CN104069843B - Preparation method of titanium dioxide nanometer photocatalyst - Google Patents
Preparation method of titanium dioxide nanometer photocatalyst Download PDFInfo
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- CN104069843B CN104069843B CN201410349364.0A CN201410349364A CN104069843B CN 104069843 B CN104069843 B CN 104069843B CN 201410349364 A CN201410349364 A CN 201410349364A CN 104069843 B CN104069843 B CN 104069843B
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Abstract
The invention aims to provide a preparation method of a titanium dioxide nanometer photocatalyst which is simple in technology and environment friendly, so as to reduce the technology cost. The preparation method provided by the invention comprises the following steps: A, taking inorganic compound containing titanium ions as a raw material, mixing the raw material and an acidic solution, dissolving the mixture, placing the solution in an ultrasonic cleaning machine, adding an alkali solution to adjust the pH value of the liquid to 10-14; B, using deionized water and alcohol to cleaning a white sediment which is obtained at the end of the preset time of the ultrasonic reaction, and airing or baking to obtain a solid; C, calcining the solid in a muffle furnace to obtain titanium dioxide nanometer photocatalyst in different crystal forms.
Description
Technical field
The present invention relates to new material and environmental protective chemical industry technical field are and in particular to a kind of titanium dioxide nano photocatalysis agent
Preparation method.
Background technology
Nano titanium oxide is a kind of common photocatalyst, has photocatalysis hydrogen production, goes removal organic polluter, sensing etc.
The purposes of aspect.The titanium dioxide nano-rod that this patent is related to can be used for Volatile Organic Compounds in Indoor Air (V DEG C of s,
Volatile Organic Compounds) removal.V DEG C of s is the primary pollution source of room air pollution, and it is wide that it has source
General, species is various, the feature big to Health Impact.At present, conventional indoor V DEG C of s Treatment process have physical adsorption techniques,
Anion technology, non-equilibrium plasma technology, photocatalysis technology, biotechnology and specified plant purification techniques etc..Wherein
Photocatalysis technology, as a kind of main Treatment process, has advantages below with respect to other technology：Reaction condition is gentle, normal
Carry out under normal temperature and pressure；Reaction rate is fast, and required time is short；Nearly all pollutant thoroughly can be degraded to CO2And H2O etc., no two
Secondary pollution.Air pollution treatment aspect shows huge potentiality, at present in air purifier to photocatalysis technology indoors
Obtain practical application.
One-dimensional titanium dioxide includes the materials such as nanotube, nanometer rods, nano wire, and this kind of material is with its unique pattern, relatively
High specific surface area and efficient electron-hole stalling characteristic and extensively concerned.Its preparation method mainly has template, hydro-thermal method
And anodizing etc..Template carries out target material synthesis by the use of the hole in host material structure as template.Template
Size and the nanometer material structure of morphology controllable can be obtained by synthesizing the template of suitable size and structure, the method needs
Select suitable template, complex process.Highly basic hydro-thermal method is under conditions of highly basic, high temperature, high pressure, is former with titanium dioxide
Material, prepares one-dimensional titanium dioxide, and gained catalyst catalytic performance is preferable, but preparation process condition is harsh.Anodizing adopts
The method of electrochemistry prepares titanium dioxide it is easy to control load on the surface of titanium, but limits throughput.
Content of the invention
The purpose of the present invention is to propose to the preparation side of a kind of process is simple, eco-friendly titanium dioxide nano photocatalysis agent
Method, to reduce technical costss.
The preparation method of the titanium dioxide nano photocatalysis agent of the present invention comprises the steps：
A：Using the inorganic compound containing titanium ion as raw material, in corrosion-resistant container, raw material is mixed with acid solution
Close dissolving, then solution is placed in ultrasonic washing unit, adds aqueous slkali, the pH value of liquid is adjusted to 10～14；
B：Ultrasonic reaction obtains white depositions after the scheduled time, after white depositions deionized water and ethanol purge
Dry or dry and obtain solidss；
C：Solidss are placed in calcining in Muffle furnace, the titanium dioxide nano photocatalysis agent of different crystal forms can be obtained.
The present invention prepares titanium dioxide nano-rod using the method for sonochemistry, and ultrasonic is a kind of conventional energy input side
Formula, can accelerate and control chemical reaction, mainly affect chemical reaction by the form of cavitation energy.Under ultrasonication, in liquid
Create micro- gas core（Also referred to as cavitation nucleus）, ultrasonic cavitation just refers in the presence of sound field, this micro- gas nuclear vibration growth and
The dynamic process of collapse closure.When cavitation nuclear disruption closes, the gas in bubble or steam are compressed and are produced TRANSIENT HIGH TEMPERATURE
And partial high pressure, and along with phenomenons such as luminous, shock waves, it is that chemical reaction creates a special reaction condition.Ultrasonic
The microcell that chemical ultrasonic cavitation produces is very hot, but the persistent period is very short, and this is different from traditional photochemistry, thermochemical process.
Using the method for sonochemistry, condition is more gentle, and gained catalyst effect in the application removing V DEG C of s of room air is preferable.
