CN103657646A - Method for loading gold nanoparticles on titanium dioxide nanotube - Google Patents
Method for loading gold nanoparticles on titanium dioxide nanotube Download PDFInfo
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- CN103657646A CN103657646A CN201210328995.5A CN201210328995A CN103657646A CN 103657646 A CN103657646 A CN 103657646A CN 201210328995 A CN201210328995 A CN 201210328995A CN 103657646 A CN103657646 A CN 103657646A
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Abstract
The invention discloses a method for loading gold nanoparticles on a titanium dioxide nanotube. Butyl titanate and butanol are used as raw materials to prepare rutile phase titanium dioxide powder, a hydrothermal method is adopted for synthesizing the rutile phase titanium dioxide powder into the titanium dioxide nanotube, HAuCl4 solution and trisodium citrate solution are added into mercaptoacetic acid solution containing the rutile phase titanium dioxide powder for reaction under an acidic condition to obtain the titanium dioxide nanotube with the surface loaded with Au. According to the method, the process is simple, the equipment requirement is low, the loading rate is high.
Description
Technical field
The present invention relates to a kind of preparation method of nano titanic oxide catalyst.
Background technology
Titania nanotube is a kind of of titanium dioxide nano material, and for nano TiO 2 powder and titanic oxide nano-membrane, it has larger specific area, and its adsorption capacity is also stronger, therefore has excellent PhotoelectrocatalytiPerformance Performance.Titania nanotube has stronger photocatalysis performance can be made into catalyst, and he has good degradation capability to the most pollutants in water.After titania nanotube doping metals, increased the surface area of titanium dioxide optical catalyst and improved the photocatalysis efficiency of titanium deoxide catalyst; More convenient to use and improved the service efficiency of luminous energy after carrier is fixing, be convenient to again recycling of catalyst.The method of titanium dioxide nano-particle surface deposition noble metal is a lot, mainly contains at present light deposition, electronation and high-temperature calcination three classes.Although these methods can realize metal nanoparticle in the load of titanium dioxide surface, method is loaded down with trivial details, and stricter to reflecting requirement, cost is higher, and load factor is conventionally lower.
Summary of the invention
For solving problems of the prior art, the object of the invention is to substantially overcome the defect that on existing titania nanotube, load gold nano particle method is comparatively loaded down with trivial details, reaction condition is high, load factor is lower, provide a kind of technique simple, equipment requirement is low, the new method of load gold nano particle on the higher titania nanotube of load factor.
The present invention realizes the technical scheme that its object is taked: a kind of method of titania nanotube load gold nano particle, comprises the steps:
(1) HNO that is 3-4 by every 1LpH value
3in solution, add 50-200ml tetraethyl titanate and 20-80ml n-butanol, stirring at room 10-15h, is transferred in reactor and reacts 4-6h at 120-200 ℃, and product is cooling, filter, washing, dry, and obtains rutile TiO 2 nano particles;
(2) by adding 1-50g rutile TiO 2 nano particles in the NaOH solution of every 1L10mol/L, after magnetic agitation is even, be transferred in sealed reactor, be heated to 110 ℃ of reaction 12-48h, cooling, ultrasonic dispersion after taking out, filtration, washing, oven dry, obtain TiO
2nanotube;
(3) by every 1L50% TGA solution, add the 1-50gTiO making
2nanotube, stirs 1-3h, then adds 10-50ml0.1mol/lHAuCl
4solution, stirs 1-3h, adds 200-500ml1% citric acid three sodium solution, is transferred to 120 ℃ of reaction 1-5h in reactor, and product is cooling, filter, washing, dry.
beneficial effect of the present invention:the present invention not only can realize load Au nano particle on TiO2 nanotube and nanobelt equably, nano particle uniform particles, distribute narrow, decentralization is high, load is controlled, and technique is simple, operability and highly versatile, be suitable for large-scale production, equipment needed thereby is simple.
Accompanying drawing explanation
Fig. 1 is the TiO of the embodiment of the present invention 1
2the transmission electron microscope picture of nanoparticle;
Fig. 2 is the TiO of the embodiment of the present invention 1
2the transmission electron microscope picture of nanotube;
Fig. 3 is the Au doped Ti O of the embodiment of the present invention 1
2the transmission electron microscope picture of nanotube.
