CN110485062A - A kind of polychrome composite nano-fiber film and preparation method thereof - Google Patents
A kind of polychrome composite nano-fiber film and preparation method thereof Download PDFInfo
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- CN110485062A CN110485062A CN201910772099.XA CN201910772099A CN110485062A CN 110485062 A CN110485062 A CN 110485062A CN 201910772099 A CN201910772099 A CN 201910772099A CN 110485062 A CN110485062 A CN 110485062A
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- composite nano
- fiber film
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
- D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0076—Electro-spinning characterised by the electro-spinning apparatus characterised by the collecting device, e.g. drum, wheel, endless belt, plate or grid
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
Abstract
A kind of polychrome composite nano-fiber film includes 9- pyrene -1- base -9H- carbazole (PyCz) and N, N- dibutyl -3,4,9,10- tetracarboxylic acid diimide (PTCDI-DC in film4H9) and polymer substrate, composite nano-fiber film is in silk thread layered laminate, and the diameter of silk thread is the nm of 100 nm ~ 400.The present invention is by by carbazole pyrene and N, N- dibutyl -3,4,9,10- tetracarboxylic acid diimide is doped in configured polymer solution, and color change can be presented after contacting prepared nano fibrous membrane with vapor, and has the advantages that colour developing is sensitive, selectivity is high, visual.
Description
Technical field
The invention belongs to fluorescence humidity response technology fields, and in particular to a kind of polychrome composite nano-fiber film and its system
Preparation Method.
Background technique
Humidity response plays an important role in control life system and monitoring industrial process.But due to commonly partly leading
Most of steps and low flexibility all with complexity in the humidity sensors such as body, therefore they still cannot be fitted extensively
With.Alternatively, fluorescence imaging is a kind of ideal tool, and the stimulation from ambient water vapor is converted to optics letter
Breath can incude for humidity (RH) and provide simple, accurate and readable mode.Fluorescence imaging method had not both needed specific element,
Complicated step is not needed yet.Different with monochromatic detection, colorimetric fluorescence detection is protected from environmental small, color and intensity because of it
Variation be easy to the advantages that differentiating and get more and more people's extensive concerning.A kind of entire visible light region of luminous covering of fluorescent molecule
It is not easy to, can be compound by two or more fluorescent molecule, such as feux rouges, green light or blue light are mixed with certain proportion
Conjunction can become white light (Kubo Y, Nishiyabu R. Polymer, 2017,128,257-275).If a kind of substance
After fluorescence is quenched by vapor, tertiary colour will change, and the invisible information about vapor is converted into different
Fluorescence color shows, so as to directly observe by the naked eye.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the deficiencies of the prior art and provide a kind of polychrome composite nano fiber
Film and preparation method thereof, by the way that by carbazole pyrene and N, N- dibutyl -3,4,9,10- tetracarboxylic acid diimides are doped to
In the polymer solution being configured, color change can be presented after contacting prepared nano fibrous membrane with vapor, and have
There are develop the color sensitive, selectivity height, visual advantage.
The present invention provides a kind of polychrome composite nano-fiber film, include in film 9- pyrene -1- base -9H- carbazole PyCz and
N, N- dibutyl -3,4,9,10- tetracarboxylic acid diimide PTCDI-DC4H9 and polymer substrate, composite nano-fiber film
In silk thread layered laminate, the diameter of silk thread is 100 ~ 400 nm.
As further technical solution of the present invention, polymer substrate is poly-N-isopropyl acrylamide PNIPAM, polycyclic
Oxidative ethane PEO, polyacrylamide PA, PVAC polyvinylalcohol, polyethylene glycol PEG, kayexalate PSS.
Further, the mass ratio of polymer substrate is 3:325-6:325；PTCDI-DC4H9With the quality of polymer substrate
Than for 6:325-10:325.
The present invention also provides a kind of preparation methods of polychrome composite nano-fiber film, include the following steps,
Step S1, PyCz, PTCDI-DC are weighed in mass ratio4H9And polymer substrate, and will be mixed in DMF solvent, 20
Uniform stirring obtains uniform polymer solution at DEG C；
Step S2, polymer solution is prepared by polychrome composite nano-fiber membrane by method of electrostatic spinning, and is spun in quartz plate
On.