Specifically：
The described inorganic compound containing titanium ion is the sulfate of titanyl compound or titanium, typically adopt titanium dioxide or
Titanyl sulfate.
Acid solution in described step A is Fluohydric acid..
The parameter of the ultrasonic washing unit in described step B is as follows：Power is 100～300W, and frequency is 10～25kHz,
Temperature is 50～80 DEG C；The described scheduled time is 4～8 hours.
In described step B, first with deionized water, white depositions are carried out, until the pH value of cleanout fluid is less than
8, then use time white depositions of ethanol purge again；Finally dry under conditions of 40～60 DEG C again or dry white precipitate
Thing.
In described step C, the calcining heat of Muffle furnace is 300～700 DEG C, and calcination time is 1～4 hour.
Aqueous slkali in described step B is sodium hydroxide or potassium hydroxide solution.
By said method prepare titanium dioxide nano photocatalysis agent, its microstructure is nano bar-shape, and length exists
Between 50～300nm, diameter is between 1～50nm.It is that titanium dioxide nano photocatalysis agent is ground to form purifying the air of a room
Powder, for air cleaning device assembly or be sprayed at indoor wall.
Present invention achieves prepared by the excusing from death chemical method of titanium dioxide nano photocatalysis agent, method therefor avoids template
Use, simplify preparation technology, without reacting at high temperature under high pressure, reduce technical difficulty.Products obtained therefrom specific surface area is big,
Photocatalytic activity is high, and good cycling stability has wide range of applications, can be used for the building materials such as indoor air cleaner and light catalyzed coating
Product, has good application prospect.
Brief description
Fig. 1 is the XRD spectrum of the titanium dioxide nano photocatalysis agent of embodiment 1 preparation.
Fig. 2 is the SEM spectrum of the titanium dioxide nano photocatalysis agent of embodiment 1 preparation.
Fig. 3 is the titanium dioxide nano photocatalysis agent of embodiment 1 and embodiment 3 preparation and commercial photocatalyst P25 performance
Comparison, wherein curve A is titanium dioxide nano photocatalysis agent, and curve B is commercial photocatalyst P25.
Specific embodiment
Below against accompanying drawing, by the description to embodiment, for example involved to the specific embodiment of the present invention is each
Mutual alignment between the shape of component, construction, each several part and annexation, the effect of each several part and operation principle etc. are made into one
The detailed description of step.
Embodiment 1：
The preparation method of the titanium dioxide nano photocatalysis agent of the present embodiment is as follows：
Weigh 2g titanium dioxide to put in polytetrafluoro beaker, add Fluohydric acid. stirring and dissolving, the solution after dissolving is placed in
In ultrasonic washing unit, the operating power of setting supersonic cleaning machine is 200W, 20kHz, 55 DEG C, the ultrasonic response time is 4 little
When, add sodium hydroxide solution to adjust pH value to 14 during ultrasonic reaction；
After ultrasonic reaction finishes, collect white solid deionized water cleaning, until cleanout fluid pH is less than 8, then use second
Alcohol cleans one time, puts in baking oven, dries 2 hours for 50 DEG C；Gained dry solid is placed in Muffle furnace, at 450 DEG C, calcining 2 is little
When, obtain titanium dioxide nano photocatalysis agent.
Fig. 1 is the XRD spectrum of catalyst, chooses（101）Crystal face, as benchmark crystal face, calculates sample using Scherrer formula
Mean diameter is 10.3 nm.Fig. 2 is the SEM image of catalyst, it can be seen that the length of nanometer rods is 200～300
Between nm, diameter is in 30 nm.
Make the typical pollutant toluene experiment of the indoor V DEG C of s of degraded of the photocatalyst being obtained, the concentration of vapor phase toluene adopts
Gas chromatography（GC-FID）Detection, is compared with P25 photocatalyst, result is shown in Fig. 3 simultaneously.Photocatalysis manufactured in the present embodiment
The photocatalytic degradation efficiency of the typical pollutant toluene to indoor V DEG C of s for the agent is substantially better than P25.
Embodiment 2：
The preparation method of the titanium dioxide nano photocatalysis agent of the present embodiment is as follows：
Weigh 2g titanium dioxide to put in polytetrafluoro beaker, add Fluohydric acid. stirring and dissolving, the solution after dissolving is placed in
In ultrasonic washing unit, the operating power of setting supersonic cleaning machine is 300W, 20kHz, 55 DEG C, the ultrasonic response time is 6 little
When, add sodium hydroxide solution to adjust pH value to 14 in ultrasonic procedure；
After ultrasonic reaction finishes, collect white solid deionized water cleaning, until cleanout fluid pH is less than 8, then use second
Alcohol cleans one time, puts in baking oven, dries 2 hours for 50 DEG C；Gained dry solid is placed in Muffle furnace, at 450 DEG C, calcining 2 is little
When, obtain titanium dioxide nano photocatalysis agent.
