CN102877151A - Preparation method of CdS/carbon nano tube/polyacrylonitrile hybrid nano-fiber - Google Patents
Preparation method of CdS/carbon nano tube/polyacrylonitrile hybrid nano-fiber Download PDFInfo
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Abstract
The invention relates to a preparation method of CdS/carbon nano tube/polyacrylonitrile hybrid nano-fiber. The technical scheme is as follows: the preparation method comprises the following steps: by taking CdCl2, Na2S and 2-mercaptoethanol as raw materials, and N,N-dimethylformamide (DMF) and water as solvents, synthesizing CdS-OH/DMF suspension; uniformly dispersing the carbon nano tube (CNT) in the CdS-OH/DMF suspension through ultrasonic, slowly stirring CNT/Cds-OH/DMF suspension into the prepared polyacrylonitrile/DMF solution, stirring and ultrasonically treating to obtain mixed spinning liquid; and obtaining the hybrid nano-fiber by adopting an electrostatic spinning technology. According to the invention, a solution growth method and the electrostatic spinning method are combined, the process is simple, and the prepared hybrid nano-fiber has the characteristics of large specific surface area and good mechanical property. Meanwhile, the preparation method has efficient performance of photocatalytic degradation of organic dye, and the hybrid nano-fiber is easier to recycle than a powdery photocatalytic material.
Description
Technical field
The present invention relates to field of nanometer material technology, be specifically related to a kind of preparation method of CdS-OH/ carbon nanotube/polypropylene nitrile Hybrid nanofibers.This Hybrid nanofibers material can be used for catalysis material.
Background technology
Cadmium sulfide (CdS) nano particle is a kind of semi-conducting material of very important II-VI family, and band-gap energy at room temperature is 2.42eV.CdS has non-linear optical property, fluorescence property and quantum size effect, thereby has obtained scientific research personnel's broad research.The CdS nano particle has very large specific area, reunites easily.For fear of the generation of reuniting, the form of how controlling nano particle with stabilizing agent has become an important research topic, and realistic problem in the urgent need to address in actual applications.Wherein a kind of synthetic method of very simple gentleness is exactly at room temperature 2 mercapto ethanol (ME) to be obtained to disperse CdS nano particle (CdS-OH) (Feng etc. by the list of hydroxyl modified as organic ligand, CdS nanoparticles chemically modified PAN functional materials:preparation and nonlinear optical properties, Eur. Polym. J., 2009,45,1058-1064).
In order to keep even further improve the excellent properties of CdS nano particle, a kind of effective technology combines CdS nano particle and polymer exactly, makes hybrid inorganic-organic materials.Polymer is not only as a carrier, and can stop the reunion of CdS nano particle, size and the distribution of control nano particle and the photostability of improving them.It is tens to the polymer nanofibers of hundreds of nanometer that method of electrostatic spinning can be prepared diameter easily, and its productive rate is higher, can satisfy the application at aspects such as filtration, catalysis, compound and timbering materials.The topmost characteristics of nanofiber are exactly to have high surface area and large draw ratio.In order to utilize fully these characteristics, people have combined by method of electrostatic spinning and solution infusion method and have prepared CdS/ polyacrylonitrile (PAN) Hybrid nanofibers at present, but because CdS introduces the nanofiber surface by infusion method, the bond strength of CdS and PAN nanofiber is lower on the one hand, in use easily come off, on the other hand, agglomeration easily occurs in the CdS particle that infusion method obtains, granular size is tens to hundreds of nanometer (Yang etc., Electrospinning of carbon/CdS coaxial nanofibers with photoluminescence and conductive properties, Mater Sci Eng B-Adv., 2007,140,48-52).And the CdS-OH nano particle (5 nm) that adopts solution growth method to make is made spinning solution jointly with PAN, the CdS-OH/PAN Hybrid nanofibers that obtains through electrostatic spinning more then not only can guarantee stable the combining of CdS-OH nano particle and PAN, and the reunion (Wang etc. of CdS-OH nano particle have effectively been prevented, Fabrication and characterization of electrospun CdS-OH/polyacrylonitrile hybrid nanofibers, Composites Part A, 2012,43,1869-1876).On this basis, in spinning solution, mix CNT (CNT), make the spinning solution that contains CdS-OH, CNT and these three kinds of components of PAN, obtain the CdS-OH/CNT/PAN Hybrid nanofibers of ternary by method of electrostatic spinning.Just be subject to people's favor because of its excellent mechanical performance, high electrical conductivity, high chemical stability and large specific area since the CNT self-discovery.Therefore, the adding of CNT makes Hybrid nanofibers on the high-specific surface area, CdS-OH nano particle low dimensional and the equally distributed basis that guarantee material, the good electric conductivity of CNT has been strengthened again the light induced electron hole right separation of its CdS-OH nano particle under illumination condition, has further improved its light and has urged efficient.The present invention is with CdCl
2, Na
2S, ME, CNT and PAN are raw material, combine by solution growth method and method of electrostatic spinning, prepared ternary CdS-OH/CNT/PAN Hybrid nanofibers, compare with the hybrid inorganic-organic materials of conventional method preparation, Hybrid nanofibers has high-specific surface area and draw ratio, the low dimensional of CdS-OH nano particle and evenly distribution, the electrical conductance of CNT suppresses the right superiority such as hydridization in light induced electron hole.And this Hybrid nanofibers is easier to later on recycle in light-catalyzed reaction.
