CN102205238A - Method for preparing MWCNTs/ZnO (multi-wall carbon nano tubes/zinc oxide) nanometer composite material - Google Patents
Method for preparing MWCNTs/ZnO (multi-wall carbon nano tubes/zinc oxide) nanometer composite material Download PDFInfo
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Abstract
The invention relates to a method for preparing a MWCNTs/ZnO (multi-wall carbon nano tubes/zinc oxide) nanometer composite material, which comprises the following steps: (1) mixing MWCNTs with strong oxidizing acids according to a mass ratio of (1:200)-(1:400), acidizing the MWCNTs after ultrasonically dispersing, and then washing, drying and grinding the MWCNTs after acidizing, thereby acquiring the acidized MWCNTs; and (2) adding ethanediol, anhydrous sodium acetate, a zinc salt and a dispersing agent into the acidized MWCNTs, ultrasonically stirring for 1-3 hours, and then reacting for 12-18 hours at 150-180 DEG C, and lastly washing and drying a product, thereby acquiring the MWCNTs/ZnO nanometer composite material. The process is simple and the industrial production is easily achieved. The prepared MWCNTs/ZnO nanometer composite material has the advantages of pure crystalline phase, excellent dispersibility, good photochemical catalysis, and wide application prospect.
Description
Technical field
The invention belongs to the preparation field of nano composite material, particularly a kind of preparation method of MWCNTs/ZnO nano composite material.
Background technology
Zinc oxide (ZnO) is as a kind of wide bandgap semiconductor (energy gap is 3.37eV), except can being widely used in rubber additive, gas sensor, UV-preventing material, transformer and multiple Optical devices, also has photocatalysis performance, can be that light source comes degradable organic pollutant with the sunshine, this will make it play an important role aspect environmental pollution improvement.Under the irradiation of sunlight, its energy decomposing organic matter, and have antibiotic and deodorization.This photocatalysis property has been widely used in the industry such as fiber, cosmetics, pottery, environmental project and building materials.CNT has particular structure, nano level size, high effective ratio area and can present property of conductor.Because it has great specific area and chemical stability, and unique electronic structure, vestibule structure and absorption property, also be considered to a kind of good carrier.The luminal structure of the uniqueness of CNT particularly, the efficient of raising catalyst that can be to a great extent.
At present, the MWCNTs/ZnO nano composite material has multiple preparation method, comprising: chemical vapour deposition technique (CVD), and plasma enhanced chemical vapor deposition method (PECVD), water oil microemulsion liquid method, hydro-thermal method, non-covalent bond is legal etc.Kim etc. are at Applied Physics Letters, and 81,2085, reported on (2002) that the method by CVD prepares the MWCNTs/ZnO nano composite material.Zhu etc. are at Advanced Materials, 587-592, (2006) reported on and adopted the method for PECVD to prepare the MWCNTs/ZnO nano-powder, and by the time of directly change ZnO coating and the thickness of coating film, average grain diameter and the grain spacing of control ZnO.Sun etc. are at Chemical Communications, and 7, reported on the 832-833 (2004) that the method for water oil microemulsion liquid has prepared the MWCNTs/ZnO nano composite material.Byrappa etc. are at Journal of Materials Science, 43, reported on the 2348-2355 (2008) and utilized Hydrothermal Preparation MWCNTs/ZnO nano composite material, and the experiment confirm by the catalysis methylene blue MWCNTs/ZnO nano composite material compare with nano-ZnO, photocatalytic activity obviously improves.Still being difficult ethylene glycol at present is solvent, and polyethylene glycol-200 prepares the report of MWCNTs/ZnO nano composite material for the solvent-thermal method of surfactant.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method of MWCNTs/ZnO nano composite material, and this method technology is simple, is easy to suitability for industrialized production; Pure, the good dispersion of MWCNTs/ZnO nano composite material crystalline phase of preparation, photocatalytic are good, have a good application prospect.
