CN102205244A - Silver-carrying titanium dioxide anti-bacterial agent and preparation method thereof - Google Patents
Silver-carrying titanium dioxide anti-bacterial agent and preparation method thereof Download PDFInfo
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- CN102205244A CN102205244A CN2011100923944A CN201110092394A CN102205244A CN 102205244 A CN102205244 A CN 102205244A CN 2011100923944 A CN2011100923944 A CN 2011100923944A CN 201110092394 A CN201110092394 A CN 201110092394A CN 102205244 A CN102205244 A CN 102205244A
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Abstract
The invention belongs to the technical field of environmental catalytic materials and specifically relates to a preparation method of a silver-carrying titanium dioxide anti-bacterial agent. The anti-bacterial agent comprises titanium dioxide microspheres as carriers with a high length-diameter ratio and silver particles distributed on surfaces or interiors of the titanium dioxide microspheres. The preparation method comprises a titanium dioxide microsphere preparation method and a silver particle carrying method, wherein the silver particle carrying method adopts the following three methods of a complex reaction and photo-reduction combined method, a direct photo-reduction method and an excessive immersion method. The operation of the present preparation method is simple. Titanium dioxide carriers prepared by the present preparation method has a high length-diameter ratio, a high crystallinity and thus can reduce effectively recombination of electrons and holes and enhance titanium dioxide photocatalytical and anti-bacterial effects, and the silver particle carrying method can effectively control a dispersibility of silver and make silver be distributed on surfaces or interiors of titanium dioxide microspheres to realize a slow release of silver, avoid color change, and enhance anti-bacterial effects simultaneously.
Description
Technical field
The invention belongs to environmental catalysis material technology field, be specifically related to antiseptic of a kind of titanium dioxide microballoon sphere load silver particles and preparation method thereof.
Background technology
Metal oxide titanium dioxide (TiO
2) have a special photo-catalysis function, yet, because its energy gap is 3.2eV,, form electronegative high activity electronics e so only when wavelength was penetrated less than the illumination of 387.5nm, the electronics on the valence band just can be excited into conduction band
-, and on valence band, produce corresponding hole h
+, under electric field action, separate and move to particle surface, with water and oxygen reaction, generate hydroxyl radical free radical (OH) and active oxygen (O
2 -), thereby be adsorbed on lip-deep harmful substance and carry out redox reaction.But electron-hole pair is easily compound, has influenced its catalytic activity, and this conditional request of UV-irradiation must be arranged, so limited the application of titanium dioxide.Silver has excellent antibiotic, bactericidal action, but costing an arm and a leg, sustained release performance is bad, variable color easily under high temperature or oxidizing atmosphere.By increasing the carrier draw ratio, simultaneously, combine with silver, both can reduce titanic oxide electronic-hole-recombination, improve photocatalytic activity, and can not influenced by external condition again, with a spot of silver, reach good antibacterial effect, overcome its shortcoming such as easy to change simultaneously.
Summary of the invention
The object of the present invention is to provide a kind of photo-catalysis capability strong, and have simultaneously sterilizing function antiseptic and the preparation method, discharge and reach allochroic deficiency soon to overcome existing inorganic antibacterial material titanic oxide electronic commute and hole-recombination and to carry ag material silver.
Antiseptic provided by the invention is distributed in by silver particles and has surface or inner form of draw ratio up to the carrier titanium dioxide microballoon sphere of 25-35.Wherein, the diameter of described titanium dioxide microballoon sphere is 1.5-2.5 μ m, and silver carrying amount is the 0.5-1.5% of titanium dioxide microballoon sphere quality.
The preparation method of of the present invention year silver-colored titanium dioxide anti-bacterial agent is as follows:
1, adopts hydro-thermal reaction synthetic vectors TiO
2Microballoon.TiCl with 0.1-0.2M
3The NaCl powder of solution and 9-11M dissolves with appropriate amount of deionized water, is transferred in the 250ml volumetric flask behind the constant volume, put in the reactor 150-250 ℃ hydro-thermal reaction 14-18 hour, suction filtration, washing, 70-100 ℃ of oven dry ground 300-500 ℃ of back roasting 4-8 hour.The cold back of stove is taken out and is promptly obtained the carrier titanium dioxide microballoon sphere, and diameter is 1.5-2.5 μ m.
2, adopt three kinds of method load silver, a kind of is the method that complex reaction and photo-reduction combine, and a kind of is the direct sunshine reducing process, and a kind of is excessive infusion process.
