CN102151561A - Photocatalyst consisting of carbon nanotubes loaded with titanium dioxide and preparation method thereof - Google Patents
Photocatalyst consisting of carbon nanotubes loaded with titanium dioxide and preparation method thereof Download PDFInfo
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Abstract
The invention provides a preparation method of a photocatalyst consisting of carbon nanotubes loaded with titanium dioxide. The photocatalyst refers to carbon nano-tubes with titanium dioxide on the outer surfaces. The preparation method comprises the following steps: (1) acidifying the multi-walled carbon nanotubes; (2) dispersing the carbon nanotubes subjected to acidification in a solvent, and then adding a titanium dioxide precursor to perform hydrolysis so as to generate nano-titanium dioxide and enabling the nano-titanium dioxide to be attached to the surfaces of the carbon nanotubes; and (3) performing high-temperature treatment on the carbon nanotubes with the titanium dioxide so as to transform the crystal form of the titanium dioxide into anatase to finally obtain the photocatalyst consisting of the carbon nanotubes loaded with the titanium dioxide. The method has the advantages of simple production process, low cost and wide application scope and is convenient for large-scale industrial production; and the obtained loaded photocatalyst has no selectivity in degradation, no secondary pollution and high photocatalytic efficiency.
Description
Technical field
The present invention relates to nano-carbon tube load titanium dioxide optical catalyst and preparation method thereof, belong to inorganic chemistry photochemical catalyst field.
Background technology
Along with the continuous development of various countries' industrial or agricultural, low concentration, organic pollution poisonous, difficult degradation have become a global significant problem, and traditional method for treating wastewater for this class material to dispel effect unsatisfactory.Great deal of research results shows in recent years, and nano material titanium dioxide has good photocatalytic activity in environmental pollution improvement's process.But in the application of reality, the separation of catalyst fines, recovery still do not have good solution.The load of catalyst fixedly is to solve the effective way that the suspended phase catalyst separation reclaims, and can overcome shortcomings such as poor catalyst stability and easy poisoning.
In the technique for fixing that Chinese scholars has been attempted, once the carrier of Cai Yonging had bead, glass plate, fiber optics, Bio-sil, porous ceramic film and active carbon etc.CNT is because electricity, machinery and the hot property of its uniqueness, at electronics, and computer, fields such as Aero-Space have potential wide application prospect, are the representatives of current new material and nanometer technology.For optimizing and promote CNT, need assemble certain nanostructured in carbon nano tube surface usually in each Application for Field.Being assembled of CNT and nano particle can form similar coaxial nano cable, and the structure of nano-probe is expected to be applied at aspects such as solar cell, catalyst material, nano electron devices.In recent years, adhere to the various oxides of assembling in carbon nano tube surface, as SiO
2, SnO
2, Al(OH)
3And Al
2O
3Existing report.The compound of these CNTs and oxide normally in solution nano particle be attached to carbon nano tube surface in the mode of Electrostatic Absorption.But this preparation method process complexity, and product structure is inhomogeneous.
Summary of the invention
The object of the present invention is to provide photochemical catalyst of a kind of nano-carbon tube load titanium dioxide and preparation method thereof.This preparation method's production technology is simple, with low cost, use is wide, be convenient to realize large-scale industrial production.
For achieving the above object, the technical solution used in the present invention is:
The photochemical catalyst of nano-carbon tube load titanium dioxide of the present invention is that the outer surface at CNT is attached with nano titanium oxide.
The preparation method of the photochemical catalyst of nano-carbon tube load titanium dioxide of the present invention comprises the steps:
(1) multiple-wall carbon nanotube is carried out acidification;
(2) CNT after the acidification is dispersed in the solvent, the back adds TiO 2 precursor and is hydrolyzed reaction to generate nano titanium oxide and to make the surface of nano titanium oxide attached to CNT;
(3) nano-sized carbon that will be attached with titanium dioxide is carried out high-temperature process, and making the crystal transfer of titanium dioxide is Detitanium-ore-type, thereby makes the photochemical catalyst of nano-carbon tube load titanium dioxide.
Further, the described TiO 2 precursor of step of the present invention (2) be in butyl titanate, isopropyl titanate, the metatitanic acid n-propyl any or appoint several.
Further, the described hydrolysis of step of the present invention (2) is to be catalyst with acid.
