CN1321741C - Carbon nano tube/zinc oxide composite powder with photocatalysis performance and method for preparing the same - Google Patents
Carbon nano tube/zinc oxide composite powder with photocatalysis performance and method for preparing the same Download PDFInfo
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- CN1321741C CN1321741C CNB2004100990239A CN200410099023A CN1321741C CN 1321741 C CN1321741 C CN 1321741C CN B2004100990239 A CNB2004100990239 A CN B2004100990239A CN 200410099023 A CN200410099023 A CN 200410099023A CN 1321741 C CN1321741 C CN 1321741C
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Abstract
The present invention provides a method for preparing carbon nanometer tube/zinc oxide composite powder with photocatalytic activity, which is mainly characterized in that an electronegative active group is successfully led on the surface of a carbon nanometer tube by using anionic surfactant as dispersant, and the structure of the carbon nanometer tube is not changed; furthermore, zinc salt and lithium hydroxide are used as raw materials for synthetizing zinc oxide, the composite powder of zinc oxide nanometer crystals covered on the surface of the carbon nanometer tube can be obtained by utilizing the electrostatic action of reaction ions and the active group and the chemical reaction among the reaction ions, and the diameter of crystal grains is about 5 to 10 nm. The prepared zinc oxide/carbon nanometer tube composite powder displays the hypochromatic shift effect in an ultraviolet-visible spectrum test, and the composite powder has the higher photocatalytic activity superior to pure zinc oxide powder by the indication of a photocatalysis test. The method is simple and effective and realizes the tight combination of matrix granules and the carbon nanometer tube, the prepared composite powder has the favorable photocatalytic activity, and the present invention is a good carbon nanometer tube composite material with high performance.
Description
Technical field
The invention relates to a kind of CNT/zinc oxide composite powder and preparation method with photocatalysis performance, the prepared catalyst harmful substance in the environment that can be used for degrading belongs to field of nanocomposite materials.
Technical background
Photochemical catalyst is one of most active research field of international academic community in recent years.Photocatalysis technology has broad application prospects at aspects such as environmental protection, solar energy utilization and new functional material exploitations, is the high-new shape art with substantial economics and social benefit.As effective catalyst support, the oxide catalyst carrier that carbon ratio is general has more excellent performance: (1) chemical inertness; (2) in the catalytic degradation process, provide more activity site and better dispersed.And in recent ten years, the appearance of CNT has promoted the application advantage of carbon as catalyst carrier again greatly.CNT is owing to have bigger specific area, and well chemical stability and high conductivity are more suitable in the carrier (Jitianu A, Cacciaguerra T, Benoit R, et al.Carbon., 2004,42,1147) of preparation semiconductor light-catalyst.Nano zine oxide is a kind of n type semi-conducting material, along with reducing of its particle size, and corresponding absorption spectrum generation blue shift, show quantum confined effect, be considered to one of high activated catalyst that has application prospect (Pal B, Sharon M.Mater.Chem.Phys., 2002,76,82).Therefore, CNT/zinc oxide composite powder will have broad application prospects aspect photochemical catalyst, be expected to become the novel photocatalysis agent with high catalytic activity.
The interface of CNT and matrix is one of most important link in the nanometer tube composite materials research.In the process of development carbon nano tube compound material, this research can guarantee in the carbon nano tube compound material structure that CNT follows the transmission of good electron is arranged between matrix.CNT is made up of single carbon atom, and the surface lacks active group, thereby will carry out chemical modification to its surface.Oxidizer treatment CNTs such as nitration mixture can be introduced active group on the surface, but the electronic structure of carbon pipe itself has been caused certain destruction.How, improve the interface binding ability of CNT and zinc oxide by rational finishing, and don't the electrical properties of destroying carbon nanometer tube itself, be an important research project.Introduce active group by the ion dispersant in carbon nano tube surface, in-situ deposition prepares carbon nano tube compound material, is the effective way that addresses this problem.