The preparation method of a kind of MWCNTs/ZnO nano composite material of the present invention comprises:
(1) multi-walled carbon nano-tubes (MWCNTs) was mixed by mass ratio with acid with strong oxidizing property in 1: 200～1: 400, acidification is carried out to multi-walled carbon nano-tubes in ultrasonic dispersion back; Multi-walled carbon nano-tubes after acid treatment washing back is dry, grind and obtain acid-treated multi-walled carbon nano-tubes;
(2) in above-mentioned acid-treated multi-walled carbon nano-tubes, add ethylene glycol, anhydrous sodium acetate, zinc salt and dispersant again, wherein, the mass ratio of multi-walled carbon nano-tubes and ZnO (is the quality of ZnO with the mass conversion of zinc salt) is 0.14: 1～0.22: 1, the mass volume ratio of multi-walled carbon nano-tubes and ethylene glycol is 1.2～1.5mg: 1mL, the mass ratio of anhydrous sodium acetate and ZnO is 21.2: 1～28.2: 1, and the volume ratio of dispersant and ethylene glycol is 0.02: 1～0.04: 1; , that the product washing is dry behind the ultrasonic agitation 1-3h in 150～180 ℃ of reaction 12～18h, promptly get the MWCNTs/ZnO nano composite material.
Acid with strong oxidizing property in the described step (1) is red fuming nitric acid (RFNA), the concentrated sulfuric acid or both mixed acid, and concentration is 16～19mol/L, preferred red fuming nitric acid (RFNA).
Ultrasonic jitter time in the described step (1) is 30～60min, and the acidification temperature is 100～120 ℃, and the processing time is 18～30h.
Washing in the described step (1) is for spending the deionised water product 3～7 times, absolute ethanol washing 3～6 times; Drying is in 50～60 ℃ of dry 18-36h.
Zinc salt in the described step (2) is zinc acetate, zinc nitrate, zinc chloride or zinc sulfate, preferred zinc nitrate.
Dispersant in the described step (2) is a Macrogol 200.
Washing in the described step (2) is for spending the deionised water product 3～6 times, absolute ethanol washing 4～7 times; Drying is in 50～70 ℃ of dry 12-24h.
Beneficial effect
Technology of the present invention is simple, is easy to suitability for industrialized production; Pure, the good dispersion of MWCNTs/ZnO nano composite material crystalline phase of preparation, photocatalytic are good, have a good application prospect.
Description of drawings
Fig. 1 is the X-ray diffractogram of MWCNTs/ZnO nano composite material;
Fig. 2 is a MWCNTs/ZnO nano composite material electron scanning micrograph;
Fig. 3 is that MWCNTs/ZnO nano composite material and pure ZnO nano particle are to methylene blue degraded light-catalyzed reaction concentration and the change curve of time;
Fig. 4 is a MWCNTs/ZnO nano composite material degradation of methylene blue different time sections sample uv-vis spectra.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
Take by weighing 0.1g MWCNTs and add three-neck flask, add 16mol/L red fuming nitric acid (RFNA) 50mL again, ultrasonic dispersion 40min is warming up to 100 ℃, acidification reaction 18h then.Reaction finishes the back cleans 3 times with ethanol MWCNTs suspension, and washed with de-ionized water 6 times is taken out after placing drying baker inner drying 18h, grinds and obtains acid treatment MWCNTs.Take by weighing acid treatment MWCNTs0.06g, add in the there-necked flask, adding ethylene glycol again is 50mL, and anhydrous sodium acetate is 3.6g, and zinc nitrate is 1.487g, and polyethylene glycol-200 is 1mL, and ultrasonication disperses 1h down.Subsequently above-mentioned reactant liquor is added in the reactor.Reactor is placed in the baking oven, be warming up to 150 ℃, reaction 12h.Question response finishes, washed with de-ionized water 3 times, and ethanol cleans 4 times, dries 12h in 50 ℃ in the baking oven, takes out to grind promptly to obtain MWCNTs/ZnO nano composite material sample.Fig. 1 is the X-ray diffractogram of the synthetic MWCNTs/ZnO nano composite material of present embodiment, can obviously find