CN110106627A - A kind of preparation method and applications of bismuthyl carbonate-polyethylene oxide film - Google Patents
A kind of preparation method and applications of bismuthyl carbonate-polyethylene oxide film Download PDFInfo
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- CN110106627A CN110106627A CN201910252663.5A CN201910252663A CN110106627A CN 110106627 A CN110106627 A CN 110106627A CN 201910252663 A CN201910252663 A CN 201910252663A CN 110106627 A CN110106627 A CN 110106627A
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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
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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
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0069—Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
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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
- D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
- D01D5/0092—Electro-spinning characterised by the electro-spinning apparatus characterised by the electrical field, e.g. combined with a magnetic fields, using biased or alternating fields
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- 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
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- 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
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/94—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of other polycondensation products
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- 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
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
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- Chemical Kinetics & Catalysis (AREA)
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- Artificial Filaments (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
Abstract
The present invention provides a kind of preparation method of bismuthyl carbonate-polyethylene oxide film, and polyethylene oxide, pentaerythritol triacrylate solution and solvent is used to prepare spinning solution, is crosslinked electrospun fibers film with preparation；Spinning solution is prepared using polyethylene oxide, bismuthyl carbonate inorganic material, pentaerythritol triacrylate solution and solvent, electrostatic spinning is carried out using the crosslinking electrospun fibers film of preparation as substrate is received, electron beam irradiation processing will be carried out after the oxygen barrier processing of resulting tunica fibrosa, obtain bismuthyl carbonate-polyethylene oxide composite crosslinking electrospun fibers film.The invention further relates to using bismuthyl carbonate-polyethylene oxide film and its application made from above-mentioned preparation method.The present invention provides energy using electron beam, and pentaerythritol triacrylate is cross-linking modified by polyethylene oxide tunica fibrosa as grafted monomers, to improve solvent resistance, the heat resistance of tunica fibrosa, it is easily recycled, and further increases the photocatalysis performance of composite fibre, can be used for organic sewage processing.
Description
Technical field
The present invention relates to technical field of composite materials more particularly to a kind of bismuthyl carbonate-polyethylene oxide film preparation sides
Method and its application.
Background technique
Bismuthyl carbonate is a kind of n-type semiconductor, and band gap is between 2.8-3.5eV, in visible light or sunlight
Under show higher photocatalytic activity, can be used for handling waste water containing dye.But bismuthyl carbonate is in powdered, directly
As photochemical catalyst be used to degrade the dyestuff in water body when be easily scattered, be not easily recycled.
Electrostatic spinning is a kind of technology that is simple, easily and efficiently preparing tunica fibrosa.It is prepared by electrostatic spinning technique
Fibrous material has many advantages, such as that manufacturing equipment is simple, and technology is easy to control, and has been widely used for preparing organic-inorganic
Composite fiber, this can substantially improve the shortcomings that inorganic material is not easily recycled.
Polyethylene oxide is a kind of polymer of hydrophilic, very wide in field of biomedicine application.Pass through Static Spinning
The preparation method of silk, polyethylene oxide solution are sprayed by strong electrostatic force from capillary, and it is uniform to obtain diameter, pattern rule
Whole polymer fiber.But the high solubility of polyethylene oxide in water limits its application.
Electron beam irradiation makes macromolecule polyalcohol backbone breaking by radiation and is crosslinked, to change polymer physics
Matter.By crosslinking with radiation, the solubility of high polymer can effectively improve, make it insoluble in inorganic and organic solvent, its subsequent is answered
With offer convenience.Thus polyethylene oxide is modified using electron beam irradiation method, is crosslinked polyethylene oxide, obtained
Obtain the improvement of thermal stability and solvent resistance.
But there is not any report that bismuthyl carbonate and polyethylene oxide combination can be prepared to tunica fibrosa in the prior art.
Summary of the invention
The purpose of the present invention is to overcome the defects in the prior art, provides a kind of bismuthyl carbonate-polyethylene oxide film
Preparation method and applications can combine bismuthyl carbonate and polyethylene oxide, can be by improving polyethylene oxide tunica fibrosa
Stability and solvent resistance realize the recycling of bismuthyl carbonate.