The specific embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
Embodiment 1
After being mixed, 150ml tetraethyl titanate and 75ml n-butanol be added to 1000mlpH value and be 3.5 HNO
3in solution, stirring at room 15h, is transferred in reactor and reacts 5h at 180 ℃, and product is cooling, filter, washing, dry, and obtains rutile TiO
2nano particle; By 20g rutile TiO
2nano particle is added in the NaOH solution of 1000ml10mol/L, after stirring, is transferred in sealed reactor, is heated to 110 ℃ of reaction 36h, and cooling, ultrasonic dispersion after product takes out, filtration, washing, oven dry, obtain TiO
2nanotube; By 20gTiO
2nanotube is added to 1000ml50% TGA solution, stirs 3h, then adds 30ml0.1mol/lHAuCl
4solution, stirs 3h, adds 400ml1% citric acid three sodium solution, is transferred to 120 ℃ of reaction 5h in reactor, and product is cooling, filter, washing, dry, and obtains the TiO of doped precious metal gold
2nanotube.
Embodiment 2
After being mixed, 200ml tetraethyl titanate and 80ml n-butanol be added to 1000mlpH value and be 4 HNO
3in solution, stirring at room 15h, is transferred in reactor and reacts 6h at 200 ℃, and product is cooling, filter, washing, dry, and obtains rutile TiO
2nano particle; By 50g rutile TiO
2nano particle is added in the NaOH solution of 1000ml10mol/L, after stirring, is transferred in sealed reactor, is heated to 110 ℃ of reaction 48h, and cooling, ultrasonic dispersion after product takes out, filtration, washing, oven dry, obtain TiO
2nanotube; By 50gTiO
2nanotube is added to 1000ml50% TGA solution, stirs 3h, then adds 50ml0.1mol/lHAuCl
4solution, stirs 3h, adds 500ml1% citric acid three sodium solution, is transferred to 120 ℃ of reaction 5h in reactor, and product is cooling, filter, washing, dry, and obtains the TiO of doped precious metal gold
2nanotube.
Embodiment 3
After being mixed, 50ml tetraethyl titanate and 20ml n-butanol be added to 1000mlpH value and be 3 HNO
3in solution, stirring at room 10h, is transferred in reactor and reacts 4h at 120 ℃, and product is cooling, filter, washing, dry, and obtains rutile TiO
2nano particle; By 1g rutile TiO
2nano particle is added in the NaOH solution of 1000ml10mol/L, after stirring, is transferred in sealed reactor, is heated to 110 ℃ of reaction 12h, and cooling, ultrasonic dispersion after product takes out, filtration, washing, oven dry, obtain TiO
2nanotube; By 1gTiO
2nanotube is added to 1000ml50% TGA solution, stirs 1h, then adds 10ml0.1mol/lHAuCl
4solution, stirs 1h, adds 200ml1% citric acid three sodium solution, is transferred to 120 ℃ of reaction 1h in reactor, and product is cooling, filter, washing, dry, and obtains the TiO of doped precious metal gold
2nanotube.
Embodiment 4
After being mixed, 100ml tetraethyl titanate and 60ml n-butanol be added to 1000mlpH value and be 4 HNO
3in solution, stirring at room 10h, is transferred in reactor and reacts 5h at 180 ℃, and product is cooling, filter, washing, dry, and obtains rutile TiO
2nano particle; By 30g rutile TiO
2nano particle is added in the NaOH solution of 1000ml10mol/L, after stirring, is transferred in sealed reactor, is heated to 110 ℃ of reaction 30h, and cooling, ultrasonic dispersion after product takes out, filtration, washing, oven dry, obtain TiO
2nanotube; By 25gTiO
2nanotube is added to 1000ml50% TGA solution, stirs 1-3h, then adds 10-50ml0.1mol/lHAuCl
4solution, stirs 2h, adds 300ml1% citric acid three sodium solution, is transferred to 120 ℃ of reaction 3h in reactor, and product is cooling, filter, washing, dry, and obtains the TiO of doped precious metal gold
2nanotube.
Embodiment 5
After being mixed, 100ml tetraethyl titanate and 40ml n-butanol be added to 1000mlpH value and be 3 HNO
3in solution, stirring at room 10h, is transferred in reactor and reacts 5h at 180 ℃, and product is cooling, filter, washing, dry, and obtains rutile TiO
2nano particle; By 30g rutile TiO
2nano particle is added in the NaOH solution of 1000ml10mol/L, after stirring, is transferred in sealed reactor, is heated to 110 ℃ of reaction 30h, and cooling, ultrasonic dispersion after product takes out, filtration, washing, oven dry, obtain TiO
2nanotube; By 25gTiO
2nanotube is added to 1000ml50% TGA solution, stirs 2h, then adds 10-50ml0.1mol/lHAuCl
4solution, stirs 1-3h, adds 200ml1% citric acid three sodium solution, is transferred to 120 ℃ of reaction 4h in reactor, and product is cooling, filter, washing, dry, and obtains the TiO of doped precious metal gold
2nanotube.