Summary of the invention
The present invention utilizes the preparation that combines of solution growth method and method of electrostatic spinning to have light and urge degradation property, the CdS-OH/CNT/PAN Hybrid nanofibers that is easy to recycle.Utilizing the average diameter of the CdS-OH/ CNT/PAN Hybrid nanofibers of this method preparation is 310 nm, and the average diameter of the CdS-OH nano particle of Hybrid nanofibers inside is about 5 nm.The diameter of nanofiber can be realized by adjusting the conditions such as concentration of dope, nozzle diameter, nozzle and receiver distance.
For realizing that the technical scheme that the object of the invention adopts is:
(1) preparation of CdS-OH/DMF suspension
1. under magnetic agitation, DMF (DMF) solution of 30 mL is dropwise joined the CdCl of 3 mL
2The aqueous solution in, stir 10min, obtain A solution.
Described DMF solution contains the 2 mercapto ethanol of 5 mmol, described CdCl
2The aqueous solution in contain the CdCl of 2.5 mmol
2
2. with the Na of 3 mL
2The aqueous solution of S dropwise joins in the A solution, and mixing is mixed with mixed solution, and at this moment, water white mixed solution elder generation's yellowing also becomes muddy gradually.Leave standstill, 30 ℃ of lower reactions 4～5.5 hours, the yellow solution clear that again becomes obtained B solution.
Described Na
2Contain 1.5 mmol Na in the aqueous solution of S
2S.
3. B solution is transferred to and under 85～92 ℃, carried out decompression distillation on the Rotary Evaporators, except anhydrating.In the process of decompression distillation, therefore NaCl, just obtains the CdS-OH/DMF suspension of clear because being insoluble to DMF Precipitation from solution by the centrifugal NaCl that removes Precipitation.
(2) preparation of electrostatic spinning liquid
1. PAN is dissolved in the solution of making clarification among 65 ℃ of DMF, will makes C solution in acetone and cetrimonium bronmide (CTAB) the adding solution afterwards.PAN in the C solution, mass concentration is 11%, acetone quality concentration is that 6.1%, CTAB mass concentration is 0.03%.
2. CNT (CNT) is joined in the CdS-OH/DMF suspension of step (1) preparation, magnetic agitation 30 min, and in ultrasonator ultrasonic 3 hours, make uniform black suspension D.
The mass fraction of CNT is 0.004%～0.4% among the black suspension D.
3. under magnetic agitation, black suspension D is slowly splashed in the C solution, stirred behind 30 min in ultrasonator ultrasonic 3 hours.Obtain uniform CdS-OH/ CNT/PAN spinning solution.
(3) electrostatic spinning prepares CdS-OH/ CNT/PAN Hybrid nanofibers
The CdS-OH/CNT/PAN spinning solution is transferred in the syringe of 10 mL (internal diameter of syringe needle is 1mm), utilize electric spinning equipment, high-voltage power cathode is connected with syringe needle, negative pole is connected with the flat receiver that is coated with aluminium foil, is 24～30 ℃ in temperature, and humidity is 40～60%, supply voltage is 12～15 kV, the distance of syringe needle and receiver is 15 cm, and the spinning solution flow velocity is to carry out electrostatic spinning under the condition of 2.5 μ L/min, obtains the CdS-OH/CNT/PAN Hybrid nanofibers.
The advantage of the CdS-OH/CNT/PAN Hybrid nanofibers of the present invention's preparation is:
1, the present invention adopts solution growth method and the method for electrostatic spinning preparation Hybrid nanofibers that combines, and technique is simple, and output is high.