out the characteristic peak of ZnO and MWCNTs, and do not find other obviously assorted peaks, thereby the sample that preliminary judgement obtains is the MWCNTs/ZnO nano composite material.Fig. 2 is a MWCNTs/ZnO nano composite material sample stereoscan photograph, has ZnO nano particle coating situation better as can be seen, and particle diameter is at 50～100nm.Fig. 3 be MWCNTs/ZnO nano composite material and pure ZnO nano particle to methylene blue degraded light-catalyzed reaction concentration and the change curve of time, the photocatalysis efficiency of MWCNTs/ZnO nano composite material is apparently higher than the photocatalysis efficiency of pure ZnO particle as can be seen.Fig. 4 is a MWCNTs/ZnO nano composite material degradation of methylene blue different time sections sample uv-vis spectra, and preceding as can be seen 30min MWCNTs is very strong to the suction-operated of methylene blue, and photocatalysis effect subsequently is also fine.
Embodiment 2
Take by weighing 0.12g MWCNTs and add three-neck flask, add 17mol/L red fuming nitric acid (RFNA) 50mL again, ultrasonic dispersion 30min is warming up to 110 ℃, acidification reaction 24h then.Reaction finishes the back cleans 4 times with ethanol MWCNTs suspension, and washed with de-ionized water 4 times is taken out after placing drying baker inner drying 20h, grinds and obtains acid treatment MWCNTs powder.Take by weighing acid treatment MWCNTs 0.08g, add in the there-necked flask, adding ethylene glycol again is 60mL, and anhydrous sodium acetate is 4.32g, and zinc nitrate is 1.784g, and polyethylene glycol-200 is 1mL, and ultrasonication disperses 1.5h down.Subsequently above-mentioned reactant liquor is poured in the reactor.Reactor is placed in the baking oven, be warming up to 160 ℃, reaction 15h.Question response finishes, washed with de-ionized water 4 times, and ethanol cleans 5 times, dries 18h in 50 ℃ in the baking oven, takes out to grind promptly to obtain MWCNTs/ZnO nano composite material sample.The test result of XRD shows the characteristic peak that can obviously find out ZnO and MWCNTs, and does not find other obviously assorted peaks, thereby the sample that preliminary judgement obtains is the MWCNTs/ZnO nano composite material.Scanning electron microscopic observation shows that ZnO nano particle coating situation is better, and particle diameter is at 50～100nm.
Embodiment 3
Take by weighing 0.15g MWCNTs and add three-neck flask, add 18mol/L red fuming nitric acid (RFNA) 60mL again, ultrasonic dispersion 50min is warming up to 120 ℃, acidification reaction 28h then.Reaction finishes the back cleans 5 times with ethanol MWCNTs suspension, and washed with de-ionized water 5 times is taken out after placing drying baker inner drying 24h, grinds and obtains acid treatment MWCNTs powder.Take by weighing acid treatment MWCNTs 0.1g, add in the there-necked flask, adding ethylene glycol again is 80mL, and anhydrous sodium acetate is 5.4g, and zinc nitrate is 2.230g, and polyethylene glycol-200 is 1.5mL, and ultrasonication disperses 2h down.Subsequently above-mentioned reactant liquor is poured in the reactor.Reactor is placed in the baking oven, be warming up to 170 ℃, reaction 12h.Question response finishes, washed with de-ionized water 5 times, and ethanol cleans 6 times, dries 18h in 60 ℃ in the baking oven, takes out to grind promptly to obtain MWCNTs/ZnO nano composite material sample.The test result of XRD shows the characteristic peak that can obviously find out ZnO and MWCNTs, and does not find other obviously assorted peaks, thereby the sample that preliminary judgement obtains is the MWCNTs/ZnO nano composite material.MWCNTs/ZnO nano composite material and pure ZnO nano particle are to methylene blue degraded light-catalyzed reaction test shows, and the photocatalysis efficiency of MWCNTs/ZnO nano composite material sample is apparently higher than the photocatalysis efficiency of pure ZnO particle.