Further, acid catalyst of the present invention be in sulfuric acid, hydrochloric acid, the nitric acid any or appoint several.
Further, the hydrolysis temperature of the described hydrolysis of step of the present invention (2) is 30 ~ 60
oC, hydrolysis time are 6 ~ 12 h.
Further, the temperature of the described high-temperature process of step of the present invention (3) is 350 ~ 500
oC, time are 2 ~ 4 h.
Compared with prior art, advantage of the present invention is:
(1) the present invention utilizes nano titanium oxide because its unique photocatalysis and electric conductivity, CNT and nano-titania particle is carried out compound, forms new catalysis material, and the organic matter environment of high concentration is provided for catalytic degradation reaction; Simultaneously, by diffusion, the organic matter that is adsorbed moves to titanium dioxide, and the organic matter on titanium dioxide degradable CNT surface makes carrier realize in-situ regeneration again, and this synergy has further improved the photocatalysis performance of titanium dioxide.(2) photochemical catalyst of the present invention combine CNT itself as carrier to the organic strong adsorption capacity of aromatic ring, help organic matter in its surperficial enrichment; CNT can be used as titanic oxide electronic and excites acceptor simultaneously, thereby has also accelerated organic pollution photocatalytic degradation speed.
(3) preparation method's technology of the present invention is simple, and the preparation condition gentleness is easy and simple to handle, small investment, and energy consumption is low, therefore, is easy to promote and industrialization.
(4) good degrading effect of the loaded photocatalyst that obtains of preparation method of the present invention, degradation speed is fast, generally only needs dozens of minutes can obtain good treatment effect to several hrs.
(5) the loaded photocatalyst degraded non-selectivity that obtains of preparation method of the present invention, any organic matter of almost degrading is particularly suitable for chlorinatedorganic, polycyclic aromatic hydrocarbon etc.Be applicable to the organic matter of handling industry and sanitary wastewater and airborne poisonous and harmful and bio-refractory.
(6) the loaded photocatalyst non-secondary pollution that obtains of preparation method of the present invention, organic matter thoroughly is degraded to CO
2And H
2Innocuous substances such as O; Applied range, nearly all sewage can adopt.
Description of drawings
The invention will be further described below in conjunction with drawings and Examples, and the cited case does not influence protection scope of the present invention.
Fig. 1 a is multiple-wall carbon nanotube transmission electron microscope (TEM) figure;
Fig. 1 b is the ESEM behind the multiple-wall carbon nanotube carried titanium dioxide (SEM) figure among the embodiment 1;
Fig. 2 a is the X-ray diffractogram behind the multiple-wall carbon nanotube carried titanium dioxide among the embodiment 1;
Fig. 2 b is a nano-carbon tube load titanium dioxide compound photocatalytic degradation aqueous solution of methylene blue change curve in time among the embodiment 1;
Fig. 3 a is the ESEM behind the multiple-wall carbon nanotube carried titanium dioxide (SEM) figure among the embodiment 2;
Fig. 3 b is a nano-carbon tube load titanium dioxide compound photocatalytic degradation aqueous solution of methylene blue change curve in time among the embodiment 2;
Fig. 4 a is the ESEM behind the multiple-wall carbon nanotube carried titanium dioxide (SEM) figure among the embodiment 3;
Fig. 4 b is a nano-carbon tube load titanium dioxide compound photocatalytic degradation aqueous solution of methylene blue change curve in time among the embodiment 3;
Fig. 5 a is the ESEM behind the multiple-wall carbon nanotube carried titanium dioxide (SEM) figure among the embodiment 4;
Fig. 5 b is a nano-carbon tube load titanium dioxide compound photocatalytic degradation aqueous solution of methylene blue change curve in time among the embodiment 4;
Fig. 6 a is the ESEM behind the multiple-wall carbon nanotube carried titanium dioxide (SEM) figure among the embodiment 5;
Fig. 6 b is a nano-carbon tube load titanium dioxide compound photocatalytic degradation aqueous solution of methylene blue change curve in time among the embodiment 5;
Fig. 7 a is the ESEM behind the multiple-wall carbon nanotube carried titanium dioxide (SEM) figure among the embodiment 6;
Fig. 7 b is a nano-carbon tube load titanium dioxide compound photocatalytic degradation aqueous solution of methylene blue change curve in time among the embodiment 6.