To achieve the above object, the present invention adopts the following technical scheme:
The first purpose of the invention is to provide a kind of bismuthyl carbonate-polyethylene oxide film preparation methods comprising such as
Lower step:
Step (1) is spun using polyethylene oxide (PEO), pentaerythritol triacrylate (PETA) solution and solvent preparation
Silk liquid, and electrospun fibers film is crosslinked by electrostatic spinning and electron beam irradiation preparation；
Step (2) uses polyethylene oxide (PEO), bismuthyl carbonate inorganic material (Bi2O2CO3), three propylene of pentaerythrite
Acid esters (PETA) solution and solvent prepare spinning solution, using the crosslinking electrospun fibers film that step (1) obtains as reception base
Bottom carries out electrostatic spinning, electron beam irradiation processing will be carried out after the oxygen barrier processing of resulting tunica fibrosa, obtains bismuthyl carbonate-polycyclic
Oxidative ethane composite crosslinking electrospun fibers film.
In order to advanced optimize above-mentioned preparation method, the technical measures that the present invention takes further include:
Further, the preparation step of crosslinking electrospun fibers film described in step (1) includes:
(A) polyethylene oxide prepares precursor solution, adds pentaerythritol triacrylate solution, system is mixed with solvent
Standby spinning solution；
(B) by step (A) prepare described spinning solution be contained in electrostatic spinning apparatus syringe, syringe needle with
The connection of high pressure generator anode, aluminium foil roller receiver are connect with high pressure receiver cathode, carry out electrospinning, what electrostatic spinning went out
Tunica fibrosa is undertaken on the aluminium foil roller receiver；
(C) the resulting tunica fibrosa of step (B) is subjected to oxygen barrier processing, and carries out electron beam irradiation processing, handed over
Join electrospun fibers film；
Further, bismuthyl carbonate described in step (2)-polyethylene oxide composite crosslinking electrospun fibers film system
Include: for step
(a) polyethylene oxide prepares precursor solution, adds bismuthyl carbonate inorganic material, adds three propylene of pentaerythrite
Acid esters solution is mixed with spinning solution with solvent；
(b) by step (a) prepare the spinning solution be contained in electrostatic spinning apparatus syringe, syringe needle with
The connection of high pressure generator anode, aluminium foil roller receiver are connect with high pressure receiver cathode, the friendship that step (C) is obtained
Join electrospun fibers film as substrate is received and carry out electrospinning, the tunica fibrosa that electrostatic spinning goes out is undertaken on the aluminium foil roller and connects
It receives on device；
(c) the resulting tunica fibrosa of step (b) is subjected to oxygen barrier processing, and carries out electron beam irradiation processing, obtain carbonic acid gas
Bismuth-polyethylene oxide composite crosslinking electrospun fibers film.
Further, in the step (A), in terms of the gross mass of spinning solution, the polyethylene oxide accounts for 8~15%.
Further, in the step (A), in terms of the gross mass of spinning solution, the pentaerythritol triacrylate accounts for 1
~3%.
Further, in the step (A), the solvent includes methylene chloride (DCM), in dimethylformamide (DMF)
At least one.
Further, in the step (A), the mixing step of each reagent is as follows: polyethylene oxide being added in solvent and is mixed
1.5~3h is closed, pentaerythritol triacrylate solution is added and is protected from light 5~15min of mixing.
Further, in the step (B), syringe spinning head internal diameter is 0.33mm, and syringe spinning head connects with roller
Receipts device surface distance is 8~15cm, and application voltage is 10~20kV.
Further, in the step (B), syringe fltting speed is 8~18 μ Lmin-1, roller receive speed be
60~100rpm, it is 22~30mm that syringe, which injects horizontal reciprocating moving distance, guarantees that electrostatic spinning obtains uniform fiber
Film.
Further, in the step (C), the oxygen barrier processing is that tunica fibrosa packs the logical oxygen barrier sealing of nitrogen.
Further, in the step (C), the electron beam irradiation is horizontal irradiation, and dosage is 90~300 kGy, is protected
Card tunica fibrosa is uniformly irradiated.