Further, the mass ratio of PyCz and polymer substrate is 3:325-6:325；PTCDI-DC4H9With polymer substrate
Mass ratio be 6:325-10:325, the mass ratio 1:5.74 of polymer substrate and DMF.
Further, the mass percent concentration of polymer solution is 14wt%-16wt%.
Further, in step S2, during electrostatic spinning, voltage is 5-15 kV, and syringe needle is at a distance from receiver
10-20 cm, the internal diameter of syringe needle are 0.60 mm, and solution flow velocity is 0.12 μ L/s, when spinning a length of 2 min.
Further, PyCz is blue light compound, PTCDI-DC4H9For feux rouges compound.
Further, it spins tilt respectively in the polychrome composite nano-fiber membrane on quartz plate and is put into several water and quiet is housed
It sets in closed fluorescence pond for 24 hours, then closed fluorescence pond is placed in Fluorescence Spectrometer, 370 nm of excitation wavelength, detects Nanowire
Tie up film fluorescence intensity at 380-700 nm.
Further, the volume in closed fluorescence pond is the cm × 4 of 1 cm × 1 cm.
The present invention is prepared for by doping method and electrostatic spinning technique to the sensitive colour developing of vapor, and selectivity is high, in tide
It can be relieved the polychrome composite nano-fiber film of visual fatigue under wet environment, which has at low cost, simple process, can quickly make
Standby advantage.
Detailed description of the invention
Fig. 1 is polychrome composite nano-fiber film scanning electron microscope (SEM) photograph prepared by the present invention；
Fig. 2 is PTCDI-DC in polychrome composite nano fiber4H9Individually it is dissolved in the fluorescence of polymer preparation gained nano fibrous membrane
Spectrogram；
Fig. 3 is the fluorescence spectra that PyCz is individually dissolved in nano fibrous membrane prepared by polymer in polychrome composite nano fiber；
Fig. 4 is that the polychrome composite nano-fiber film of preparation is exposed to containing after 1h in not same amount water and the silica dish of standing for 24 hours
Fluorescence spectra；
Fig. 5 is that the polychrome composite nano-fiber film of preparation is exposed to containing after 1h in not same amount water and the silica dish of standing for 24 hours
Fluorescent quenching efficiency chart.
Specific embodiment
Referring to Fig. 1, including 9- in composite nano-fiber film the present embodiment provides polychrome composite nano-fiber film
Pyrene -1- base -9H- carbazole PyCz and N, N- dibutyl -3,4,9,10- tetracarboxylic acid diimide PTCDI-DC4H9And polymer matrix
Matter, composite nano-fiber film are in silk thread layered laminate, and the diameter of silk thread is the nm of 100 nm ~ 400.
Embodiment 1
Weigh the PTCDI-DC of the PyCz and 7 mg of 3 mg4H9(PyCz: PTCDI-DC4H9And 325 molar ratio is 1: 1.7)
The PNIPAM polymer of mg is dissolved in the DMF solution of 2 mL, at 20 DEG C stirring formed 15wt% uniform Electrospun it is molten
Liquid.
The good above-mentioned electrospun solution of configuration is injected in the plastic injector of 2 mL, open end is connected work with stainless steel syringe needle
For spray head, it is connected with positive pole, uses aluminium foil as receiving screen, be connected with power cathode, in the stainless steel that internal diameter is 0.6 mm
Apply the DC voltage of 10 kV on syringe needle, with 0.12 μ L/s flow velocity sample introduction, the distance of receiver and syringe needle is polymer solution
15 cm, relative air humidity 60%, temperature carries out electrospinning under conditions of being 24.5 DEG C, wherein being used for the tunica fibrosa of spectrum test
Be fiber is deposited in electro-spinning process it is obtained on quartz plate.
It is as follows that vapor responds experimental procedure:
The quartz plate that deposited nanofiber inclination is put into containing 0.2 μ L deionized water and is stood in the closed fluorescence pond of 24 h
Between (cm × 4 of 1 cm × 1 cm), then this closed fluorescence pond is placed on the bracket of luminoscope, 370 nm of excitation wavelength, detection is received
Rice fiber membrane fluorescence intensity at 380-700 nm.