The specific embodiment
Embodiment 1
With commercially available multiple-wall carbon nanotube be (about 20 ~ 30 nm of diameter, the about 20mm of length, purity〉95%) carry out acidification by usual method.Specific as follows: as earlier the mixed acid of 1.0 g multiple-wall carbon nanotubes with 50 mL sulfuric acid and nitric acid (volume ratio of sulfuric acid and nitric acid is 1 ︰ 3) to be mixed; The gained mixed liquor is at ultrasonic 20 min of room-temperature water bath, then 120
oBackflow stirring reaction 24 h about C wash with water until eluate pH after reaction finishes and approximate 7, get the CNT of acidified processing after the separation drying.
Be dispersed in the 20mL acetone solvent 0.5 g CNT of acidified processing is ultrasonic, 50% sulfuric acid that adds about 1 wt% of concentration then is controlled at 50 as catalyst with reaction temperature
oAbout C, slowly drip the mixed liquor of (about 1 hour) 5 mL butyl titanates and 20 mL isopropyl alcohols, drip the back and continue reaction 6 hours.Reaction finishes the back centrifugation, gets the CNT of carried titanium dioxide.Fig. 1 a is multiple-wall carbon nanotube transmission electron microscope (TEM) figure.Pure multiple-wall carbon nanotube smooth surface is clean.And the CNT composite surface of carried titanium dioxide is slightly made, and many concavo-convex positions are arranged on its surface, and this explanation has nano particle titanium dioxide attached to the CNT surface.The material of last step gained is carried out high-temperature process in air atmosphere, the high-temperature process temperature is 450
oC after the high-temperature process time is 2 hours, can get the photocatalyst material of nano-carbon tube load titanium dioxide.Fig. 1 b is depicted as ESEM (SEM) figure behind the multiple-wall carbon nanotube carried titanium dioxide.For determining the crystal formation of titanium dioxide on the nano-carbon tube load titanium dioxide compound, we have carried out X-ray diffraction analysis to prepared product, shown in Fig. 2 a, discovery equals 25.44,37.89,48.25,54.44,63.12,70.25 and 75.37 places at the angle of diffraction 2 θ the obvious diffraction peak, corresponding to the titanium dioxide crystal form of Detitanium-ore-type.
Utilize prepared nano-carbon tube load titanium dioxide compound to carry out the degradation of methylene blue aqueous solution for photochemical catalyst.Get catalyst 0.1 g of embodiment, put into the quartz container of the 100 mL aqueous solution of methylene blue (concentration is 30 mg/L) that configure, this quartz container is placed carry out the photocatalytic degradation reaction under the 500 W high-pressure sodium lamps again.With formula: R=(ρ
0ρ
i)/ρ
0* 100% calculates the degradation rate under the different time, wherein ρ
0Be aqueous solution of methylene blue, ρ
iBe the aqueous solution of methylene blue behind the degradation reaction certain hour.ρ
0And ρ
iCan measure λ by uv-vis spectra
MaxThe absorbance at=546 nm places is calculated according to calibration curve and is obtained.Nano-carbon tube load titanium dioxide compound photocatalytic degradation aqueous solution of methylene blue in time change curve shown in Fig. 2 b.The navy blue aqueous solution of methylene blue decoloured for the aqueous solution of alkalescence and neutrality substantially at pH after one hour, and relatively poor in the aqueous solution decolouring of acidity.
Embodiment 2
Method by embodiment 1 is carried out acidification to CNT.Be dispersed in the 20mL acetone solvent 0.5 g CNT of acidified processing is ultrasonic, the concentrated hydrochloric acid that adds about 1 wt% of concentration then is as catalyst, control reaction temperature about 30
oAbout C, slowly drip the mixed liquor of (about 1 hour) 5 mL metatitanic acid n-propyls and 20 mL isopropyl alcohols, drip the back and continue reaction 12 hours.Reaction finishes the back centrifugation, gets the CNT of carried titanium dioxide.The material of last step gained is carried out high-temperature process in air atmosphere, the high-temperature process temperature is 400
oC after the high-temperature process time is 3 hours, can get the photocatalyst material (the SEM figure shown in Fig. 3 a) of nano-carbon tube load titanium dioxide.