Further, in the step (a), in terms of the gross mass of spinning solution, the polyethylene oxide accounts for 5~10%.
Further, in the step (a), in terms of the gross mass of spinning solution, the bismuthyl carbonate inorganic material accounts for 5~
10%.
Further, in the step (a), in terms of the gross mass of spinning solution, the pentaerythritol triacrylate accounts for 1
~3%.
Further, in the step (a), the solvent includes methylene chloride, at least one in dimethylformamide
Kind.
Further, in the step (a), the mixing step of each reagent is as follows: polyethylene oxide being added in solvent and is mixed
0.5~1.5h is closed, pentaerythritol triacrylate solution is added and is protected from light 5~15min of mixing, it is inorganic to add bismuthyl carbonate
Material mixes 0.5~1.5h.
Further, in the step (b), syringe spinning head internal diameter is 0.60mm, and syringe spinning head connects with roller
Receipts device surface distance is 8~15cm, and application voltage is 15~20kV.
Further, in the step (b), syringe fltting speed is 18~35 μ Lmin-1, roller receive speed be
60~100rpm, it is 25~35mm that syringe, which injects horizontal reciprocating moving distance, guarantees that electrostatic spinning obtains uniform fiber
Film.
Further, in the step (c), the oxygen barrier processing is that tunica fibrosa packs the logical oxygen barrier sealing of nitrogen.
Further, in the step (c), the electron beam irradiation is horizontal irradiation, and dosage is 90~300 kGy, is protected
Card tunica fibrosa is uniformly irradiated.
A second object of the present invention is to provide a kind of bismuthyl carbonate-polycyclics as made from any above-mentioned preparation method
Oxidative ethane film.
Third object of the present invention is a kind of bismuthyl carbonate as made from any above-mentioned preparation method-polycyclic oxygen second
Application of the alkane film in sewage treatment.
Further, the bismuthyl carbonate-polyethylene oxide film is used as photochemical catalyst.
Compared with prior art, the present invention has the advantages that by adopting the above technical scheme
The present invention utilizes electron beam to provide energy during the preparation process, pentaerythritol triacrylate as grafted monomers,
Polyethylene oxide tunica fibrosa is cross-linking modified, polymer formed tridimensional network, can be improved tunica fibrosa solvent resistance,
Heat resistance is easily recycled, and the composite nano fiber of acquisition has positive meaning to the photocatalysis performance for further increasing composite fibre
Justice can be used for organic sewage processing.
Detailed description of the invention
Fig. 1 is bismuthyl carbonate/polyethylene oxide film scanning electron microscope (SEM) photograph made from the embodiment of the present invention 1；
Fig. 2 is bismuthyl carbonate/polyethylene oxide film scanning electron microscope (SEM) photograph made from the embodiment of the present invention 2；
Fig. 3 is bismuthyl carbonate/polyethylene oxide film scanning electron microscope (SEM) photograph made from the embodiment of the present invention 3；
Fig. 4 is removal curve graph of the bismuthyl carbonate/polyethylene oxide film made from one embodiment of the invention to methyl orange.
Specific embodiment
The present invention provides a kind of preparation method of bismuthyl carbonate-polyethylene oxide film comprising following steps: step
(1) spinning solution is prepared using polyethylene oxide, pentaerythritol triacrylate solution and solvent, and passes through electrostatic spinning and electricity
Beamlet irradiation preparation crosslinking electrospun fibers film；Step (2) uses polyethylene oxide, bismuthyl carbonate inorganic material, season penta
Tetrol triacrylate solution and solvent prepare spinning solution, and the crosslinking electrospun fibers film obtained using step (1) is as connecing
It receives substrate and carries out electrostatic spinning, electron beam irradiation processing will be carried out after the oxygen barrier processing of resulting tunica fibrosa, obtain bismuthyl carbonate-
Polyethylene oxide composite crosslinking electrospun fibers film.The invention further relates to using bismuthyl carbonate-made from above-mentioned preparation method
Polyethylene oxide film and its application.
