CN102489283B - Carbon nanotube and {001}surface TiO2 microsphere composite material photocatalyst - Google Patents

Carbon nanotube and {001}surface TiO2 microsphere composite material photocatalyst Download PDF

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CN102489283B
CN102489283B CN2011103628220A CN201110362822A CN102489283B CN 102489283 B CN102489283 B CN 102489283B CN 2011103628220 A CN2011103628220 A CN 2011103628220A CN 201110362822 A CN201110362822 A CN 201110362822A CN 102489283 B CN102489283 B CN 102489283B
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photocatalyst
material photocatalyst
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CN102489283A (en
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安太成
陈江耀
聂信
黄勇
李桂英
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Guangzhou Institute of Geochemistry of CAS
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Abstract

The invention, belonging to the technical field of adsorption catalysis materials, discloses a carbon nanotube and {001}surface TiO2 microsphere composite material photocatalyst, its preparation method and application. The preparation method comprises the following steps: adding titanium tetrafluoride in water, fully stirring, and then adding nanotubes pretreated by acids, carrying out ultrasonicdispersion, carrying out hydro-thermal reaction in a teflon pot, collecting precipitates in the pot, cleaning in a centrifugal way, and drying to obtain the carbon nanotube and {001}surface TiO2 microsphere composite material photocatalyst. The photocatalyst has strong adsorption properties to volatile organic compounds and strong photocatalytic activity, so as to realize the integration of the absorption and photocatalytic oxidation of the volatile organic compounds, thus hydroxy radicals generated on the surface of the catalyst can be allowed to effectively mineralize and degrade the volatile organic compounds absorbed and gathered by the adsorption material in situ, and the reaction rate and efficiency of the photocatalytic oxidation of organic pollutants are greatly enhanced. The photocatalyst can be applied as an adsorbent or photocatalyst for the field of environmental protection.

Description

CNT and { 001} face TiO 2The microballoon composite material photocatalyst
Technical field
The invention belongs to absorbent-type catalysis material technical field, particularly a kind of CNT and { 001} face TiO 2Microballoon composite photocatalyst agent material and preparation method thereof and in the atmospheric environment protection Application for Field.
Background technology
Volatile organic matter has brought a large amount of environmental problems to us, and has seriously threatened human life security.Increasing physics, chemistry and biotechnology are used to the improvement of volatile organic matter, and wherein photocatalysis oxidation technique can finally be oxidized to CO with volatile organic matter because of it in the presence of the irradiation of light and photochemical catalyst 2And H 2O and being paid close attention to widely.In numerous photochemical catalysts, TiO 2Be used to handle all kinds of environmental problems such as water and air purifying problem etc. as a kind of stable photochemical catalyst.
No matter be that theory is calculated or experimental result all shows anatase TiO 2{ the 001} mask has very high activity.Yet, because the relatively low and TiO of concentration of the volatile organic matter in the environment 2Specific area less, make TiO 2The amount of absorption pollutant is less, thereby has reduced photocatalytic degradation speed and final total removal efficient, makes high activity { 001} high energy face TiO 2Application be subjected to certain restriction.
(Carbon Nanotube is just found a kind of novel carbon nanomaterial in 1991 CNT) to CNT, and it is seamless, the hollow tube body that is rolled into by the Graphene lamella that carbon atom forms.CNT is as monodimension nanometer material, and is in light weight, and hexagonal structure connects perfect, has many unusual mechanics, electricity and chemical property.CNT is expected at hydrogen storage material, novel battery, electrochemical sensor, isolation technics and have very important using value aspect pollution control.The diameter of CNT is little, its pore structure is fit to rapid absorption and the desorption of a large amount of volatile organic matters, the surface treatment of different condition also can change the functional group on CNT surface, makes it have different selection suction-operateds, therefore can be used to control the pollution of variety classes volatile organic matter.And at present also not about CNT and { 001} face TiO 2The preparation of microballoon composite material photocatalyst and the report of aspect the volatile organic matter degraded, using thereof.
Summary of the invention
In order to solve above-mentioned the deficiencies in the prior art part, primary and foremost purpose of the present invention provides a kind of CNT and { 001} face TiO 2The preparation method of microballoon composite material photocatalyst.
Another object of the present invention provides the CNT and { 001} face TiO that method for preparing obtains 2The microballoon composite material photocatalyst.This CNT and { 001} face TiO 2The microballoon composite material photocatalyst not only has stronger absorption property to typical volatile organic matter, and has stronger photocatalytic activity.