Embodiment 3：
The preparation method of the titanium dioxide nano photocatalysis agent of the present embodiment is as follows：
Weigh 2g titanium dioxide to put in polytetrafluoro beaker, add Fluohydric acid. stirring and dissolving.Solution after dissolving is placed in super
In sound wave cleaning machine, setting supersonic cleaning machine operating power be 200W, 30kHz, 75 DEG C, the ultrasonic response time be 4 hours,
Sodium hydroxide solution is added to adjust pH value to 14 in ultrasonic procedure；
After ultrasonic reaction finishes, collect white solid deionized water cleaning, until cleanout fluid pH is less than 8, then use second
Alcohol cleans one time, puts in baking oven, dries 2 hours for 50 DEG C；Gained dry solid is placed in Muffle furnace, at 600 DEG C, calcining 2 is little
When, obtain titanium dioxide nano photocatalysis agent.
Make the typical pollutant toluene experiment of the indoor V DEG C of s of degraded of the photocatalyst being obtained, the concentration of vapor phase toluene adopts
Gas chromatography（GC-FID）Detection, is compared with P25 photocatalyst, result is shown in Fig. 3 simultaneously.Photocatalysis manufactured in the present embodiment
The photocatalytic degradation efficiency of the typical pollutant toluene to indoor V DEG C of s for the agent is substantially better than P25.
Embodiment 4：
The preparation method of the titanium dioxide nano photocatalysis agent of the present embodiment is as follows：
Weigh 4g titanium dioxide to put in polytetrafluoro beaker, add Fluohydric acid. stirring and dissolving.Solution after dissolving is placed in super
In sound wave cleaning machine, setting supersonic cleaning machine operating power be 200W, 20kHz, 65 DEG C, the ultrasonic response time be 4 hours,
Sodium hydroxide solution is added to adjust pH value to 14 in ultrasonic procedure；
After ultrasonic reaction finishes, collect white solid deionized water cleaning, until cleanout fluid pH is less than 8, then use second
Alcohol cleans one time, puts in baking oven, dries 2 hours for 50 DEG C；Gained dry solid is placed in Muffle furnace, at 500 DEG C, calcining 2 is little
When, obtain titanium dioxide nano photocatalysis agent.
Claims (7)
1. a kind of preparation method of titanium dioxide nano photocatalysis agent is it is characterised in that comprise the steps：
A：Using the inorganic compound containing titanium ion as raw material, in corrosion-resistant container, raw material is mixed molten with acid solution
Solution, then solution is placed in ultrasonic washing unit, adds aqueous slkali, the pH value of liquid is adjusted to 10～14；
B：Ultrasonic reaction obtains white depositions after the scheduled time, dries after white depositions deionized water and ethanol purge
Or drying obtains solidss；
C：Solidss are placed in calcining in Muffle furnace, the titanium dioxide nano photocatalysis agent of different crystal forms can be obtained；
The described inorganic compound containing titanium ion is the sulfate of titanyl compound or titanium.
2. the preparation method of titanium dioxide nano photocatalysis agent according to claim 1 is it is characterised in that described contain titanium
The inorganic compound of ion is titanium dioxide or titanyl sulfate.
3. the preparation method of titanium dioxide nano photocatalysis agent according to claim 1 is it is characterised in that in described step A
Acid solution be Fluohydric acid..
4. the preparation method of titanium dioxide nano photocatalysis agent according to claim 1 is it is characterised in that in described step B
Ultrasonic washing unit parameter as follows：Power is 100～300W, and frequency is 10～25kHz, and temperature is 50～80 DEG C；Described
The scheduled time is 4～8 hours.
5. the preparation method of titanium dioxide nano photocatalysis agent according to claim 1 is it is characterised in that described step B
In, first with deionized water, white depositions are carried out, until the pH value of cleanout fluid is less than 8, then clear with ethanol again
Wash white depositions；Finally dry under conditions of 40～60 DEG C again or dry white depositions.
6. the preparation method of titanium dioxide nano photocatalysis agent according to claim 1 is it is characterised in that in described step B
Aqueous slkali be sodium hydroxide or potassium hydroxide solution.
7. the preparation method of titanium dioxide nano photocatalysis agent according to claim 1 is it is characterised in that described step C
In, the calcining heat of Muffle furnace is 300～700 DEG C, and calcination time is 1～4 hour.
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| CN1147431C (en) * | 2002-02-01 | 2004-04-28 | 武汉大学 | Process for preparing anatase-phase nano TiO2 |
| CN100484880C (en) * | 2005-09-22 | 2009-05-06 | 中国科学院理化技术研究所 | Low temperature crystallized nano titanium dioxide powder and sol synthesizing method |
| US7749468B2 (en) * | 2006-08-17 | 2010-07-06 | Gm Global Technology Operations, Inc. | Cavitation reaction apparatus |
| CN102976401A (en) * | 2012-10-22 | 2013-03-20 | 山东轻工业学院 | Ultrasonic chemical preparation method for nitrogen-doped nano-titanium dioxide crystal |
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| Selective synthesis of anatase and rutile via ultrasound irradiation;Weiping Huang, et al;《 Chem. Commun.》;20000711;第2000卷;第1415右栏第1段至1416页左栏第1段 * |
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