Claims (4)
1. a method for titania nanotube load gold nano particle, is characterized in that: comprise the steps:
(1) by adding 50-200ml tetraethyl titanate and 20-80ml n-butanol in every 1L, stirring at room 10-15h, is transferred in reactor and reacts 4-6h at 120-200 ℃, and product is cooling, filter, washing, dry, and obtains rutile TiO 2 nano particles;
(2) by adding 1-50g rutile TiO in the NaOH solution of every 1L10mol/L
2nano particle, after magnetic agitation is even, is transferred in sealed reactor, is heated to 110 ℃ of reaction 12-48h, and cooling, ultrasonic dispersion after taking out, filtration, washing, oven dry, obtain TiO
2nanotube;
(3) TiO that adds 1-50g to make by every 1L50% TGA solution
2nanotube, stirs 1-3h, then adds 10-50ml0.1mol/lHAuCl
4solution, stirs 1-3h, adds 200-500ml1% citric acid three sodium solution, is transferred to 120 ℃ of reaction 1-5h in reactor, and product is cooling, filter, washing, dry.
2. the method for titania nanotube load gold nano particle according to claim 1, is characterized in that: described HNO
3pH is 3-4.
3. the method for titania nanotube load gold nano particle according to claim 1, is characterized in that: described rutile TiO
2nano particle addition is 1-50g.
4. the method for titania nanotube load gold nano particle according to claim 1, is characterized in that: described TiO
2nanotube addition is 1-50g.
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|---|---|---|---|
| CN201210328995.5A CN103657646A (en) | 2012-09-07 | 2012-09-07 | Method for loading gold nanoparticles on titanium dioxide nanotube |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104368003A (en) * | 2014-11-14 | 2015-02-25 | 郑州大学 | Preparation method and application of hyaluronic acid modified Au-doped titanium dioxide nano-tube |
| CN104689815A (en) * | 2015-02-15 | 2015-06-10 | 福建工程学院 | Preparation technology of Au-TiO2 nanotube at atmospheric pressure |
| CN104722298A (en) * | 2015-03-26 | 2015-06-24 | 电子科技大学 | Method for preparing titania composite nano-gold photocatalyst |
| WO2016116776A1 (en) * | 2015-01-23 | 2016-07-28 | Umm Al-Qura University | Gold loaded tio2 nanotube-multiwalled carbon nanotube composites as active photocatalysts for cyclohexane oxidation |
| CN109621948A (en) * | 2019-01-23 | 2019-04-16 | 深圳市至霸化工有限公司 | One kind having weak light-catalysed nano-titanium dioxide and preparation method thereof |
| CN111111709A (en) * | 2020-01-06 | 2020-05-08 | 山东鲁泰化学有限公司 | Acetylene hydrochlorination non-mercury catalyst taking titanium dioxide nanotube as carrier |
-
2012
- 2012-09-07 CN CN201210328995.5A patent/CN103657646A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104368003A (en) * | 2014-11-14 | 2015-02-25 | 郑州大学 | Preparation method and application of hyaluronic acid modified Au-doped titanium dioxide nano-tube |
| CN104368003B (en) * | 2014-11-14 | 2017-04-12 | 郑州大学 | Preparation method and application of hyaluronic acid modified Au-doped titanium dioxide nano-tube |
| WO2016116776A1 (en) * | 2015-01-23 | 2016-07-28 | Umm Al-Qura University | Gold loaded tio2 nanotube-multiwalled carbon nanotube composites as active photocatalysts for cyclohexane oxidation |
| US9452418B2 (en) | 2015-01-23 | 2016-09-27 | Umm Al-Qura University | Gold loaded TiO2 nanotube-multiwalled carbon nanotube composites as active photocatalysts for cyclohexane oxidation |
| CN104689815A (en) * | 2015-02-15 | 2015-06-10 | 福建工程学院 | Preparation technology of Au-TiO2 nanotube at atmospheric pressure |
| CN104722298A (en) * | 2015-03-26 | 2015-06-24 | 电子科技大学 | Method for preparing titania composite nano-gold photocatalyst |
| CN109621948A (en) * | 2019-01-23 | 2019-04-16 | 深圳市至霸化工有限公司 | One kind having weak light-catalysed nano-titanium dioxide and preparation method thereof |
| CN111111709A (en) * | 2020-01-06 | 2020-05-08 | 山东鲁泰化学有限公司 | Acetylene hydrochlorination non-mercury catalyst taking titanium dioxide nanotube as carrier |
| CN111111709B (en) * | 2020-01-06 | 2023-02-28 | 山东鲁泰化学有限公司 | Acetylene hydrochlorination non-mercury catalyst taking titanium dioxide nanotube as carrier |
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Application publication date: 20140326 |