Embodiment 4
Take by weighing 0.2g MWCNTs and add three-neck flask, add 19mol/L concentrated sulfuric acid 60mL again, ultrasonic dispersion 60min is warming up to 120 ℃, acidification reaction 30h then.Reaction finishes the back cleans 7 times with ethanol MWCNTs suspension, and washed with de-ionized water 6 times is taken out after placing drying baker inner drying 36h, grinds and obtains acid treatment MWCNTs powder.Take by weighing acid treatment MWCNTs 0.15g, add in the there-necked flask, adding ethylene glycol again is 100mL, and anhydrous sodium acetate is 7.2g, and zinc sulfate is 2.974g, and polyethylene glycol-200 is 2mL, and ultrasonication disperses 3h down.After treating to dissolve fully, more above-mentioned reactant liquor is poured in the reactor.Reactor is placed in the baking oven, be warming up to 180 ℃, reaction 18h.Question response finishes, washed with de-ionized water 6 times, and ethanol cleans 7 times, dries 24h in 70 ℃ in the baking oven, takes out to grind promptly to obtain MWCNTs/ZnO nano composite material sample.Scanning electron microscopic observation shows that ZnO nano particle coating situation is better.30min MWCNTs is very strong to the suction-operated of methylene blue before the test of MWCNTs/ZnO nano composite material degradation of methylene blue different time sections sample uv-vis spectra and different time sections photocatalytic degradation methylene blue as can be seen, and photocatalysis effect subsequently is also fine.
Claims (7)
1. the preparation method of a MWCNTs/ZnO nano composite material comprises:
(1) multi-walled carbon nano-tubes was mixed by mass ratio with acid with strong oxidizing property in 1: 200～1: 400, acidification is carried out to multi-walled carbon nano-tubes in ultrasonic dispersion back; Multi-walled carbon nano-tubes after acid treatment washing back is dry, grind and obtain acid-treated multi-walled carbon nano-tubes;
(2) in above-mentioned acid-treated multi-walled carbon nano-tubes, add ethylene glycol, anhydrous sodium acetate, zinc salt and dispersant again, wherein, the mass ratio of multi-walled carbon nano-tubes and ZnO is 0.14: 1～0.22: 1, the mass volume ratio of multi-walled carbon nano-tubes and ethylene glycol is 1.2～1.5mg: 1mL, the mass ratio of anhydrous sodium acetate and ZnO is 21.2: 1～28.2: 1, and the volume ratio of dispersant and ethylene glycol is 0.02: 1～0.04: 1; , that the product washing is dry behind the ultrasonic agitation 1-3h in 150～180 ℃ of reaction 12～18h, promptly get the MWCNTs/ZnO nano composite material.
2. the preparation method of a kind of MWCNTs/ZnO nano composite material according to claim 1 is characterized in that: the acid with strong oxidizing property in the described step (1) is red fuming nitric acid (RFNA), the concentrated sulfuric acid or both mixed acid, and concentration is 16～19mol/L.
3. the preparation method of a kind of MWCNTs/ZnO nano composite material according to claim 1 is characterized in that: the ultrasonic jitter time in the described step (1) is 30～60min, and the acidification temperature is 100～120 ℃, and the processing time is 18～30h.
4. the preparation method of a kind of MWCNTs/ZnO nano composite material according to claim 1 is characterized in that: the washing in the described step (1) is for spending the deionised water product 3～7 times, absolute ethanol washing 3～6 times; Drying is in 50～60 ℃ of dry 18-36h.
