CN109355803A - A kind of preparation method coating polysulfide Electrospun nano-fibers film and its application in the case where aoxidizing stimuli responsive in adsorbing metal ions - Google Patents
A kind of preparation method coating polysulfide Electrospun nano-fibers film and its application in the case where aoxidizing stimuli responsive in adsorbing metal ions Download PDFInfo
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- CN109355803A CN109355803A CN201811455953.1A CN201811455953A CN109355803A CN 109355803 A CN109355803 A CN 109355803A CN 201811455953 A CN201811455953 A CN 201811455953A CN 109355803 A CN109355803 A CN 109355803A
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- 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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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/261—Synthetic macromolecular compounds obtained by reactions only involving carbon to carbon unsaturated bonds
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
- B01J20/28038—Membranes or mats made from fibers or filaments
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- 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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- 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
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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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- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
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- 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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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Abstract
The invention discloses a kind of preparation method for coating polysulfide Electrospun nano-fibers film and its applications in the case where aoxidizing stimuli responsive in adsorbing metal ions, it is to be dissolved in polysulfide in methylene chloride obtaining polysulfide solution, then it instills in Kynoar solution and forms homogeneous blend spinning liquid, then cladding polysulfide Electrospun nano-fibers film is prepared in the method for electrostatic spinning.Such film can significantly improve the adsorbance to metal ion, and have selection characterization of adsorption to special metal.
Description
Technical field
The present invention relates to Material Field, in particular to a kind of preparation method for coating polysulfide Electrospun nano-fibers film and
Its application in the case where aoxidizing stimuli responsive in adsorbing metal ions.
Background technique
Elemental sulfur is a kind of substance of reserves very abundant on the earth, and annual yield is very huge, and purposes is mainly
Produce the vulcanizer in the products such as sulfuric acid and various sulfide and China Synthetic Rubber Industry (such as production tire).However it is traditional
Sulphur-containing substance production industry can generate a large amount of sulphur waste, and the utilization rate of sulphur is not high, and discarded sulphur is usually arranged to big
Naturally, causing the serious wasting of resources and problem of environmental pollution.How a large amount of sulphur is utilized, so that it is turned waste into wealth always difficult
Point.The patent of invention CN201510207935.1 of inventor's earlier application discloses a kind of sulphur/terpene copolymer and its synthesis side
Method, it is using the method for " devulcanization " that terpenes and simple substance sulphur is directly mixed using monoterpene alkene (R)-(+)-limonene as comonomer
It closes and carries out ontology melting free radicals copolymerization reaction, obtain the sulfur-rich oligomer with good solubility.Inventor is further
The study found that this polysulfide (Psf) with good solubility has oxidation stimulating responsive, in different oxidants and different oxygen
Under the effect of change degree, the element sulphur in polysulfide molecule can be oxidized to different structures；And aoxidize polysulfide prove containing sulfone and
Sulfoxide radicals, therefore speculate that it has the ability with metallic ion coordination.
This special nature of polysulfide oxidation front and back can be used for adsorbing different metal ions, and metal ion has difference
Coordination ability, can with different ligands formed different structure complex.Trivalent chromic ion Cr (III), cobalt ions Co
(II), nickel ion Ni (II) is three metal ion species common in industrial wastewater, these metals are after entering environment water, no
It can be by beneficial microbial degradation, it is difficult to be completely eliminated by the self-purification capacity of water body, but also the richness of food chain can be passed through
Collection effect causes the accumulation poisoning of acute food poisoning or body tissue, has and be not easy the characteristic for being metabolized, easily transmitting.
Waste water handling problem is always the critical issue of water prevention and cure of pollution and processing, the relationship people's livelihood and Environmental security, waste water
In metal ion have seriously polluted the environment and endanger human health.How to avoid heavy metal pollution to ecology to greatest extent
It is seriously affected caused by system, people have been working hard the new technology for seeking to handle heavy metal.Currently, a huge sum of money for development and application
Belong to processing method it is very much, mainly have chemical precipitation method, cohesion-flocculence, oxidation-reduction method, ion-exchange, solvent extraction,
Bioremediation, absorption method etc..Wherein, absorption method have it is easy to operate, effective, and be easy to reuse, cost is relatively low
Advantage.Absorption method is substantially that porous adsorbing material is applied to carry out the heavy metal in adsorption treatment waste water, and adsorption mechanism can be divided into object
Reason absorption and chemisorption.Physical absorption generally meets Langmuir adsorption isothermal curve by electrostatic interaction, and part is inhaled
It is re-used for adsorbing after adsorbate being desorbed by processing after attached dose of saturation absorption, be recycled to realize；Chemisorption is logical
It crosses chelation or other chemical bonds adsorbing metal ions, adsorbance and adsorption is stronger.Common adsorbents type
Very much, including active carbon, calcium silicates, zeolite, seaweed etc..