Specifically, above-mentioned bismuthyl carbonate-polyethylene oxide film preparation method includes:
(1) polyethylene oxide (PEO) prepares precursor solution, with methylene chloride (DCM) and dimethylformamide (DMF)
Mixed solution as organic solvent, and add account for spinning solution gross mass 1~3% pentaerythritol triacrylate (PETA) it is molten
Mentioned reagent is mixed with spinning solution by liquid, and the total mass fraction of polyethylene oxide is 8%~15% in the spinning solution；
(2) step (1) described spinning solution is contained in electrostatic spinning apparatus syringe, syringe needle and high pressure
Raw device anode connection, aluminium foil receiver are connect with high pressure receiver cathode, carry out electrospinning, and the tunica fibrosa that electrostatic spinning goes out is accepted
On aluminium foil roller receiver.In the present invention, syringe spinning head internal diameter is 0.33 mm, and syringe spinning head connects with roller
Receipts device surface distance is 8~15cm, and application voltage is 10~20kV, and syringe fltting speed is 8~18 μ Lmin-1, roller
Reception speed is 60~100rpm, and it is 22~30mm that syringe, which injects horizontal reciprocating moving distance, guarantees that electrostatic spinning obtains
Even tunica fibrosa.
(3) tunica fibrosa for obtaining step (2) packs the logical oxygen barrier sealing of nitrogen；
(4) tunica fibrosa for obtaining step (3) carries out electron beam irradiation processing, the electrospun fibers film being crosslinked.
In the present invention, electron beam irradiation dosage is 90~300kGy, and horizontal irradiation guarantees that tunica fibrosa is uniformly irradiated；
(5) polyethylene oxide (PEO) prepares precursor solution, adds bismuthyl carbonate (Bi2O2CO3) inorganic material, with two
Chloromethanes (DCM) and dimethylformamide (DMF) mixed solution are used as organic solvent, and addition account for spinning solution gross mass 1~
3% pentaerythritol triacrylate (PETA) solution mixes, and the electrostatic spinning precursor solution and solvent are mixed with
Spinning solution, the total mass fraction of polyethylene oxide is 5~10% in the spinning solution, bismuthyl carbonate (Bi2O2CO3) inorganic material
Mass fraction be 5~10%；
(6) step (5) described spinning solution is contained in electrostatic spinning apparatus syringe, syringe needle and high pressure
Raw device anode connection, aluminium foil receiver are connect with high pressure receiver cathode, using cross filament film that step (4) obtains as connecing
It receives substrate and carries out electrospinning, the tunica fibrosa that electrostatic spinning goes out is undertaken on aluminium foil roller receiver.In this experiment, syringe sprays
Silk head internal diameter is 0.60mm, and syringe spinning head and roller receiver surface distance are 8~15cm, apply voltage be 15~
20kV, syringe fltting speed are 18~35 μ Lmin-1, it is 60~100rpm that roller, which receives speed, and syringe injects level
Moving back and forth distance is 25~35mm, and guarantee obtains uniform electrospun fibers film；
(7) tunica fibrosa obtained by step (6) is packed into the logical oxygen barrier sealing of nitrogen；
(8) step (7) is obtained into fiber and carries out electron beam irradiation processing, obtain composite crosslinking electrospun fibers film.?
In this experiment, electron beam irradiation dosage is 90~300kGy, and horizontal irradiation guarantees that tunica fibrosa is uniformly irradiated.
With reference to the accompanying drawings and examples, further description of the specific embodiments of the present invention.Following embodiment is only
For clearly illustrating technical solution of the present invention, and not intended to limit the protection scope of the present invention.
Embodiment 1
(a) 4mL organic solvent is added in 0.5159g polyethylene oxide (includes 2mL methylene chloride and 2mL dimethyl formyl
Amine) in, magnetic agitation (500rpm) about 2h；
(b) 0.1032g pentaerythritol triacrylate (is added and accounts for the pentaerythrite 3 third of spinning solution gross mass 2%
Olefin(e) acid ester solution) acquired solution in step (a) is added, it is protected from light about 10 min of magnetic agitation (500rpm)；
(c) step (b) acquired solution is contained in electrostatic spinning apparatus syringe, the spray for the use of internal diameter being 0.33 mm
Silk head, adjusts syringe spinning head and roller receiver surface distance is 15cm, and syringe fltting speed is 12 μ Lmin-1,
It is 100rpm that roller, which receives speed, and it is 22mm that syringe, which injects horizontal reciprocating moving distance, and syringe needle and high pressure are occurred
The connection of device anode, aluminium foil receiver are connect with high pressure receiver cathode, and adjusting voltage is 15kV, carries out electrospinning, and electrostatic spinning goes out
Tunica fibrosa be undertaken on aluminium foil roller receiver.