As shown in Fig. 2, PNIPAM/PTCDI-DC4H9Fluorescence spectrum (the λ of nano fibrous membraneex=370 nm) it is arrived in 570 nm
Be continuous transmitting band between 701 nm, wherein the transmitting band between 570 nm to 644 nm is weaker and 644 nm to 701 nm it
Between transmitting band it is stronger, therefore PNIPAM/PTCDI-DC4H9Nano fibrous membrane glows.
As shown in figure 3, fluorescence spectrum (the λ of PNIPAM/PyCz nano thin-filmex=340 nm) it is shown at 408 nm by force
Emission peak, neighbouring fluorescent belt is all located at greatly blue light region, therefore PNIPAM/PyCz nano thin-film turns blue coloured light.Therefore feux rouges with
The compound obtained complex light of blue light is purple, and the polychrome variation of tunica fibrosa fluorescence color may be implemented.
As shown in figure 4, being respectively as follows: a from left to right is to be placed in containing in 0.2 μ L deionized water silica dish, b is to be placed in containing 0.3
In μ L deionized water silica dish, c is to be placed in containing in 0.8 μ L deionized water silica dish, and after 1h, the fluorescence intensity of blue light is reduced, red
Light without changing, i.e. the fluorescence intensity of PyCz reduces and PTCDI-DC4H9It is constant that fluorescence intensity is not responded to vapor.
As shown in figure 5, being from left to right respectively to be placed in 0.2 μ L, 0.3 μ L, in 0.8 μ L silica dish, polychrome is compound after 1h
The fluorescent quenching efficiency of tunica fibrosa is respectively 18.50%, 29.80%, 55.06%.
Embodiment 2
Weigh the PTCDI-DC of the PyCz and 7 mg of 3 mg4H9(PyCz: PTCDI-DC4H9And 325 molar ratio is 1: 1.7)
The PNIPAM polymer of mg is dissolved in the DMF solution of 2 mL, at 20 DEG C stirring formed 15wt% uniform Electrospun it is molten
Liquid.
The good above-mentioned electrospun solution of configuration is injected in the plastic injector of 2 mL, open end is connected work with stainless steel syringe needle
For spray head, it is connected with positive pole, uses aluminium foil as receiving screen, be connected with power cathode, in the stainless steel that internal diameter is 0.6 mm
Apply the DC voltage of 10 kV on syringe needle, with 0.12 μ L/s flow velocity sample introduction, the distance of receiver and syringe needle is polymer solution
15 cm, relative air humidity 60%, temperature carries out electrospinning under conditions of being 24.5 DEG C, wherein being used for the fiber of spectrum test
Film be fiber is deposited in electro-spinning process it is obtained on quartz plate.
It is as follows that vapor responds experimental procedure:
The quartz plate that deposited nanofiber inclination is put into containing 0.3 μ L deionized water and is stood in the closed fluorescence pond of 24 h
Between (cm × 4 of 1 cm × 1 cm), then this closed fluorescence pond is placed on the bracket of luminoscope, 370 nm of excitation wavelength, detection is received
Rice fiber membrane fluorescence intensity at 380-700 nm.
Embodiment 3:
Weigh the PTCDI-DC of the PyCz and 7 mg of 3 mg4H9(PyCz: PTCDI-DC4H9And 325 molar ratio is 1: 1.7)
The PNIPAM polymer of mg is dissolved in the DMF solution of 2 mL, at 20 DEG C stirring formed 15wt% uniform Electrospun it is molten
Liquid.
The good above-mentioned electrospun solution of configuration is injected in the plastic injector of 2 mL, open end is connected work with stainless steel syringe needle
For spray head, it is connected with positive pole, uses aluminium foil as receiving screen, be connected with power cathode, in the stainless steel that internal diameter is 0.6 mm
Apply the DC voltage of 10 kV on syringe needle, with 0.12 μ L/s flow velocity sample introduction, the distance of receiver and syringe needle is polymer solution
15 cm, relative air humidity 60%, temperature carries out electrospinning under conditions of being 24.5 DEG C, wherein being used for the fiber of spectrum test
Film be fiber is deposited in electro-spinning process it is obtained on quartz plate.