Summary of the invention
The object of the present invention is to provide a kind of CNT/zinc-oxide nano composite granule and preparation method with photocatalytic activity.
The objective of the invention is to implement: the electronic structure of introducing active group and don't change CNT by anionic dispersing agents in carbon nano tube surface by following manner, utilize the electrostatic interaction of the active group and the zinc ion of carbon nano tube surface, make the zinc ion original position be adsorbed in carbon nano tube surface, and then form the composite granule that the zinc oxide original position is covered in carbon nano tube surface.The method that is provided is simply effective, does not need special equipment, has realized combining closely of zinc oxide nanocrystalline and CNT, is the effective way that preparation has the CNT/zinc oxide composite powder of photocatalytic activity.
The invention is characterized in: successfully introducing active group with anion surfactant in carbon nano tube surface, is raw material with zinc salt, lithium hydroxide, and absolute ethyl alcohol is a solvent.By the electrostatic interaction of reactive ion and active group and the ionic bond effect between the reactive ion, zinc oxide nanocrystalline in-situ deposition, the intensive carbon nano tube surface that covers.
Concrete steps are:
(1) CNT is joined in anionic dispersing agents (as lauryl sodium sulfate, dodecyl sodium sulfate, a kind of in tiron or the polyacrylic acid) weak solution, the quality of anion surfactant is 0.5～2% of a CNT.Through ultrasonic dispersion in 0.5-2 hour, introduce the negative electrical charge active group in carbon nano tube surface it is carried out finishing, by the distilled water washing, 60～80 ℃ of vacuum dryings are standby then.
(2) 0.2g being joined concentration by the CNT of anionic dispersing agents modifying and decorating is 0.1～0.2mol L
-1In (zinc acetate, zinc nitrate, zinc chloride) ethanolic solution of zinc salt, and at 60～80 ℃ of backflow 3-6 hours.
(3) mixed solution that step (2) is obtained was 80～95 ℃ of distillations 3-8 hour.Zn
2+By electrostatic interaction and SO
4 2-, SO
3 2-Or COO
-In a kind of anionic group combination.
(4) with 0.1～0.25mol L
-1The ethanolic solution of lithium hydroxide dropwise is added in the mixed ethanol solution of step (3) gained, is reflected in 0 ℃ the ice-water bath to carry out OH
-Zn with carbon nano tube surface absorption
2+Carry out chemical reaction, thus original position synthesizing zinc oxide/carbon nano-tube composite powder.
(5) drip behind the lithium hydroxide solution and again this mixed solution is continued to stir 1 hour, react fully and carry out.Product respectively washs 3 times through ethanol, distilled water, promptly obtains the composite granule of zinc oxide nanocrystalline coated carbon nanotube after the drying.
The composite granule of prepared zinc oxide coated carbon nanotube is carried out the photocatalysis test, to test its photocatalytic activity.
(1) light-catalyzed reaction is carried out in self-control reactor (see figure 1), and reactor is three layers of concentric circles tubular glass container, the middle outstanding 300W medium pressure mercury lamp that has, and logical recirculated cooling water is a reactor in the middle of the interior overcoat in the inner sleeve.
(2) under magnetic agitation with composite granule and 20mg L
-1Methylene blue solution, adopt powerful the stirring to keep particle to be uniformly dispersed, uviol lamp is clock reaction after preheating, from reactor bottom cloth breather pipe with the certain flow aerating oxygen, with the residue percentage of the methylene blue after reaction a period of time, promptly react back methylene blue concentration C and initial concentration C
orecently weigh the particle photocatalytic activity.Centrifugal elimination compound powder particle is analyzed the methylene blue solution change in concentration.
Synthetic CNT/the zinc oxide composite powder of this method has the photocatalytic activity that is better than the pure zinc oxide powder, can be applicable to the processing of pollutant in the environment.