(d) electrospun fibers obtained by step (c) are contained in irradiation bag, oxygen in nitrogen isolation bag are passed through, by bag
Son sealing；
(e) fiber sealed bag obtained by step (d) is subjected to level electron beam radiation treatment, by fiber cross-linking radiation, irradiation
Dosage is 210kGy, preparation crosslinking electrospun fibers film；
(f) 4mL organic solvent is added in 0.2640g polyethylene oxide (includes 2mL methylene chloride and 2mL dimethyl formyl
Amine) in, magnetic agitation (500rpm) about 1h；
(g) 0.0528g pentaerythritol triacrylate (is added and accounts for the pentaerythrite 3 third of spinning solution gross mass 1%
Olefin(e) acid ester solution) acquired solution in step (f) is added, it is protected from light about 10 min of magnetic agitation (500rpm)；
(h) acquired solution in step (g), magnetic agitation (500rpm) about 1h is added in 0.4223g bismuthyl carbonate；
(i) gained spinning solution in step (h) is contained in electrostatic spinning apparatus syringe, the use of internal diameter is 0.60mm
Spinning head, adjusting syringe spinning head and roller receiver surface distance is 15cm, and syringe fltting speed is 35 μ L
min-1, it is 100rpm that roller, which receives speed, and it is 25mm that syringe, which injects horizontal reciprocating moving distance, by syringe needle and height
The connection of generator anode is pressed, aluminium foil receiver is connect with high pressure receiver cathode, and adjusting voltage is 15kV, carries out electrospinning, electrostatic
The tunica fibrosa that spinning goes out is undertaken on using crosslinking electrospun fibers film obtained in step (d) as on the roller receiver of substrate.
(j) electrospun fibers obtained by step (i) are contained in irradiation bag, are passed through nitrogen for oxygen-barrier in bag, incite somebody to action
Sack sealing；
(k) fiber sealed bag obtained by step (j) is subjected to level electron beam radiation treatment, by fiber cross-linking radiation, irradiation
Dosage is 210kGy, prepares bismuthyl carbonate-polyethylene oxide composite crosslinking electrospun fibers film.
Embodiment 2
(a) 0.4681g polyethylene oxide is added in 4mL organic solvent (4mL methylene chloride), magnetic agitation
(500rpm) about 1.5h；
(b) 0.0691g pentaerythritol triacrylate (is added and accounts for the pentaerythrite three of spinning solution gross mass 1.2%
Acrylate solution) acquired solution in step (a) is added, it is protected from light magnetic agitation (500rpm) about 5min；
(c) step (b) acquired solution is contained in electrostatic spinning apparatus syringe, the spray for the use of internal diameter being 0.33 mm
Silk head, adjusts syringe spinning head and roller receiver surface distance is 8cm, and syringe fltting speed is 8 μ Lmin-1, rolling
It is 60rpm that cylinder, which receives speed, and it is 25 mm that syringe, which injects horizontal reciprocating moving distance, by syringe needle and high pressure generator
Anode connection, aluminium foil receiver are connect with high pressure receiver cathode, and adjusting voltage is 10kV, carry out electrospinning, what electrostatic spinning went out
Tunica fibrosa is undertaken on aluminium foil roller receiver.