Utilize prepared nano-carbon tube load titanium dioxide compound to handle with embodiment 1 for photochemical catalyst carries out the degradation of methylene blue aqueous solution.The navy blue aqueous solution of methylene blue promptly can be observed obvious variable color in about 10 minutes at pH in for the alkalescence and the neutral aqueous solution, and at the aqueous solution variable color of acidity not obvious (shown in Fig. 3 b).
Method by embodiment 1 is carried out acidification to CNT.Be dispersed in the 20mL acetone solvent 0.5 g CNT of acidified processing is ultrasonic, the concentrated hydrochloric acid that adds about 1 wt% of concentration then is as catalyst, control reaction temperature about 60
oAbout C, slowly drip the mixed liquor of (about 1 hour) 2.5 mL butyl titanates and 2.5 mL isopropyl titanates and 20 mL isopropyl alcohols, drip the back and continue reaction 12 hours.Reaction finishes the back centrifugation, gets the CNT of carried titanium dioxide.The material of last step gained is carried out high-temperature process in air atmosphere, the high-temperature process temperature is 500
oC after the high-temperature process time is 1.5 hours, can get the photocatalyst material (the SEM figure shown in Fig. 4 a) of nano-carbon tube load titanium dioxide.
Utilize prepared nano-carbon tube load titanium dioxide compound to handle with embodiment 1 for photochemical catalyst carries out the degradation of methylene blue aqueous solution.The navy blue aqueous solution of methylene blue promptly can be observed obvious variable color in about 10 minutes at pH in for the alkalescence and the neutral aqueous solution, and degradation efficiency is higher, and not obvious in the aqueous solution variable color of acidity, degradation efficiency lower (shown in Fig. 4 b).
Embodiment 4
Method by embodiment 1 is carried out acidification to CNT.Be dispersed in the 20mL acetone solvent 0.5 g CNT of acidified processing is ultrasonic, 50% nitric acid that adds about 1 wt% of concentration then is as catalyst, control reaction temperature about 90
oAbout C, slowly drip the mixed liquor of (about 1 hour) 5 mL isopropyl titanates and 20 mL isopropyl alcohols, drip the back and continue reaction 2 hours.Reaction finishes the back centrifugation, gets the CNT of carried titanium dioxide.The material of last step gained is carried out high-temperature process in air atmosphere, the high-temperature process temperature is 500
oC after the high-temperature process time is 1.5 hours, can get the photocatalyst material of nano-carbon tube load titanium dioxide.But because reaction temperature is too high, hydrolysis reaction is too fast, and titanium dioxide can not be evenly distributed on the CNT surface and form gathering (the SEM figure shown in Fig. 5 a).
Utilize prepared nano-carbon tube load titanium dioxide compound to handle with embodiment 1 for photochemical catalyst carries out the degradation of methylene blue aqueous solution.The navy blue aqueous solution of methylene blue just can be observed obvious variable color in about 30 minutes at pH in for the alkalescence and the neutral aqueous solution, and degradation efficiency is lower, and constant substantially at the aqueous solution of acidity, degradation efficiency low (shown in Fig. 5 b).
Method by embodiment 1 is carried out acidification to CNT.Be dispersed in the 20mL acetone solvent 0.5 g CNT of acidified processing is ultrasonic, add the red fuming nitric acid (RFNA) of about 0.5 wt% of concentration and the concentrated sulfuric acid (volume ratio of the red fuming nitric acid (RFNA) and the concentrated sulfuric acid is 1:1) then as catalyst, control reaction temperature about 60
oAbout C, slowly drip the mixed liquor of (about 1 hour) 2.5 mL isopropyl titanates and 2.5 mL metatitanic acid n-propyls and 20 mL isopropyl alcohols, drip the back and continue reaction 10 hours.Reaction finishes the back centrifugation, gets the CNT of carried titanium dioxide.The material of last step gained is carried out high-temperature process in air atmosphere, the high-temperature process temperature is 250
oC after the high-temperature process time is 4 hours, can get the photocatalyst material of nano-carbon tube load titanium dioxide, and titanium dioxide can be evenly distributed on CNT surface (the SEM figure shown in Fig. 6 a).
Utilize prepared nano-carbon tube load titanium dioxide compound to handle with embodiment 1 for photochemical catalyst carries out the degradation of methylene blue aqueous solution.No matter in acidity still in alkaline solution, methylene blue solution variable color not obvious (shown in Fig. 6 b), this is because the high-temperature process temperature is low excessively, and titanium dioxide is converted into due to the anatase crystal with high catalytic activity.