The characteristics of CNT provided by the invention/zinc-oxide nano composite granule and preparation method thereof are:
(1) successfully introducing active group with surfactant in carbon nano tube surface and can not change the structure of CNT, combines closely in the composite granule zinc oxide grain and the CNT interface of preparation.By the electrostatic interaction of reactive ion and active group and the ionic bond effect between the reactive ion, the zinc oxide in-situ deposition, cover carbon nano tube surface thick and fast.
(2) realized the effective coating of zinc oxide to CNT, the particle diameter of zinc oxide is about 5-10nm; The caliber of CNT is 20-30nm.
(3) preparation method is simply effective, need not special installation.
(4) realized effective degraded to the industrial dye methylene blue, its photocatalytic activity is doubled than pure zinc oxide powder.
Description of drawings
Fig. 1 makes jacket type ultraviolet catalytic reactor by oneself.
The X-ray diffraction spectrogram of Fig. 2 CNT/zinc oxide composite powder.
(a) CNT (b) CNT/zinc oxide composite powder
The transmission electron microscope photo of Fig. 3 CNT/zinc oxide composite powder.
Fig. 4 uv-visible absorption spectra, tangible blue shift phenomenon has taken place in the absorption spectrum of CNT/zinc oxide composite powder as can be seen from Figure.
(a) CNT (b) pure zinc oxide powder (c) CNT/zinc oxide composite powder.
The methylene blue degradation rate is over time under UV-irradiation for Fig. 5.CNT/zinc oxide composite powder is fast to the degradation speed of methylene blue as can be seen, and degradation amount is big, and its catalytic activity height is described.
(a) pure zinc oxide powder (b) CNT/zinc oxide composite powder (c) CNT.
The specific embodiment
Further specify embodiment and effect with following non-limiting embodiment:
CNT is added the 2wt% sodium dodecyl sulfate solution, and ultrasonic dispersion 2 hours is with distilled water washing, 60 ℃ of vacuum dryings.0.2 the carbon pipe after gram is handled adds in the 200ml 0.1M zinc acetate ethanolic solution, refluxes 3 hours in 80 ℃ of silicone oil baths.Then in 95 ℃, distilled 3 hours, naturally cool to room temperature then.100ml 0.14M lithium hydroxide ethanolic solution is dropwise joined in the above-mentioned mixed solution, be reflected in 0 ℃ of ice-water bath and carry out, drip the back and continue to stir 1 hour, carry out to guarantee sufficient reacting.Products therefrom promptly obtains the composite granule that zinc oxide is covered in carbon nano tube surface through ethanol, distilled water washing three times after the oven dry.Fig. 2 is the X-ray diffraction spectrogram of the prepared CNT/zinc oxide composite powder of present embodiment.The diffraction maximum that comprises carbon pipe and zinc oxide among the figure.Fig. 3 is the transmission electron microscope photo of CNT/zinc oxide composite powder.Zinc oxide nanocrystalline evenly is covered in carbon nano tube surface, and crystallite dimension is about 6nm.Prepared powder is carried out the uv-visible absorption spectra analysis, show, be shown in Fig. 4 with respect to the tangible blue shift phenomenon of pure zinc oxide powder.
Light-catalyzed reaction is carried out in self-control reactor (Fig. 1), and reactor is three layers of concentric circles tubular glass container, the middle outstanding 300W medium pressure mercury lamp that has, and logical recirculated cooling water is a reactor in the middle of the interior overcoat in the inner sleeve.Under magnetic agitation, 0.16g CNT/zinc oxide joined 400ml initial concentration C
o=20mg L
-1Methylene blue solution, the catalyst powder bulk concentration is 0.4g L
-1Adopt powerful the stirring to keep particle to be uniformly dispersed, uviol lamp is clock reaction after preheating, and with the certain flow aerating oxygen, oxygen flow is 10mL min from the reactor bottom gas distribution pipe
-1,, promptly react back methylene blue concentration C and initial concentration C with the residue percentage of methylene blue after reaction a period of time
orecently weigh the particle photocatalytic activity.Concrete grammar is for getting 4ml solution at regular intervals, concentration for ease of the test methylene blue, dilute 5 times, centrifugal elimination zinc oxide particle, on the ultraviolet-visible spectrometer in its UV absorption intensity of 650nm place test, thereby analyze methylene blue solution concentration rate, i.e. Fig. 5 over time.Prepared CNT/zinc oxide composite powder demonstrates the photocatalytic activity that doubles than pure zinc oxide powder.