(d) electrospun fibers obtained by step (c) are contained in irradiation bag, oxygen in nitrogen isolation bag are passed through, by bag
Son sealing；
(e) fiber sealed bag obtained by step (d) is subjected to level electron beam radiation treatment, by fiber cross-linking radiation, irradiation
Dosage is 90kGy, preparation crosslinking electrospun fibers film；
(f) 0.4837g polyethylene oxide is added in 4mL organic solvent (including 4mL dimethylformamide), magnetic force stirs
Mix (500rpm) about 0.5h；
(g) 0.0967g pentaerythritol triacrylate (is added and accounts for the pentaerythrite 3 third of spinning solution gross mass 2%
Olefin(e) acid ester solution solution) acquired solution in step (f) is added, it is protected from light magnetic agitation (500rpm) about 5min；
(h) acquired solution in step (g), magnetic agitation (500rpm) about 0.5h is added in 0.3023g bismuthyl carbonate；
(i) gained spinning solution in step (h) is contained in electrostatic spinning apparatus syringe, the use of internal diameter is 0.60mm
Spinning head, adjusting syringe spinning head and roller receiver surface distance is 8cm, and syringe fltting speed is 18 μ L
min-1, it is 60rpm that roller, which receives speed, and it is 28mm that syringe, which injects horizontal reciprocating moving distance, by syringe needle and high pressure
The connection of generator anode, aluminium foil receiver are connect with high pressure receiver cathode, and adjusting voltage is 18kV, carry out electrospinning, Static Spinning
The tunica fibrosa that silk goes out is undertaken on using crosslinking electrospun fibers film obtained in step (d) as on the roller receiver of substrate.
(j) electrospun fibers obtained by step (i) are contained in irradiation bag, are passed through nitrogen for oxygen-barrier in bag, incite somebody to action
Sack sealing；
(k) fiber sealed bag obtained by step (j) is subjected to level electron beam radiation treatment, by fiber cross-linking radiation, irradiation
Dosage is 90kGy, prepares bismuthyl carbonate-polyethylene oxide composite crosslinking electrospun fibers film.
Embodiment 3
(a) 4mL organic solvent is added in 0.7971g polyethylene oxide (includes 1.5mL methylene chloride and 2.5mL dimethyl
Formamide) in, magnetic agitation (500rpm) about 3h；
(b) 0.1594g pentaerythritol triacrylate (is added and accounts for the pentaerythrite three of spinning solution gross mass 3.0%
Acrylate solution solution) acquired solution in step (a) is added, it is protected from light magnetic agitation (500rpm) about 15min；
(c) step (b) acquired solution is contained in electrostatic spinning apparatus syringe, the spray for the use of internal diameter being 0.33 mm
Silk head, adjusts syringe spinning head and roller receiver surface distance is 12cm, and syringe fltting speed is 18 μ Lmin-1,
It is 80rpm that roller, which receives speed, and it is 30mm that syringe, which injects horizontal reciprocating moving distance, and syringe needle and high pressure are occurred
The connection of device anode, aluminium foil receiver are connect with high pressure receiver cathode, and adjusting voltage is 20kV, carries out electrospinning, and electrostatic spinning goes out
Tunica fibrosa be undertaken on aluminium foil roller receiver.
(d) electrospun fibers obtained by step (c) are contained in irradiation bag, oxygen in nitrogen isolation bag are passed through, by bag
Son sealing；
(e) fiber sealed bag obtained by step (d) is subjected to level electron beam radiation treatment, by fiber cross-linking radiation, irradiation
Dosage is 300kGy, preparation crosslinking electrospun fibers film；
(f) 4mL organic solvent is added in 0.3060g polyethylene oxide (includes 3mL methylene chloride and 1mL dimethyl formyl
Amine) in, magnetic agitation (500rpm) about 1.5h；
(g) 0.0612g pentaerythritol triacrylate (is added and accounts for the pentaerythrite three of spinning solution gross mass 1.1%
Acrylate solution solution) acquired solution in step (f) is added, it is protected from light magnetic agitation (500rpm) about 15min；
(h) acquired solution in step (g), magnetic agitation (500rpm) about 1.5h is added in 0.2785g bismuthyl carbonate；
(i) gained spinning solution in step (h) is contained in electrostatic spinning apparatus syringe, the use of internal diameter is 0.60mm
Spinning head, adjusting syringe spinning head and roller receiver surface distance is 13cm, and syringe fltting speed is 27 μ L
min-1, it is 90rpm that roller, which receives speed, and it is 35mm that syringe, which injects horizontal reciprocating moving distance, by syringe needle and high pressure
The connection of generator anode, aluminium foil receiver are connect with high pressure receiver cathode, and adjusting voltage is 20kV, carry out electrospinning, Static Spinning
The tunica fibrosa that silk goes out is undertaken on using crosslinking electrospun fibers film obtained in step (d) as on the roller receiver of substrate.