A further object of the present invention provides above-mentioned CNT and { 001} face TiO 2The application of microballoon composite material photocatalyst.
Purpose of the present invention is achieved through the following technical solutions: a kind of CNT and { 001} face TiO 2The preparation method of microballoon composite material photocatalyst comprises the steps:
(1) 0.5～10g CNT being joined 4～200mL volume ratio is in 1～10: 1 the nitration mixture, refluxed 5～180 minutes down at 60～140 ℃, filtering washing then, is 3～11 until the pH of washing lotion value, the sediment after the washing is dried down at 50～180 ℃ obtain purifying carbon nano-tube;
(2) 0.01～1g titanium tetrafluoride is joined in 10～200mL water, fully stir, obtain the titanium tetrafluoride settled solution;
(3) 0.01～1g step (1) gained purifying carbon nano-tube is added in 10～100mL step (2) gained titanium tetrafluoride settled solution, obtains mixed solution after the ultrasonic dispersion;
(4) 5～100mL step (3) gained mixed solution is packed in the polytetrafluoroethyltank tank, 60～250 ℃ of following hydro-thermal reactions 2～72 hours;
(5) treat in the polytetrafluoroethyltank tank solution cooling after, collect tank bottoms, water is centrifuge washing repeatedly, is 3～11 until the pH of washing lotion value, and the sediment after the washing 50～180 ℃ of oven dry 1～36 hour down, is namely got CNT and { 001} face TiO 2The microballoon composite material photocatalyst.
The described nitration mixture of step (1) is two kinds of mixing in concentrated hydrochloric acid, red fuming nitric acid (RFNA) and the concentrated sulfuric acid.
The described CNT of step (1) is SWCN, double-walled carbon nano-tube or multi-walled carbon nano-tubes;
The described well-beaten time of step (2) is 1～60 minute.
The time of the described ultrasonic dispersion of step (3) is 1～60 minute.
The water that relates in the above-mentioned steps is deionized water.
A kind of CNT and { 001} face TiO 2The microballoon composite material photocatalyst forms by method for preparing.
CNT of the present invention and { 001} face TiO 2The microballoon composite material photocatalyst can have wide environmental protection application potential in the environmental protection field as selective absorbent or the photochemical catalyst of volatile organic matter.
The present invention compares with prior art, has following advantage and beneficial effect:
The present invention is with the adsorption and enrichment effect and { 001} face TiO of CNT to volatile organic matter 2The photocatalysis mineralization of microsphere photocatalyst combines, and prepares a kind of new and effective absorption-photocatalysis integrated material---CNT and { 001} face TiO 2The microballoon composite material photocatalyst found through experiments CNT and { 001} face TiO that the present invention prepares 2The microballoon composite material photocatalyst shows good adsorption and photocatalytic activity to gas phase typical case volatile organic matter styrene, it is 300 minutes that absorption penetrates the needed time fully, be that the cinnamic degradation rate of gas phase of 25 ± 1.5ppmv is up to 47.3% to initial concentration in other 180 minutes, thereby realized the integrated of the absorption of typical volatile organic matter and photochemical catalytic oxidation, the mineralizing and degrading sorbing material is adsorbed effectively in position to make the hydroxyl radical free radical that catalyst surface produces, the volatile organic matter of enrichment, strengthen reaction rate and the efficient of photocatalysis degradation organic contaminant greatly, original position has solved the regeneration difficult problem of adsorbent simultaneously, has avoided back disposal and the secondary pollution problem of adsorbent.
Description of drawings
Fig. 1 is CNT and { 001} face TiO 2The X-ray powder diffraction of microballoon composite material photocatalyst (XRD) collection of illustrative plates; Wherein, ■: TiO 2The anatase characteristic peak.
Fig. 2 is CNT and { 001} face TiO 2The scanning electron microscope diagram of microballoon composite material photocatalyst (SEM) and transmission electron microscope figure (TEM).
Fig. 3 is CNT and { 001} face TiO 2The microballoon composite material photocatalyst is to the cinnamic adsorption penetration curve of gas phase and kinetics of photocatalytic degradation curve map.
The specific embodiment
The present invention is described in further detail below in conjunction with embodiment and accompanying drawing, but embodiments of the present invention are not limited thereto.