CNT is added the 2wt% polyacrylic acid solution, and ultrasonic dispersion 2 hours is with distilled water washing, 80 ℃ of vacuum dryings.0.2 the carbon pipe after gram is handled adds in the 200ml 0.1M zinc nitrate ethanolic solution, refluxes 6 hours in 60 ℃ of silicone oil baths.Then in 80 ℃, distilled 8 hours, naturally cool to room temperature then.100ml 0.14M lithium hydroxide ethanolic solution is dropwise joined in the above-mentioned mixed solution, be reflected in 0 ℃ of ice-water bath and carry out, drip the back and continue to stir 1 hour, carry out to guarantee sufficient reacting.Products therefrom promptly obtains the composite granule that zinc oxide closely is covered in carbon nano tube surface through ethanol, distilled water washing three times after the oven dry.The ZnO crystal grain diameter is 10nm in the gained composite granule, the intensive surface that caliber is the CNT of 20-30nm (as shown in Figure 3) that covers.All the other are with embodiment 1.
Embodiment 3
CNT is added 1wt% tiron solution, and ultrasonic dispersion 2 hours is with distilled water washing, 60 ℃ of vacuum dryings.0.2 the carbon pipe after gram is handled adds in the 200ml 0.1M zinc chloride ethanolic solution, refluxes 6 hours in 60 ℃ of silicone oil baths.Then in 90 ℃, distilled 5 hours, naturally cool to room temperature then.100ml 0.14M lithium hydroxide ethanolic solution is dropwise joined in the above-mentioned mixed solution, be reflected in 0 ℃ of ice-water bath and carry out, drip the back and continue to stir 1 hour, carry out to guarantee sufficient reacting.Products therefrom promptly obtains the composite granule that zinc oxide closely is covered in carbon nano tube surface through ethanol, distilled water washing three times after the oven dry.All the other are with embodiment 1.
Claims (8)
1. CNT/zinc-oxide nano composite granule is characterized in that zinc oxide nanocrystalline in-situ deposition, the intensive surface that covers CNT, and the zinc oxide nanocrystalline crystal grain diameter is 5～10nm.
2. by the described CNT of claim 1/zinc-oxide nano composite granule, it is characterized in that described CNT caliber is 20-30nm.
3. the preparation method who prepares CNT as claimed in claim 1/zinc-oxide nano composite granule is characterized in that concrete steps are:
(a) CNT ultrasonic time in dispersant solution is 0.5-2 hour, the quality of dispersant is 0.5～2% of a CNT quality, introduce electronegative active group in carbon nano tube surface, and through the distilled water washing, 60～80 ℃ of vacuum drying can get the anionic dispersing agents modified carbon nanotube;
(b) the CNT 0.2g of the anionic dispersing agents modifying and decorating of gained in the step (a) being joined concentration is 0.1～0.2mol L
-1In the ethanolic solution of zinc salt, refluxed Zn 3～6 hours at 60～80 ℃
2+Combine with anionic group by electrostatic interaction;
(c) gained mixed solution in the step (b) was distilled in 80～95 ℃ 3～8 hours, obtain the mixed ethanol solution of CNT and zinc ion;
(d) with 0.1～0.25mol L
-1The lithium hydroxide ethanolic solution dropwise joins in step (c) the gained solution, is reflected in 0 ℃ of ice-water bath and carries out OH
-Zn with carbon nano tube surface absorption
2+Carry out chemical reaction, thus reaction in-situ synthesizing zinc oxide/carbon nano-tube composite powder; Product respectively washs 3 times through ethanol, distilled water, promptly obtains the composite granule of zinc oxide nanocrystalline coated carbon nanotube after the drying.