(j) electrospun fibers obtained by step (i) are contained in irradiation bag, are passed through nitrogen for oxygen-barrier in bag, incite somebody to action
Sack sealing；
(k) fiber sealed bag obtained by step (j) is subjected to level electron beam radiation treatment, by fiber cross-linking radiation, irradiation
Dosage is 300kGy, prepares bismuthyl carbonate-polyethylene oxide composite crosslinking electrospun fibers film.
Verify embodiment
Bismuthyl carbonate prepared in the above embodiments-polyethylene oxide composite crosslinking electrospun fibers film is scanned
Electron microscope analysis and absorption-photocatalysis performance experiment.
Bismuthyl carbonate obtained-high-visible point of film particles of inorganic material of polyethylene oxide composite crosslinking electrospun fibers
Cloth is uniform, and spinning fibre is arranged uniformly, and form is complete.Bismuthyl carbonate made from Examples 1 to 3-polyethylene oxide electrostatic spinning
The result of fiber cross linking membrane scanning electron microscope analysis is as shown in Figures 1 to 3.
Bismuthyl carbonate-polyethylene oxide composite crosslinking electrospun fibers film can be carried out effective absorption to methyl orange, and
With preferable degradation rate.Its absorption-photocatalysis performance experimental procedure is as follows: by bismuthyl carbonate/polyethylene oxide electrostatic spinning
Fiber cross linking membrane is added in the methyl orange solution of 20ppm, is protected from light absorption 30min, then the 2h that degrades under ultraviolet light, every
20min sampling, as light urges the progress of experiment, methyl orange solution color is gradually become shallower as, until it is colourless, use uv-spectrophotometric
Landing attempt solution situation is measured, the drop of bismuthyl carbonate-polyethylene oxide electrospun fibers cross linking membrane obtained made from embodiment 1
After result is solved as shown in figure 4, opening UV illumination degradation 2h, degradation rate reaches 78%, and wherein degradation is main removal
Effect.
As can be seen from the above embodiments, the present invention utilizes electron beam to provide energy, three propylene of pentaerythrite during the preparation process
Acid esters is as grafted monomers, and polyethylene oxide tunica fibrosa is cross-linking modified, and polymer forms tridimensional network, can be improved
Solvent resistance, the heat resistance of tunica fibrosa, are easily recycled, and the composite nano fiber of acquisition is to the light for further increasing composite fibre
Catalytic performance has positive meaning, can be used for organic sewage processing.
Specific embodiments of the present invention are described in detail above, but it is only used as example, the present invention is not intended to limit
In particular embodiments described above.To those skilled in the art, the equivalent modifications and replace that any couple of present invention carries out
In generation, is also all among scope of the invention.Therefore, without departing from the spirit and scope of the invention made by equal transformation and repair
Change, all should be contained within the scope of the invention.
Claims (10)
1. a kind of bismuthyl carbonate-polyethylene oxide film preparation method, which comprises the steps of:
Step (1) prepares spinning solution using polyethylene oxide, pentaerythritol triacrylate solution and solvent, and passes through electrostatic
Spinning and electron beam irradiation preparation crosslinking electrospun fibers film；
Step (2) is using polyethylene oxide, bismuthyl carbonate inorganic material, pentaerythritol triacrylate solution and solvent preparation
Spinning solution carries out electrostatic spinning using the crosslinking electrospun fibers film that step (1) obtains as substrate is received, by resulting fibre
Electron beam irradiation processing is carried out after tieing up the oxygen barrier processing of film, obtains bismuthyl carbonate-polyethylene oxide composite crosslinking electrospun fibers
Film.
