanium dioxide micropowder prepared is ground.
As the further scheme of the present invention: in step 2) concentration of sodium hydroxide solution that adds in solution is 0.12mol/L.
As the further scheme of the present invention: in step 3) reactant liquor is placed in screw-topped heat-resisting bottle, in 100 DEG C of ageing 24h.
As the further scheme of the present invention: in step 4) colloid of the high viscosity of formation is divided the autoclave being filled to teflon lined, in 140 DEG C of ageing 72h.
As the further scheme of the present invention: in step 5) reactant liquor after ageing is in 11000r/min centrifuge, and carry out repeatedly centrifuge washing, washing is to neutral.
As the further scheme of the present invention: described copper salt solution is the one in copper nitrate solution, copper-bath or copper chloride solution.
Compared with prior art, the present invention effectively improves optically catalytic TiO 2 fungistatic effect, under sunshine He under half-light, all have stronger bacteriostasis property, and simple for process, and cost is low practical.
Embodiment
Be described in more detail below in conjunction with the technical scheme of embodiment to this patent.
Embodiment 1
There is a preparation method for photocatalysis bacteriostasis property Copper-cladding Aluminum Bar nano titanium oxide, comprise the steps: that getting butyl titanate 28.602ml mixes with triethanolamine 22.1ml solution, adds deionized water 105.34ml, form the Ti of 0.5mol/L
4+solution, adds the copper salt solution 15ml configured, makes Cu
2+shared Ti
4+mol ratio is 0.2%, stirs; In solution, add the 150ml concentration prepared is 0.12mol/L sodium hydroxide solution, stirs; Reactant liquor is placed in screw-topped heat-resisting bottle, in 90 DEG C of ageing 22h; The colloid of the high viscosity of formation is divided the autoclave being filled to teflon lined, in 130 DEG C of ageing 70h; Reactant liquor after ageing, in 10000r/min centrifuge, carries out repeatedly centrifuge washing, and washing is to neutral; Sample carries out freeze drying in vacuum freeze drier machine; The nanometer titanium dioxide micropowder prepared is ground.
Embodiment 2
There is a preparation method for photocatalysis bacteriostasis property Copper-cladding Aluminum Bar nano titanium oxide, comprise the steps: that getting butyl titanate 28.602ml mixes with triethanolamine 22.1ml solution, adds deionized water 105.34ml, form the Ti of 0.5mol/L
4+solution, adds the copper salt solution 15ml configured, makes Cu
2+shared Ti
4+mol ratio is 0.2%, stirs; In solution, add the 150ml concentration prepared is 0.12mol/L sodium hydroxide solution, stirs; Reactant liquor is placed in screw-topped heat-resisting bottle, in 110 DEG C of ageing 26h; The colloid of the high viscosity of formation is divided the autoclave being filled to teflon lined, in 150 DEG C of ageing 74h; Reactant liquor after ageing, in 12000r/min centrifuge, carries out repeatedly centrifuge washing, and washing is to neutral; Sample carries out freeze drying in vacuum freeze drier machine; The nanometer titanium dioxide micropowder prepared is ground.
Embodiment 3
There is a preparation method for photocatalysis bacteriostasis property Copper-cladding Aluminum Bar nano titanium oxide, comprise the steps: that getting butyl titanate 28.602ml mixes with triethanolamine 22.1ml solution, adds deionized water 105.34ml, form the Ti of 0.5mol/L
4+solution, adds the copper salt solution 15ml configured, makes Cu
2+shared Ti
4+mol ratio is 0.2%, stirs; In solution, add the 150ml concentration prepared is 0.12mol/L sodium hydroxide solution, stirs; Reactant liquor is placed in screw-topped heat-resisting bottle, in 100 DEG C of ageing 24h; The colloid of the high viscosity of formation is divided the autoclave being filled to teflon lined, in 140 DEG C of ageing 72h; Reactant liquor after ageing, in 11000r/min centrifuge, carries out repeatedly centrifuge washing, and washing is to neutral; Sample carries out freeze drying in vacuum freeze drier machine; The nanometer titanium dioxide micropowder prepared is ground.
At nano-TiO
2particle surface carries out metal-doped, changes the character of particle surface, effectively prevent the simple composite of electron-hole, further increases TiO
2particulate germicidal efficiency, the doping of metal simultaneously greatly strengthen nano-TiO
2photocatalysis effect under visible light.Secondly, mantoquita was once used as the Biocidal algae-killing agent of Treatment of Industrial Water for a long time and widely.For microorganism, copper belongs to enzyme inhibitor, and the mechanism of its sterilization algae removal is after copper ion contacts with bacterium, fungi, algae, copper ion infiltrates into bacterium, fungi, algae inside, condense its protein colloid, thus cause the metabolism disorder of microorganism, cause the death of cell.The mantoquita of common copper series antibacterial agent has copper sulphate, copper citrate etc.Although mantoquita has stronger killing action to aquatile, mantoquita as the metal material equipment such as carbon steel produce strong corrosion, has therefore seldom been applied to copper series antibacterial agent the sterilization of industry water to tube metal material now.Therefore select copper ion doped its photocatalytic activity under light illumination that both can strengthen also to have certain bacteriostasis property in half-light.General method of carrying out modifying transformation to titanium dioxide first carries out ageing to carry out high-temperature calcination more at present, this technique time consumption and energy consumption, and the mode that this method adopts carries out freeze drying process, when identical ageing process, adopt the bacteriostasis property mixing copper nano titanium oxide of frozen drying process relatively better.