It is as follows that vapor responds experimental procedure:
The quartz plate that deposited nanofiber inclination is put into containing 0.8 μ L deionized water and is stood in the closed fluorescence pond of 24 h
Between (cm × 4 of 1 cm × 1 cm), then this closed fluorescence pond is placed on the bracket of luminoscope, 370 nm of excitation wavelength, detection is received
Rice fiber membrane fluorescence intensity at 380-700 nm.
The basic principles, main features and advantages of the invention have been shown and described above.Those skilled in the art should
Understand, the present invention do not limited by above-mentioned specific embodiment, the description in above-mentioned specific embodiment and specification be intended merely into
One step illustrates the principle of the present invention, and under the premise of not departing from spirit of that invention range, the present invention also has various change and changes
Into these changes and improvements all fall within the protetion scope of the claimed invention.The scope of protection of present invention is by claim
Book and its equivalent thereof.
Claims (10)
1. a kind of polychrome composite nano-fiber film, which is characterized in that include 9- pyrene -1- in the composite nano-fiber film
Base -9H- carbazole PyCz and N, N- dibutyl -3,4,9,10- tetracarboxylic acid diimide (PTCDI-DC4H9) and polymer substrate,
The composite nano-fiber film is in silk thread layered laminate, and the diameter of silk thread is the nm of 100 nm ~ 400.
2. a kind of polychrome composite nano-fiber film according to claim 1, which is characterized in that the polymer substrate is
Poly-N-isopropyl acrylamide PNIPAM, polyethylene oxide PEO, polyacrylamide PA, PVAC polyvinylalcohol, polyethylene glycol PEG,
Kayexalate PSS.
3. a kind of polychrome composite nano-fiber film according to claim 1, which is characterized in that the PyCz gathers with described
The mass ratio of polymer matrix is 3:325-6:325；The PTCDI-DC4H9Mass ratio with the polymer substrate is 6:325-
10:325。
4. a kind of preparation method of polychrome composite nano-fiber film, which is characterized in that include the following steps,
Step S1, PyCz, PTCDI-DC are weighed in mass ratio4H9And polymer substrate, and dissolve them in DMF solvent, In
Uniform stirring obtains uniform polymer solution at 20 DEG C；
Step S2, polymer solution is prepared by polychrome composite nano-fiber membrane by method of electrostatic spinning, and is spun in quartz plate
On.
5. a kind of preparation method of polychrome composite nano-fiber film according to claim 4, which is characterized in that described
The mass ratio of PyCz and the polymer substrate is 3:325-6:325；The PTCDI-DC4H9With the matter of the polymer substrate
Amount is than being 6:325-10:325, the mass ratio 1:5.74 of the polymer substrate and the DMF.
6. a kind of preparation method of polychrome composite nano-fiber film according to claim 4, which is characterized in that described poly-
The mass percent concentration of polymer solution is 14wt%-16wt%.
7. a kind of preparation method of polychrome composite nano-fiber film according to claim 4, which is characterized in that the step
In rapid S2, during electrostatic spinning, voltage is 5-15 KV, and syringe needle is 10-20 cm at a distance from receiver, and the internal diameter of syringe needle is
0.60 mm, solution flow velocity are 0.12 μ L/s, when spinning a length of 2 min.
8. a kind of preparation method of polychrome composite nano-fiber film according to claim 4, which is characterized in that described
PyCz is blue light compound, the PTCDI-DC4H9For feux rouges compound.
9. a kind of preparation method of polychrome composite nano-fiber film according to claim 4, which is characterized in that spin Yu Shi
The polychrome composite nano-fiber membrane of English on piece tilts respectively is put into several equipped with water and the closed fluorescence pond of standing for 24 hours
In, then closed fluorescence pond is placed in Fluorescence Spectrometer, 370 nm of excitation wavelength, nano-fiber film is detected in 380-700 nm
Locate fluorescence intensity.
10. a kind of preparation method of polychrome composite nano-fiber film according to claim 9, which is characterized in that described
The volume in closed fluorescence pond is the cm × 4 of 1 cm × 1 cm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113201857A (en) * | 2021-04-29 | 2021-08-03 | 南京邮电大学 | Temperature-sensitive composite nanofiber film and preparation method and application thereof |
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