2, the average diameter of the CdS-OH/CNT/PAN Hybrid nanofibers of the present invention's preparation is 310 nm, and the average diameter of CdS-OH nano particle is 5 nm, and this preparation method has suppressed the reunion of CdS-OH nano particle effectively.
3, to have specific area large for the CdS-OH/CNT/PAN Hybrid nanofibers of the present invention preparation, the characteristics of good mechanical property.
4, the right compound inhibition that is subject to CNT in light induced electron hole of the CdS-OH/CNT/PAN Hybrid nanofibers of the present invention's preparation, having improved it has high light to urge degradation efficiency to organic dyestuff, and nanofiber is easy to recycle.
Description of drawings
Fig. 1 is the structural model figure of the dS-OH/CNT/PAN Hybrid nanofibers of method preparation of the present invention.
Among Fig. 1, the 1st, polyacrylonitrile (PAN); The 2nd, CdS nano particle (CdS-OH); The 3rd, CNT (CNT).
The specific embodiment
(1) preparation of CdS-OH/DMF suspension
1. under magnetic agitation, the DMF solution that 30 mL are contained 5 mmol 2 mercapto ethanols (ME) splashes into 3 mL and contains 2.5 mmol CdCl
2The aqueous solution in, stir 10min, obtain A solution.
2. 3 mL are contained 1.5 mmol Na
2The aqueous solution of S is added drop-wise in the A solution, and at this moment, water white solution is yellowing and the muddiness that becomes gradually immediately.Treat this mixed solution after 30 ℃ of lower reactions 4 hours, the yellow solution clear that again becomes obtains B solution.
3. B solution is transferred to and under 85 ℃, carried out decompression distillation on the Rotary Evaporators, remove the DMF that anhydrates with small part.After the decompression distillation, by the centrifugal NaCl that is precipitated out that removes, the mass concentration that obtains clear is 1.2% CdS-OH/DMF suspension.
(2) preparation of electrostatic spinning liquid
1. 1.5 g PAN are dissolved in the solution of making clarification among the 11.0 g DMF, afterwards 0.8 g acetone and 0.004 g cetrimonium bronmide (CTAB) are added in the solution, make mass concentration for consisting of 11% PAN, 6.1% acetone, the C solution of 0.03% CTAB.
2. the multi-walled carbon nano-tubes (MWCNT) of 0.0016 g is joined 6.6 g mass concentrations and be in 1.2% the CdS-OH/DMF suspension, magnetic agitation 30 min, and in ultrasonator ultrasonic 3 hours, make uniform black suspension D.
3. under magnetic agitation, black suspension D is slowly added in the C solution, stirred behind 30 min in ultrasonator ultrasonic 3 hours, and obtained the CdS-OH/MWCNT/PAN spinning solution that 20 g mass concentrations consist of the stable homogeneous of 7.5% PAN, 0.4% CdS-OH and 0.008% MWCNT.
(3) preparation of CdS-OH/MWCNT/PAN Hybrid nanofibers
The CdS-OH/MWCNT/PAN spinning solution is transferred in the syringe of 10 mL (internal diameter of syringe needle point is 1mm), utilize electric spinning equipment, high-voltage power cathode is connected with syringe needle point, negative pole is connected with the flat receiver that is coated with aluminium foil, be 30 ℃ in temperature, humidity is to carry out electrostatic spinning under 40% the condition.Wherein, supply voltage is 12 kV, and the distance of needle point and receiver is 15 cm, and solution flow rate is 2.5 μ L/min.The mass ratio that obtains CdS-OH:MWCNT ︰ PAN is the CdS-OH/MWCNT/PAN Hybrid nanofibers of 5 ︰, 0.1 ︰ 94.9.
(4) get the methyl orange solution that 100 mg CdS-OH/MWCNT/PAN Hybrid nanofibers is put into 100 mL, 10 mg/L, 500 W high voltage mercury lamp radiation lower magnetic forces stir 50 min, and the degradation rate of measuring methyl orange in the solution is 90%.
(1) preparation of CdS-OH/DMF suspension is with embodiment 1
(2) preparation of electrostatic spinning liquid
1. 1.5 g PAN are dissolved in the solution of making clarification among the 11.0 g DMF, then 0.83 g acetone and 0.0044 g cetrimonium bronmide (CTAB) are added in the solution, make mass concentration and consist of 11% PAN, 6.1% acetone, the C solution of 0.03% CTAB.
2. the MWCNT of 0.008 g being joined 6.61 g mass concentrations is in the 1.2% CdS-OH/DMF suspension, magnetic agitation 30 min, and in ultrasonator ultrasonic 3 hours, make uniform black suspension D.