5. the preparation method of a kind of MWCNTs/ZnO nano composite material according to claim 1 is characterized in that: the zinc salt in the described step (2) is zinc acetate, zinc nitrate, zinc chloride or zinc sulfate.
6. the preparation method of a kind of MWCNTs/ZnO nano composite material according to claim 1 is characterized in that: the dispersant in the described step (2) is a Macrogol 200.
7. the preparation method of a kind of MWCNTs/ZnO nano composite material according to claim 1 is characterized in that: the washing in the described step (2) is for spending the deionised water product 3～6 times, absolute ethanol washing 4～7 times; Drying is in 50～70 ℃ of dry 12-24h.
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Cited By (8)
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| CN102397553A (en) * | 2011-11-24 | 2012-04-04 | 中国药科大学 | Method for improving drug release in carbon nano tube drug delivery system by displacement object |
| CN106243639A (en) * | 2016-07-29 | 2016-12-21 | 佛山市高明区诚睿基科技有限公司 | A kind of can the 3D printing PBS composite wire of sensitization discoloration |
| CN106977956A (en) * | 2017-03-03 | 2017-07-25 | 深圳市佩成科技有限责任公司 | The preparation method of ZnO/MWCNTs composites |
| CN107552035A (en) * | 2017-09-07 | 2018-01-09 | 张家港市山牧新材料技术开发有限公司 | A kind of preparation method of zinc oxide carbon nano tube compound material |
| WO2018157402A1 (en) * | 2017-03-03 | 2018-09-07 | 深圳市佩成科技有限责任公司 | Preparation method for zno/mwcnts composite material |
| CN109192522A (en) * | 2018-08-06 | 2019-01-11 | 杭州电子科技大学 | Fe2O3Nano carbon tube composite material, preparation method thereof and super capacitor |
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| CN114656864A (en) * | 2022-04-05 | 2022-06-24 | 江苏师范大学 | Super-hydrophobic magnesium alloy coating and process thereof |
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| CN102397553A (en) * | 2011-11-24 | 2012-04-04 | 中国药科大学 | Method for improving drug release in carbon nano tube drug delivery system by displacement object |
| CN102397553B (en) * | 2011-11-24 | 2013-05-22 | 中国药科大学 | Method for improving drug release in carbon nano tube drug delivery system by displacement object |
| CN106243639A (en) * | 2016-07-29 | 2016-12-21 | 佛山市高明区诚睿基科技有限公司 | A kind of can the 3D printing PBS composite wire of sensitization discoloration |
| CN106977956A (en) * | 2017-03-03 | 2017-07-25 | 深圳市佩成科技有限责任公司 | The preparation method of ZnO/MWCNTs composites |
| WO2018157402A1 (en) * | 2017-03-03 | 2018-09-07 | 深圳市佩成科技有限责任公司 | Preparation method for zno/mwcnts composite material |
| CN106977956B (en) * | 2017-03-03 | 2019-10-29 | 深圳市佩成科技有限责任公司 | The preparation method of ZnO/MWCNTs composite material |
| CN107552035A (en) * | 2017-09-07 | 2018-01-09 | 张家港市山牧新材料技术开发有限公司 | A kind of preparation method of zinc oxide carbon nano tube compound material |
| CN109192522A (en) * | 2018-08-06 | 2019-01-11 | 杭州电子科技大学 | Fe2O3Nano carbon tube composite material, preparation method thereof and super capacitor |
| CN111570815A (en) * | 2020-04-28 | 2020-08-25 | 天津大学 | Synthesis method of Ru nano-particle carboxylation |
| CN114656864A (en) * | 2022-04-05 | 2022-06-24 | 江苏师范大学 | Super-hydrophobic magnesium alloy coating and process thereof |
| CN114656864B (en) * | 2022-04-05 | 2022-09-27 | 江苏师范大学 | Super-hydrophobic magnesium alloy coating and process thereof |
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Application publication date: 20111005 |