The present invention effectively improves optically catalytic TiO 2 fungistatic effect, under sunshine He under half-light, all have stronger bacteriostasis property, and simple for process, and cost is low practical.
Above the better embodiment of this patent is explained in detail, but this patent is not limited to above-mentioned embodiment, in the ken that one skilled in the relevant art possesses, can also makes a variety of changes under the prerequisite not departing from this patent aim.
Claims (6)
1. there is a preparation method for photocatalysis bacteriostasis property Copper-cladding Aluminum Bar nano titanium oxide, it is characterized in that, comprise the steps:
1) get butyl titanate 28.602ml to mix with triethanolamine 22.1ml solution, add deionized water 105.34ml, form the Ti of 0.5mol/L
4+solution, adds the copper salt solution 15ml configured, makes Cu
2+shared Ti
4+mol ratio is 0.2%, stirs;
2) in solution, adding the 150ml concentration prepared is 0.12mol/L sodium hydroxide solution, stirs;
3) reactant liquor is placed in screw-topped heat-resisting bottle, in 90-110 DEG C of ageing 22-26h;
4) colloid of the high viscosity of formation is divided the autoclave being filled to teflon lined, in 130-150 DEG C of ageing 70-74h;
5) reactant liquor after ageing, in 10000-12000r/min centrifuge, carries out repeatedly centrifuge washing, and washing is to neutral;
6) sample carries out freeze drying in vacuum freeze drier machine;
7) nanometer titanium dioxide micropowder prepared is ground.
2. the preparation method with photocatalysis bacteriostasis property Copper-cladding Aluminum Bar nano titanium oxide according to claim 1, is characterized in that, in step 2) in the concentration of sodium hydroxide solution that adds in solution be 0.12mol/L.
3. the preparation method with photocatalysis bacteriostasis property Copper-cladding Aluminum Bar nano titanium oxide according to claim 1, is characterized in that, in step 3) in reactant liquor is placed in screw-topped heat-resisting bottle, in 100 DEG C of ageing 24h.
4. the preparation method with photocatalysis bacteriostasis property Copper-cladding Aluminum Bar nano titanium oxide according to claim 1, is characterized in that, in step 4) colloid of the high viscosity of formation is divided the autoclave being filled to teflon lined, in 140 DEG C of ageing 72h.
5. the preparation method with photocatalysis bacteriostasis property Copper-cladding Aluminum Bar nano titanium oxide according to claim 1, is characterized in that, in step 5) in reactant liquor after ageing in 11000r/min centrifuge, carry out repeatedly centrifuge washing, washing is to neutral.
6. the preparation method with photocatalysis bacteriostasis property Copper-cladding Aluminum Bar nano titanium oxide according to claim 1, is characterized in that, described copper salt solution is the one in copper nitrate solution, copper-bath or copper chloride solution.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105733322A (en) * | 2016-01-25 | 2016-07-06 | 渤海大学 | Copper-doped titanium dioxide coating and preparation method thereof |
| CN106732590A (en) * | 2016-11-24 | 2017-05-31 | 郑州轻工业学院 | A kind of preparation method of copper/titanium oxide photochemical catalyst nano material |
| CN107917351A (en) * | 2017-10-27 | 2018-04-17 | 中山市汉庭照明科技有限公司 | A kind of LED light bulbs and preparation method having except effect of formaldehyde |
| CN109354061A (en) * | 2018-10-18 | 2019-02-19 | 九江学院 | A kind of preparation method of monodisperse ultra-small grain size titanium dioxide nanocrystalline |
| CN112813527A (en) * | 2020-12-28 | 2021-05-18 | 江苏品创纺织科技有限公司 | Chitin fiber blended mildew-proof fabric |
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| CN101564694A (en) * | 2008-04-25 | 2009-10-28 | 北京化工大学 | Method for preparing nitrogen doped nanometer titanium dioxide visible light photocatalyst |
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| CN101564694A (en) * | 2008-04-25 | 2009-10-28 | 北京化工大学 | Method for preparing nitrogen doped nanometer titanium dioxide visible light photocatalyst |
Non-Patent Citations (2)
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| 李慧芳: "分子筛负载改性纳米Ti02的制备及光催化活性研究", 《中南大学硕士学位论文》 * |
| 路建美，黄志斌: "《综合化学实验 第2版》", 31 May 2014, 南京大学出版社 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105733322A (en) * | 2016-01-25 | 2016-07-06 | 渤海大学 | Copper-doped titanium dioxide coating and preparation method thereof |
| CN106732590A (en) * | 2016-11-24 | 2017-05-31 | 郑州轻工业学院 | A kind of preparation method of copper/titanium oxide photochemical catalyst nano material |
| CN106732590B (en) * | 2016-11-24 | 2019-09-17 | 郑州轻工业学院 | A kind of preparation method of copper/titanium oxide photochemical catalyst nano material |
| CN107917351A (en) * | 2017-10-27 | 2018-04-17 | 中山市汉庭照明科技有限公司 | A kind of LED light bulbs and preparation method having except effect of formaldehyde |
| CN109354061A (en) * | 2018-10-18 | 2019-02-19 | 九江学院 | A kind of preparation method of monodisperse ultra-small grain size titanium dioxide nanocrystalline |
| CN112813527A (en) * | 2020-12-28 | 2021-05-18 | 江苏品创纺织科技有限公司 | Chitin fiber blended mildew-proof fabric |
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Application publication date: 20151230 |