2. a kind of preparation method of bismuthyl carbonate-polyethylene oxide film according to claim 1, which is characterized in that step
(1) described in be crosslinked electrospun fibers film preparation step include:
(A) polyethylene oxide prepares precursor solution, adds pentaerythritol triacrylate solution, is mixed with spinning with solvent
Liquid；
(B) step (A) described spinning solution prepared is contained in electrostatic spinning apparatus syringe, syringe needle and high pressure
Raw device anode connection, aluminium foil receiver are connect with high pressure receiver cathode, carry out electrospinning, and the tunica fibrosa that electrostatic spinning goes out is undertaken on
On the aluminium foil roller receiver；
(C) the resulting tunica fibrosa of step (B) is subjected to oxygen barrier processing, and carries out electron beam irradiation processing, obtain being crosslinked quiet
Electricity spinning fibre film；
Bismuthyl carbonate described in step (2)-polyethylene oxide composite crosslinking electrospun fibers film preparation step includes:
(a) polyethylene oxide prepares precursor solution, adds bismuthyl carbonate inorganic material, and addition pentaerythritol triacrylate is molten
Liquid is mixed with spinning solution with solvent；
(b) spinning solution prepared by step (a) is contained in electrostatic spinning apparatus syringe, syringe needle and high pressure
Raw device anode connection, aluminium foil receiver are connect with high pressure receiver cathode, and the crosslinking electrostatic spinning that step (C) is obtained is fine
Film is tieed up as substrate is received and carries out electrospinning, the tunica fibrosa that electrostatic spinning goes out is undertaken on the aluminium foil roller receiver；
(c) the resulting tunica fibrosa of step (b) is subjected to oxygen barrier processing, and carries out electron beam irradiation processing, it is poly- to obtain bismuthyl carbonate-
Ethylene oxide composite crosslinking electrospun fibers film.
3. a kind of preparation method of bismuthyl carbonate-polyethylene oxide film according to claim 2, which is characterized in that described
In step (A), in terms of the gross mass of spinning solution, the polyethylene oxide accounts for 8~15%, and the pentaerythritol triacrylate accounts for
1~3%, the solvent includes at least one of methylene chloride, dimethylformamide.
4. a kind of preparation method of bismuthyl carbonate-polyethylene oxide film according to claim 2, which is characterized in that described
In step (a), in terms of the gross mass of spinning solution, the polyethylene oxide accounts for 5~10%, and the bismuthyl carbonate inorganic material accounts for 5
~10%, the pentaerythritol triacrylate accounts for 1~3%, the solvent include methylene chloride, in dimethylformamide extremely
Few one kind.
5. a kind of preparation method of bismuthyl carbonate-polyethylene oxide film according to claim 2, which is characterized in that described
In step (B), syringe spinning head internal diameter is 0.33mm, and syringe spinning head and roller receiver surface distance are 8~15cm,
Application voltage is 10~20kV；Syringe fltting speed is 8~18 μ Lmin-1, it is 60~100rpm, note that roller, which receives speed,
It is 22~30mm that emitter, which injects horizontal reciprocating moving distance,.
6. according to a kind of preparation method of bismuthyl carbonate-polyethylene oxide film as claimed in claim 2, which is characterized in that the step
Suddenly in (b), syringe spinning head internal diameter is 0.60mm, and syringe spinning head and roller receiver surface distance are 8~15cm, is applied
Making alive is 15~20kV；Syringe fltting speed is 18~35 μ Lmin-1, it is 60~100rpm, injection that roller, which receives speed,
It is 25~35mm that device, which injects horizontal reciprocating moving distance,.
7. according to a kind of preparation method of bismuthyl carbonate-polyethylene oxide film as claimed in claim 2, which is characterized in that the electricity
Beamlet irradiation is horizontal irradiation, and dosage is 90~300kGy；The oxygen barrier processing is that tunica fibrosa packs the logical oxygen barrier sealing of nitrogen.
8. according to a kind of preparation method of bismuthyl carbonate-polyethylene oxide film as claimed in claim 2, which is characterized in that described molten
Agent is the mixture of methylene chloride (DCM) and dimethylformamide (DMF).
9. a kind of bismuthyl carbonate as made from preparation method according to any one of claims 1 to 8-polyethylene oxide film.
10. a kind of bismuthyl carbonate as made from preparation method according to any one of claims 1 to 8-polyethylene oxide film exists
Application in sewage treatment.
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