Embodiment 6
Method by embodiment 1 is carried out acidification to CNT.Be dispersed in the 20mL acetone solvent 0.5 g CNT of acidified processing is ultrasonic, add the red fuming nitric acid (RFNA) of about 1 wt% of concentration and concentrated hydrochloric acid (volume ratio of red fuming nitric acid (RFNA) and concentrated hydrochloric acid is 1:1) then as catalyst, control reaction temperature about 60
oAbout C, slowly drip the mixed liquor of (about 1 hour) 2.5 mL butyl titanates and 2.5 mL isopropyl titanates and 20 mL isopropyl alcohols, drip the back and continue reaction 6 hours.Reaction finishes the back centrifugation, gets the CNT of carried titanium dioxide.The material of last step gained is carried out high-temperature process in air atmosphere, the high-temperature process temperature is 1000
oC after the high-temperature process time is 2 hours, can get the photocatalyst material of nano-carbon tube load titanium dioxide, and titanium dioxide can be evenly distributed on CNT surface (shown in Fig. 7 a).Utilize prepared nano-carbon tube load titanium dioxide compound to handle with embodiment 1 for photochemical catalyst carries out the degradation of methylene blue aqueous solution.No matter in acidity still in alkaline solution, methylene blue solution variable color not obvious (shown in Fig. 7 b), this is because the high-temperature process temperature is too high, makes titanium dioxide be converted into the rutile crystal type of low catalytic activity and can not be converted into due to the anatase crystal with high catalytic activity.
Claims (7)
1. the photochemical catalyst of a nano-carbon tube load titanium dioxide, it is characterized in that: the outer surface at CNT is attached with nano titanium oxide.
2. the preparation method of the photochemical catalyst of a nano-carbon tube load titanium dioxide is characterized in that comprising the steps:
(1) multiple-wall carbon nanotube is carried out acidification;
(2) CNT after the acidification is dispersed in the solvent, the back adds TiO 2 precursor and is hydrolyzed reaction to generate nano titanium oxide and to make the surface of nano titanium oxide attached to CNT;
(3) nano-sized carbon that will be attached with titanium dioxide is carried out high-temperature process, and making the crystal transfer of titanium dioxide is Detitanium-ore-type, thereby makes the photochemical catalyst of nano-carbon tube load titanium dioxide.
3. the preparation method of the photochemical catalyst of nano-carbon tube load titanium dioxide according to claim 2 is characterized in that: the described TiO 2 precursor of step (2) be in butyl titanate, isopropyl titanate, the metatitanic acid n-propyl any or appoint several.
4. the preparation method of the photochemical catalyst of nano-carbon tube load titanium dioxide according to claim 2 is characterized in that: the described hydrolysis of step (2) is to be catalyst with acid.
5. the preparation method of the photochemical catalyst of nano-carbon tube load titanium dioxide according to claim 4 is characterized in that: described acid catalyst be in sulfuric acid, hydrochloric acid, the nitric acid any or appoint several.
6. the preparation method of the photochemical catalyst of nano-carbon tube load titanium dioxide according to claim 2 is characterized in that: the hydrolysis temperature of the described hydrolysis of step (2) is 30 ~ 60
oC, hydrolysis time are 6 ~ 12 h.
7. the preparation method of the photochemical catalyst of nano-carbon tube load titanium dioxide according to claim 2 is characterized in that: the temperature of the described high-temperature process of step (3) is 350 ~ 500
oC, time are 2 ~ 4 h.
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| CN113289574A (en) * | 2020-02-23 | 2021-08-24 | 天津大学 | Titanium dioxide-carbon nanotube flexible composite film and preparation method and application thereof |
| CN113289574B (en) * | 2020-02-23 | 2022-06-03 | 天津大学 | Titanium dioxide-carbon nanotube flexible composite film and preparation method and application thereof |
| CN114289010A (en) * | 2022-01-10 | 2022-04-08 | 江苏南大华兴环保科技股份公司 | TiO 22-SnO2Composite photocatalyst and preparation method and application thereof |
| CN114289010B (en) * | 2022-01-10 | 2024-04-12 | 江苏南大华兴环保科技股份公司 | TiO (titanium dioxide) 2 -SnO 2 Composite photocatalyst, preparation method and application thereof |
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