4. by the preparation method of the described CNT of claim 3/zinc oxide nanocrystalline coated carbon nanometer composite powder, again this mixed solution is continued to stir 1 hour after it is characterized in that dripping lithium hydroxide solution, carry out to guarantee sufficient reacting.
5. by the preparation method of the described CNT of claim 3/zinc oxide nanocrystalline coated carbon nanometer composite powder, it is characterized in that described anionic dispersing agents is a lauryl sodium sulfate, dodecyl sodium sulfate, a kind of in polyacrylic acid or the tiron.
6. by the preparation method of the described CNT of claim 3/zinc oxide nanocrystalline coated carbon nanometer composite powder, it is characterized in that described zinc salt is a kind of in zinc acetate, zinc chloride or the zinc nitrate.
7. by the preparation method of the described CNT of claim 3/zinc oxide nanocrystalline coated carbon nanometer composite powder, it is characterized in that described anionic group is SO
4 2-, SO
3 2-Or COO
-In a kind of.
8. the described CNT of claim 1/zinc-oxide nano composite granule is applied to effective degraded of industrial dye methyl orchid, and its photocatalytic activity doubles than pure zinc oxide powder.
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| CN109777243A (en) * | 2019-03-26 | 2019-05-21 | 马鞍山采石矶涂料有限公司 | A kind of preparation method of zinc oxide composite photocatalyst coating |
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| CN100396373C (en) * | 2006-06-22 | 2008-06-25 | 厦门大学 | Method for preparing carbon nanometer tube/titanium dioxide composite photocatalyst |
| CN101024579B (en) * | 2006-12-29 | 2012-04-11 | 中国科学院上海硅酸盐研究所 | Method for surface fit metn of inorganic nano particles on carbon nano tube |
| TWI393669B (en) * | 2009-04-10 | 2013-04-21 | Hon Hai Prec Ind Co Ltd | Carbon nanotube composite and method for making the same |
| CN101947442B (en) * | 2010-09-07 | 2012-11-28 | 桂林理工大学 | Method for synthesizing nano zinc oxide/bamboo charcoal photocatalysis material by precipitation and impregnation |
| CN102350337B (en) * | 2011-08-02 | 2013-05-01 | 武汉大学 | Method for preparing ZnO/rectorite/carbon nano tube composite material |
| CN111926564A (en) * | 2020-08-27 | 2020-11-13 | 秦小康 | Preparation method of novel fiber and novel antibacterial fabric |
| CN112138646A (en) * | 2020-09-07 | 2020-12-29 | 淮阴工学院 | Preparation method of ZnO/CNTS nano photocatalytic composite material |
| CN114656864B (en) * | 2022-04-05 | 2022-09-27 | 江苏师范大学 | Super-hydrophobic magnesium alloy coating and process thereof |
| CN115254089A (en) * | 2022-07-21 | 2022-11-01 | 湖北展鹏电子材料有限公司 | Carbon nanotube-based-TiO2Composite nano material and preparation method and application thereof |
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|---|---|---|---|---|
| US5527519A (en) * | 1992-12-18 | 1996-06-18 | Bayer Aktiengesellschaft | Finely divided, highly pure neutral zinc oxide powder, a process for its preparation and its use |
| CN1396117A (en) * | 2002-06-13 | 2003-02-12 | 山东小鸭集团有限责任公司 | Process for preparing nano zinc oxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5527519A (en) * | 1992-12-18 | 1996-06-18 | Bayer Aktiengesellschaft | Finely divided, highly pure neutral zinc oxide powder, a process for its preparation and its use |
| CN1396117A (en) * | 2002-06-13 | 2003-02-12 | 山东小鸭集团有限责任公司 | Process for preparing nano zinc oxide |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109777243A (en) * | 2019-03-26 | 2019-05-21 | 马鞍山采石矶涂料有限公司 | A kind of preparation method of zinc oxide composite photocatalyst coating |
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