Embodiment 1
(1) the 0.5g multi-walled carbon nano-tubes being joined the 40mL volume ratio is in 2: 1 the concentrated hydrochloric acid and red fuming nitric acid (RFNA), refluxed 120 minutes down at 100 ℃, filtering washing then, is 6 until the pH of washing lotion value, the sediment after the washing is dried down at 100 ℃ obtain purification of Multi-wall Carbon Nanotubes;
(2) the 0.05g titanium tetrafluoride is joined in the 30mL water, fully stirred 10 minutes, obtain the titanium tetrafluoride settled solution;
(3) 0.2g step (1) gained purification of Multi-wall Carbon Nanotubes is added in 20mL step (2) the gained titanium tetrafluoride settled solution, ultrasonic dispersion obtained mixed solution after 5 minutes;
(4) 10mL step (3) gained mixed solution is packed in the polytetrafluoroethyltank tank, 150 ℃ of following hydro-thermal reactions 52 hours;
(5) treat in the jar solution cooling after, collect tank bottoms, water is centrifuge washing repeatedly, is 7 until the pH of washing lotion value, and the sediment after the washing 50 ℃ of oven dry 6 hours down, is namely got multi-walled carbon nano-tubes and { 001} face TiO 2The microballoon composite material photocatalyst.
Gained CNT and { 001} face TiO 2The performance of microballoon composite material photocatalyst is as follows:
1, XRD collection of illustrative plates
To CNT and { 001} face TiO 2The microballoon composite material photocatalyst has carried out XRD analysis, and the collection of illustrative plates result as shown in Figure 1.As seen from the figure, on the XRD collection of illustrative plates of prepared photochemical catalyst typical TiO has appearred 2The anatase characteristic peak.This can forecasting institute the photochemical catalyst of preparation have certain photocatalytic activity.
2, SEM figure and TEM figure
Fig. 2 has provided CNT and { 001} face TiO 2The SEM of microballoon composite material photocatalyst and TEM figure.By SEM figure as can be seen, CNT and { 001} face TiO 2The microballoon composite material photocatalyst is made up of microballoon and CNT that diameter is about 600nm, and microballoon is made up of one one the thin plate that length and width are about 200-300nm, by tem analysis, the facing of finding these thin plates is high energy exposure { 001} face.
3. CNT and { 001} face TiO 2The research of microballoon composite material photocatalyst photocatalytic activity
Fig. 3 is CNT and { 001} face TiO 2The microballoon composite material photocatalyst is to cinnamic adsorption penetration curve and kinetics of photocatalytic degradation curve.As seen from the figure, this photochemical catalyst shows good adsorption and photocatalytic activity, and to penetrate the needed time fully be 300 minutes in absorption, and degradation results shows at 180min and can reach 47.3% to cinnamic degradation rate in addition.By above the result CNT and { 001} face TiO of the present invention preparation as can be seen 2The microballoon composite is the new material of a kind of high absorption and photocatalytic activity.
CNT of the present invention and { 001} face TiO 2The microballoon composite material photocatalyst has fine photocatalysis performance, as the organic pollution catalysts selective, has application potential widely in the environmental protection field.
Embodiment 2
(1) the 0.5g double-walled carbon nano-tube being joined the 60mL volume ratio is in 1: 1 the concentrated hydrochloric acid and the concentrated sulfuric acid, refluxed 180 minutes down at 60 ℃, filtering washing then, is 5 until the pH of washing lotion value, the sediment after the washing is dried down at 50 ℃ obtain the purifying double-walled carbon nano-tube;
(2) the 0.01g titanium tetrafluoride is joined in the 200mL water, fully stirred 60 minutes, obtain the titanium tetrafluoride settled solution;
(3) 1g step (1) gained purifying double-walled carbon nano-tube is added in 100mL step (2) the gained titanium tetrafluoride settled solution, ultrasonic dispersion obtained mixed solution after 10 minutes;
(4) 10mL step (3) gained mixed solution is packed in the polytetrafluoroethyltank tank, 250 ℃ of following hydro-thermal reactions 2 hours;
(5) treat in the jar solution cooling after, collect tank bottoms, water is centrifuge washing repeatedly, is 4 until the pH of washing lotion value, and the sediment after the washing 70 ℃ of oven dry 36 hours down, is namely got double-walled carbon nano-tube and { 001} face TiO 2The microballoon composite material photocatalyst.