3. under magnetic agitation, suspension D is slowly joined in the C solution, stirred behind 30 min in ultrasonator ultrasonic 3 hours.Obtain the CdS-OH/MWCNT/PAN spinning solution that the 20g mass concentration consists of the stable homogeneous of 7.5% PAN, 0.4% CdS-OH and 0.04% MWCNT.
(3) preparation of CdS-OH/MWCNT/PAN Hybrid nanofibers
The CdS-OH/MWCNT/PAN spinning solution is transferred in the syringe of 10 mL (internal diameter of syringe needle point is 1mm), utilize electric spinning equipment, high-voltage power cathode is connected with syringe needle point, negative pole is connected with the flat receiver that is coated with aluminium foil, be 24 ℃ in temperature, humidity is to carry out electrostatic spinning under 60% the condition.Wherein, supply voltage is 15 kV, and the distance of needle point and receiver is 15 cm, and solution flow rate is 2.5 μ L/min.The mass ratio that obtains CdS-OH:MWCNT ︰ PAN is the CdS-OH/MWCNT/PAN Hybrid nanofibers of 5 ︰, 0.5 ︰ 94.5.
(4) get the methyl orange solution that 100 mg CdS-OH/MWCNT/PAN Hybrid nanofibers is put into 100 mL, 10 mg/L, 500 W high voltage mercury lamp radiation lower magnetic forces stir 50 min, and the degradation rate of measuring methyl orange in the solution is 94%.
(1) preparation of CdS-OH/DMF suspension is with embodiment 1
(2) preparation of electrostatic spinning liquid
1. 1.5 g PAN are dissolved in the solution of making clarification among the 11.0 g DMF, afterwards 0.83 g acetone and 0.0044 g cetrimonium bronmide (CTAB) are added in the solution, make mass concentration and consist of 11% PAN, 6.1% acetone, the C solution of 0.03% CTAB.
2. the Single Walled Carbon Nanotube (SWCNT) of 0.008 g being joined 6.65 g mass concentrations is in the 1.2% CdS-OH/DMF suspension, magnetic agitation 30 min, and in ultrasonator ultrasonic 3 hours, make uniform black suspension D.
3. under magnetic agitation, suspension D is slowly joined in the C solution, stirred behind 30 min in ultrasonator ultrasonic 3 hours.Obtain the CdS-OH/SWCNT/PAN spinning solution that the 20g mass concentration consists of the stable homogeneous of 7.5% PAN, 0.4% CdS-OH and 0.04% MWCNT.
(3) preparation of CdS-OH/SWCNT/PAN Hybrid nanofibers
The CdS-OH/SWCNT/PAN spinning solution is transferred in the syringe of 10 mL (internal diameter of syringe needle point is 1mm), utilize the electric spinning equipment in laboratory, high-voltage power cathode is connected with syringe needle point, negative pole is connected with the flat receiver that is coated with aluminium foil, be 27 ℃ in temperature, humidity is to carry out electrostatic spinning under 50% the condition.Wherein, supply voltage is 12 kV, and the distance of needle point and receiver is 15 cm, and solution flow rate is 2.5 μ L/min.The mass ratio that obtains CdS-OH:SWCNT ︰ PAN is the CdS-OH/SWCNT/PAN Hybrid nanofibers of 5 ︰, 1 ︰ 94.0.
(4) get the methyl orange solution that 100 mg CdS-OH/SWCNT/PAN Hybrid nanofibers is put into 100 mL, 10 mg/L, 500 W high voltage mercury lamp radiation lower magnetic forces stir 50 min, and the degradation rate of measuring methyl orange in the solution is 97%.
Claims (6)
1.CdS/ the preparation method of carbon nanotube/polypropylene nitrile Hybrid nanofibers is characterized in that:
(1) preparation of CdS-OH/DMF suspension
1. under magnetic agitation, 30 mL DMF solution are dropwise joined the CdCl of 3 mL
2The aqueous solution in, stir 10min, obtain A solution;
2. with 3 mLNa
2The aqueous solution of S dropwise joins in the A solution, and mixing is mixed with mixed solution, leaves standstill, and 30 ℃ of lower reactions 4～5.5 hours, obtains B solution;
3. B solution is transferred to and under 85～92 ℃, carried out decompression distillation on the Rotary Evaporators, except anhydrating the centrifugal CdS-OH/DMF suspension that obtains clear;
(2) preparation of electrostatic spinning liquid
1. polyacrylonitrile is dissolved in the solution of making clarification among 65 ℃ of DMF, afterwards acetone and cetrimonium bronmide is added in the solution, mixing is made C solution;
2. CNT is joined in the CdS-OH/DMF suspension of step (1) preparation, magnetic agitation 30 min, and in ultrasonator ultrasonic 3 hours, make uniform black suspension D;
3. under magnetic agitation, black suspension D is slowly splashed in the C solution, stirred behind 30 min in ultrasonator ultrasonic 3 hours, obtain CdS-OH/ CNT/PAN spinning solution;
(3) electrostatic spinning prepares Hybrid nanofibers
The CdS-OH/CNT/PAN spinning solution is transferred in the syringe of 10 mL and carried out electrostatic spinning, obtain CdS-OH/ carbon nanotube/polypropylene nitrile Hybrid nanofibers.