The method that complex reaction and photo-reduction combine can make silver be distributed in the surface of carrier, specifically be to be the 0.5-1.5% configuration liquor argenti nitratis ophthalmicus of titanium dioxide microballoon sphere mass fraction according to silver carrying amount, press silver nitrate and 4,4-bipyridyl mass concentration ratio is 4-6:8-10 preparation 4,4-bipyridyl ethanolic solution, and with silver nitrate ethanolic solution and 4, the 4-bipyridyl mixes, join then in the titanium dioxide ethanolic solution, behind the 35-50 ℃ of rotary evaporation, adding 60-85ml ethanol, is 100-200r/min at rotating speed, 254nm, under 96 watts of ultraviolet lamp irradiations, illumination 1-3 hour, suction filtration, 70-100 ℃ of drying prepared end product and carried silver-colored titanium dioxide anti-bacterial agent.
The direct sunshine reducing process can make silver be distributed in carrier inside, specifically be to be the 0.5-1.5% of titanium dioxide microballoon sphere mass fraction according to silver carrying amount, configuration titanium dioxide ethanolic solution 20-30ml and silver nitrate ethanolic solution 45-55ml, deoxygenation, at ultraviolet light less than the 387.5nm wavelength, rotating speed is under the condition of 150-200r/min, ultraviolet lighting titanium dioxide ethanolic solution 20-40 minute, the speed of dripping according to 1-3ml/min adds 5-10ml silver nitrate ethanolic solution in titania solution then, then illumination 3-8 minute under the same conditions, after dripping residue silver nitrate ethanolic solution, continue illumination 1-3 hour, through suction filtration, 75-85 ℃ of drying obtains end product after the 400-600 ℃ of calcining and carries silver-colored titanium dioxide anti-bacterial agent.
Excessive infusion process can make silver be distributed in carrier inside, specifically be to be the 0.5-1.5% of titanium dioxide microballoon sphere mass fraction according to silver carrying amount, titanium dioxide is added in the silver nitrate aqueous solution, and 50-70 ℃ of rotary evaporation prepared end product after the 400-600 ℃ of calcining and carried silver-colored titanium dioxide anti-bacterial agent.
The inventive method is simple to operate, and synthetic carrier titanium dioxide draw ratio can reduce the compound of electronics and hole effectively up to 25-35, strengthens the optically catalytic TiO 2 antibacterial effect; The carrying method of silver can effectively be controlled silver-colored dispersiveness, makes silver be distributed in the surperficial or inner of carrier titanium dioxide, to realize silver-colored slowly-releasing and to prevent variable color, simultaneously, strengthens antibacterial effect.
Description of drawings
Fig. 1 is the TiO with high length-diameter ratio
2The microballoon transmission electron microscope photo.
Fig. 2 is three kinds and carries silver-colored TiO
2(a) complex reaction of the transmission electron microscope photo of antiseptic and the excessive infusion process of photo-reduction combined techniques (b) direct sunshine reducing process (c).
The specific embodiment
Configuration 50ml solution contains 0.15M titanium trichloride solution and 10M sodium chloride.200 ℃ of reactions are after 16 hours in baking oven, and filtration washing, is slowly pulverized after the cooling in 400 ℃ of calcinings 4 hours 85 ℃ of down dry backs, prepares the titanium dioxide microballoon sphere carrier.
Embodiment 1:
1) with the titanium dioxide incipient impregnation in ethanol, put into the vacuum drying chamber air drying, A liquid;
2) be 100:1 preparation silver nitrate ethanolic solution according to titanium dioxide and silver-colored mass ratio, silver nitrate and 4,4-bipyridyl mass concentration ratio are 5.3:9.75 preparation 4,4-bipyridyl ethanolic solution, and with silver nitrate ethanolic solution and 4,4-bipyridyl ethanolic solution mixes, and gets B liquid;
3) A liquid is mixed with B liquid, 40 ℃ of rotary evaporations get powder C;
4) add 80ml ethanol in C, the magnetic stirring apparatus rotating speed is 150r/min, at 254nm, and under 96 watts of ultraviolet lamp irradiations, illumination 2 hours;
5) suction filtration, 80 ℃ of dryings obtain carrying silver-colored titanium dioxide microballoon sphere antiseptic.
Embodiment 2:
1) be 100:1 according to titanium dioxide and silver-colored mass ratio, configuration titanium dioxide ethanolic solution 25ml and silver nitrate ethanolic solution 50ml are positioned over respectively in Photoreactor and the beaker, feed nitrogen deoxygenation 10 minutes;
2) at 254nm, under 96 watts of ultraviolet lamp irradiations, the magnetic stirring apparatus rotating speed is 150r/min, illumination titanium dioxide ethanolic solution 30 minutes;
3) keeping the same light photograph, under the speed conditions prerequisite, slowly adding part silver nitrate ethanolic solution with peristaltic pump in titania solution, it is 2ml/min that speed is dripped in control, continues illumination 5 minutes;
4) add residue silver nitrate ethanolic solution with peristaltic pump, continue illumination 2 hours;
5) suction filtration, 80 ℃ of dry backs obtain to carry silver-colored titanium dioxide microballoon sphere antiseptic in 500 ℃ of calcinings 4 hours.