Embodiment 3
(1) the 2g multi-walled carbon nano-tubes being joined the 100mL volume ratio is in 4: 1 the concentrated hydrochloric acid and red fuming nitric acid (RFNA), refluxed 80 minutes down at 80 ℃, filtering washing then, is 11 until the pH of washing lotion value, the sediment after the washing is dried down at 80 ℃ obtain purification of Multi-wall Carbon Nanotubes;
(2) the 0.08g titanium tetrafluoride is joined in the 60mL water, fully stirred 6 minutes, obtain the titanium tetrafluoride settled solution;
(3) 0.15g step (1) gained purification of Multi-wall Carbon Nanotubes is added in 45mL step (2) the gained titanium tetrafluoride settled solution, ultrasonic dispersion obtained mixed solution after 12 minutes;
(4) 5mL step (3) gained mixed solution is packed in the polytetrafluoroethyltank tank, 120 ℃ of following hydro-thermal reactions 42 hours;
(5) treat in the jar solution cooling after, collect tank bottoms, water is centrifuge washing repeatedly, is 3 until the pH of washing lotion value, and the sediment after the washing 80 ℃ of oven dry 16 hours down, is namely got multi-walled carbon nano-tubes and { 001} face TiO 2The microballoon composite material photocatalyst.
Embodiment 4
(1) the 4g SWCN being joined the 200mL volume ratio is in 6: 1 the red fuming nitric acid (RFNA) and the concentrated sulfuric acid, refluxed 10 minutes down at 100 ℃, filtering washing then, is 7 until the pH of washing lotion value, the sediment after the washing is dried down at 150 ℃ obtain the purifying SWCN;
(2) the 0.5g titanium tetrafluoride is joined in the 120mL water, fully stirred 30 minutes, obtain the titanium tetrafluoride settled solution;
(3) 0.09g step (1) gained purifying SWCN is added in 15mL step (2) the gained titanium tetrafluoride settled solution, ultrasonic dispersion obtained mixed solution after 1 minute;
(4) 5mL step (3) gained mixed solution is packed in the polytetrafluoroethyltank tank, 100 ℃ of following hydro-thermal reactions 7 hours;
(5) treat in the jar solution cooling after, collect tank bottoms, water is centrifuge washing repeatedly, is 6 until the pH of washing lotion value, and the sediment after the washing 60 ℃ of oven dry 6 hours down, is namely got SWCN and { 001} face TiO 2The microballoon composite material photocatalyst.
Embodiment 5
(1) the 1g SWCN being joined the 50mL volume ratio is in 2: 1 the concentrated hydrochloric acid and the concentrated sulfuric acid, refluxed 50 minutes down at 110 ℃, filtering washing then, is 9 until the pH of washing lotion value, the sediment after the washing is dried down at 180 ℃ obtain the purifying SWCN;
(2) the 0.7g titanium tetrafluoride is joined in the 70mL water, fully stirred 20 minutes, obtain the titanium tetrafluoride settled solution;
(3) 0.9g step (1) gained purifying SWCN is added in 65mL step (2) the gained titanium tetrafluoride settled solution, ultrasonic dispersion obtained mixed solution after 7 minutes;
(4) 50mL step (3) gained mixed solution is packed in the polytetrafluoroethyltank tank, 60 ℃ of following hydro-thermal reactions 65 hours;
(5) treat in the jar solution cooling after, collect tank bottoms, water is centrifuge washing repeatedly, is 11 until the pH of washing lotion value, and the sediment after the washing 180 ℃ of oven dry 1 hour down, is namely got SWCN and { 001} face TiO 2The microballoon composite material photocatalyst.
Embodiment 6
(1) the 10g double-walled carbon nano-tube being joined the 120mL volume ratio is in 10: 1 the red fuming nitric acid (RFNA) and the concentrated sulfuric acid, refluxed 90 minutes down at 90 ℃, filtering washing then, is 7 until the pH of washing lotion value, the sediment after the washing is dried down at 65 ℃ obtain the purifying double-walled carbon nano-tube;
(2) the 0.03g titanium tetrafluoride is joined in the 10mL water, fully stirred 1 minute, obtain the titanium tetrafluoride settled solution;
(3) 0.01g step (1) gained purifying double-walled carbon nano-tube is added in 30mL step (2) the gained titanium tetrafluoride settled solution, ultrasonic dispersion obtained mixed solution after 30 minutes;
(4) 20mL step (3) gained mixed solution is packed in the polytetrafluoroethyltank tank, 210 ℃ of following hydro-thermal reactions 72 hours;
(5) treat in the jar solution cooling after, collect tank bottoms, water is centrifuge washing repeatedly, is 6 until the pH of washing lotion value, and the sediment after the washing 60 ℃ of oven dry 12 hours down, is namely got double-walled carbon nano-tube and { 001} face TiO 2The microballoon composite material photocatalyst.