2. the preparation method of a kind of CdS according to claim 1/carbon nanotube/polypropylene nitrile Hybrid nanofibers is characterized in that containing in the described DMF solution 2 mercapto ethanol of 5 mmol, described CdCl
2The aqueous solution in contain the CdCl of 2.5 mmol
2
3. the preparation method of a kind of CdS according to claim 1/carbon nanotube/polypropylene nitrile Hybrid nanofibers is characterized in that described Na
2Contain 1.5 mmol Na in the aqueous solution of S
2S.
4. the preparation method of a kind of CdS/ carbon nanotube/polypropylene nitrile Hybrid nanofibers according to claim 1 is characterized in that PAN in the described C solution, and mass concentration is 11%, and acetone quality concentration is that 6.1%, CTAB mass concentration is 0.03%.
5. the preparation method of a kind of CdS/ carbon nanotube/polypropylene nitrile Hybrid nanofibers according to claim 1, the mass fraction that it is characterized in that CNT among the described black suspension D is 0.004%～0.4%.
6. the preparation method of a kind of CdS/ carbon nanotube/polypropylene nitrile Hybrid nanofibers according to claim 1, it is characterized in that described electrostatic spinning, the internal diameter of the syringe needle that adopts is 1mm, temperature is 24～30 ℃, humidity is 40～60%, supply voltage is 12～15 kV, and the distance of syringe needle and receiver is 15 cm, and the spinning solution flow velocity is 2.5 μ L/min.
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| CN104674365A (en) * | 2015-03-04 | 2015-06-03 | 河南省科学院能源研究所有限公司 | Biomass tar-PAN (polyacrylonitrile) fibrous material and preparation method thereof |
| CN105019056A (en) * | 2015-07-01 | 2015-11-04 | 宁波工程学院 | High-purity TiO2 / CuO / Cu nano fiber with whole mesoporous structure |
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| CN105999859A (en) * | 2016-07-14 | 2016-10-12 | 新时代健康产业（集团）有限公司 | Efficient low-resistance antibacterial filtering material containing bamboo leaf flavonoids and preparation method and application of efficient low-resistance antibacterial filtering material |
| CN110052263A (en) * | 2019-04-30 | 2019-07-26 | 广东工业大学 | A kind of photocatalytic nanometer fibrous material and its preparation method and application |
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| CN104674365A (en) * | 2015-03-04 | 2015-06-03 | 河南省科学院能源研究所有限公司 | Biomass tar-PAN (polyacrylonitrile) fibrous material and preparation method thereof |
| CN105019056A (en) * | 2015-07-01 | 2015-11-04 | 宁波工程学院 | High-purity TiO2 / CuO / Cu nano fiber with whole mesoporous structure |
| CN105019056B (en) * | 2015-07-01 | 2018-12-21 | 宁波工程学院 | High purity Ti O2The full meso-porous nano fiber of/CuO/Cu |
| CN105483938A (en) * | 2015-11-30 | 2016-04-13 | 福建师范大学 | Method for preparing PBT/chitosan graft nanofiber membrane through electrostatic spinning method |
| CN105999859A (en) * | 2016-07-14 | 2016-10-12 | 新时代健康产业（集团）有限公司 | Efficient low-resistance antibacterial filtering material containing bamboo leaf flavonoids and preparation method and application of efficient low-resistance antibacterial filtering material |
| CN110052263A (en) * | 2019-04-30 | 2019-07-26 | 广东工业大学 | A kind of photocatalytic nanometer fibrous material and its preparation method and application |
| CN113604969A (en) * | 2021-07-19 | 2021-11-05 | 东北林业大学 | Preparation method of cellulose-based composite nanofiber membrane |
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Application publication date: 20130116 |