Embodiment 3:
Titanium dioxide is added in the silver nitrate aqueous solution, and the mass ratio of titanium dioxide and silver is 100:1, calcines 4 hours for 500 ℃ behind 60 ℃ of rotary evaporations, slowly pulverizes after the cooling, prepares and carries silver-colored titanium dioxide microballoon sphere antiseptic.
Claims (2)
1. one kind carries silver-colored titanium dioxide anti-bacterial agent, it is characterized in that being distributed in by silver particles having the surface of carrier titanium dioxide microballoon sphere that draw ratio is 25-35 or inner; Wherein, the diameter of described titanium dioxide microballoon sphere is 1.5-2.5 μ m, and silver carrying amount is the 0.5-1.5% of titanium dioxide microballoon sphere quality.
2. the preparation method of year silver-colored titanium dioxide anti-bacterial agent as claimed in claim 1 is characterized in that concrete steps are as follows:
1, adopts hydro-thermal reaction synthetic vectors TiO
2Microballoon: with the TiCl of 0.1-0.2M
3The NaCl powder deionized water dissolving of solution and 9-11M is transferred in the volumetric flask behind the constant volume, put in the reactor 150-250 ℃ hydro-thermal reaction 14-18 hour, suction filtration, washing, 70-100 ℃ of oven dry ground 300-500 ℃ of back roasting 4-8 hour; The cold back of stove is taken out and is promptly obtained the carrier titanium dioxide microballoon sphere, and diameter is 1.5-2.5 μ m;
2, adopt three kinds of method load silver, a kind of is the method that complex reaction and photo-reduction combine, and a kind of is the direct sunshine reducing process, and a kind of is excessive infusion process;
The method that complex reaction and photo-reduction combine makes silver be distributed in the surface of carrier, the steps include: according to silver carrying amount to be the 0.5-1.5% configuration liquor argenti nitratis ophthalmicus of titanium dioxide microballoon sphere mass fraction, press silver nitrate and 4,4-bipyridyl mass concentration ratio is 4-6:8-10 preparation 4,4-bipyridyl ethanolic solution, and with silver nitrate ethanolic solution and 4, the 4-bipyridyl mixes, and joins then in the titanium dioxide ethanolic solution, behind the 35-50 ℃ of rotary evaporation, adding 60-85ml ethanol, is 100-200r/min at rotating speed, and wavelength is under 96 watts of ultraviolet lamp irradiations of 254nm, illumination 1-3 hour, suction filtration, 70-100 ℃ of drying makes end product and carries silver-colored titanium dioxide anti-bacterial agent;
The direct sunshine reducing process makes silver be distributed in carrier inside, the steps include: according to silver carrying amount to be the 0.5-1.5% of titanium dioxide microballoon sphere mass fraction, configuration titanium dioxide ethanolic solution 20-30ml and silver nitrate ethanolic solution 45-55ml, deoxygenation, at ultraviolet light less than the 387.5nm wavelength, rotating speed is under the condition of 150-200r/min, ultraviolet lighting titanium dioxide ethanolic solution 20-40 minute, the speed of dripping according to 1-3ml/min adds 5-10ml silver nitrate ethanolic solution in titania solution then, then illumination 3-8 minute under the same conditions, after dripping residue silver nitrate ethanolic solution, continue illumination 1-3 hour, through suction filtration, 75-85 ℃ of drying makes end product after the 400-600 ℃ of calcining and carries silver-colored titanium dioxide anti-bacterial agent;
Excessive infusion process makes silver be distributed in carrier inside, the steps include: according to silver carrying amount to be the 0.5-1.5% of titanium dioxide microballoon sphere mass fraction, titanium dioxide is added in the silver nitrate aqueous solution, and 50-70 ℃ of rotary evaporation makes end product after the 400-600 ℃ of calcining and carries silver-colored titanium dioxide anti-bacterial agent.
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|---|---|---|---|---|
| CN102764649A (en) * | 2012-07-09 | 2012-11-07 | 陕西科技大学 | Metal-silver-supported titanium dioxide photocatalyst and preparation method thereof |
| CN103342912A (en) * | 2013-07-24 | 2013-10-09 | 太仓市协诚金属制品有限公司 | Antibacterial coating used for surface of metal product |
| CN104304319A (en) * | 2014-09-16 | 2015-01-28 | 南京财经大学 | Preparation method of silver-supported titanium dioxide inorganic antiseptic |
| CN105037870A (en) * | 2015-06-10 | 2015-11-11 | 苏州宏恒化工有限公司 | Preparation method of polyethylene composite material for storage tanks |
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-
2011
- 2011-04-13 CN CN2011100923944A patent/CN102205244A/en active Pending
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Application publication date: 20111005 |