Embodiment 7
(1) the 0.5g double-walled carbon nano-tube being joined the 4mL volume ratio is in 10: 1 the red fuming nitric acid (RFNA) and the concentrated sulfuric acid, refluxed 5 minutes down at 140 ℃, filtering washing then, is 3 until the pH of washing lotion value, the sediment after the washing is dried down at 85 ℃ obtain the purifying double-walled carbon nano-tube;
(2) the 1g titanium tetrafluoride is joined in the 60mL water, fully stirred 10 minutes, obtain the titanium tetrafluoride settled solution;
(3) 1g step (1) gained purifying double-walled carbon nano-tube is added in 100mL step (2) the gained titanium tetrafluoride settled solution, ultrasonic dispersion obtained mixed solution after 60 minutes;
(4) 100mL step (3) gained mixed solution is packed in the polytetrafluoroethyltank tank, 180 ℃ of following hydro-thermal reactions 55 hours;
(5) treat in the jar solution cooling after, collect tank bottoms, water is centrifuge washing repeatedly, is 6 until the pH of washing lotion value, and the sediment after the washing 120 ℃ of oven dry 25 hours down, is namely got double-walled carbon nano-tube and { 001} face TiO 2The microballoon composite material photocatalyst.
Above-described embodiment is preferred implementation of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spiritual essence of the present invention and the principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.

Claims (8)

1. a CNT and { 001} face TiO 2The preparation method of microballoon composite material photocatalyst is characterized in that comprising the steps:
(1) 0.5～10g CNT is joined in the nitration mixture that 4～200mL volume ratio is 1～10:1, refluxed 5～180 minutes down at 60～140 ℃, filtering washing then, is 3～7 until the pH of washing lotion value, the sediment after the washing is dried down at 50～180 ℃ obtain purifying carbon nano-tube;
(2) 0.01～1g titanium tetrafluoride is joined in 10～200mL water, fully stir, obtain the titanium tetrafluoride settled solution;
(3) 0.01～1g step (1) gained purifying carbon nano-tube is added in 10～100mL step (2) gained titanium tetrafluoride settled solution, obtains mixed solution after the ultrasonic dispersion;
(4) 5～100mL step (3) gained mixed solution is packed in the polytetrafluoroethyltank tank, 60～250 ℃ of following hydro-thermal reactions 2～72 hours;
(5) treat in the polytetrafluoroethyltank tank solution cooling after, collect tank bottoms, water is centrifuge washing repeatedly, is 3～11 until the pH of washing lotion value, and the sediment after the washing 50～180 ℃ of oven dry 1～36 hour down, is namely got CNT and { 001} face TiO 2The microballoon composite material photocatalyst.
2. CNT according to claim 1 and { 001} face TiO 2The preparation method of microballoon composite material photocatalyst is characterized in that: the described nitration mixture of step (1) is two kinds of mixing in concentrated hydrochloric acid, red fuming nitric acid (RFNA) and the concentrated sulfuric acid.
3. CNT according to claim 1 and { 001} face TiO 2The preparation method of microballoon composite material photocatalyst is characterized in that: the described CNT of step (1) is SWCN, double-walled carbon nano-tube or multi-walled carbon nano-tubes.
4. CNT according to claim 1 and { 001} face TiO 2The preparation method of microballoon composite material photocatalyst is characterized in that: the described well-beaten time of step (2) is 1～60 minute.
5. CNT according to claim 1 and { 001} face TiO 2The preparation method of microballoon composite material photocatalyst is characterized in that: the time of the described ultrasonic dispersion of step (3) is 1～60 minute.
6. CNT according to claim 1 and { 001} face TiO 2The preparation method of microballoon composite material photocatalyst is characterized in that: described water is deionized water.
7. a CNT and { 001} face TiO 2The microballoon composite material photocatalyst is prepared by each described preparation method in the claim 1～6.
8. the described CNT of claim 7 and { 001} face TiO 2The microballoon composite material photocatalyst is in the environmental protection Application for Field.
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