Absorption is a kind of mass transport process, and metal ion is spread by the concentration difference that physical/chemical method is formed to adsorbent,
And the material with bigger serface, suction-operated surface is bigger, and adsorption group has more chances to contact with metal ion, because
And adsorptivity is stronger.Electrostatic spinning nano material has a large amount of reports, Electrospun nano-fibers film for the research of absorption at present
It can be stabilized with large specific surface area, and in aqueous solution, facilitate recycling, there is no secondary pollutions.In addition to this,
Introduce the material of specific specific absorption property in nanofiber, the property of can choose, can anti-interference adsorb and recycles specifically
Metal ion.In nanofiber functional molecular introducing may exist different morphosis, by the selection of spin solvent,
The optimization of spinning technique and the additional proportion of functional molecular can prepare functional molecular cladding and the structure among fiber.This
The fiber of kind clad structure diffuses under capable of preventing adsorbent environmental stimuli from acting on and forms secondary pollution in water, while being saturated suction
Attached adsorbent can be convenient to be taken out in water outlet.
Therefore, polysulfide cladding is stimulated into item in different oxidants and different degree of oxidation with Electrospun nano-fibers
It under part, acts in the aqueous solution containing different metal ions, will have specific absorption property to different metal ions.
Summary of the invention
It is an object of the invention to overcome disadvantage existing in the prior art, a kind of cladding polysulfide electrostatic spinning nano is provided
The preparation method of tunica fibrosa.
Another object of the present invention is to provide a kind of applications of above-mentioned cladding polysulfide Electrospun nano-fibers film, are used for
The adsorbing metal ions in the case where aoxidizing stimuli responsive.
The purpose of the invention is achieved by the following technical solution:
A kind of preparation method coating polysulfide Electrospun nano-fibers film is that polysulfide is dissolved in methylene chloride (DCM) to obtain
To polysulfide solution, then instills in Kynoar (PVDF) solution and form homogeneous blend spinning liquid, then with the side of electrostatic spinning
Cladding polysulfide Electrospun nano-fibers film is prepared in method.
The PVDF solution is that Kynoar is dissolved in the solution of dimethyl acetamide (DMAc), PVDF solution it is dense
Degree is 12~18wt.%, and the dosage of polysulfide is the 10~30% of PVDF mass.
The operating parameter of the electrostatic spinning are as follows: 12~20kV of voltage, 1~4mL/h of speed, receiver sheet distance 10~
15cm。
The application of the cladding polysulfide Electrospun nano-fibers film is will to coat polysulfide Electrospun nano-fibers film use
In the adsorbing metal ions in the case where aoxidizing stimuli responsive, first cladding polysulfide Electrospun nano-fibers film is infiltrated to containing oxidant
Aqueous solution aoxidized, take out clean drying after a certain period of time, be then immersed in the aqueous solution containing metal ion and inhaled
Attached metal ion.
The oxidant is the aqueous solution of hydrogen peroxide or sodium hypochlorite, and oxidant concentration is 0.05~0.25 mmol/L (letter
Claim mM).
The time of the oxidation is 2~for 24 hours, clean and embathed more than three times using distilled water and dehydrated alcohol, absorption when
Between for 0.5~for 24 hours.
The metal ion is one of Cr (III), Co (II), Ni (II)；Initial concentration is 1~100ppm.
The present invention has the following advantages that compared with prior art and effect:
(1) cladding polysulfide Electrospun nano-fibers film of the invention, by the difference for adjusting degree of oxidation and oxidant
Type forms the different oxidation polysulfide molecule of coordinating group, rationally designs the type and initial concentration for being adsorbed metal, compares oxygen
Change the saturated extent of adsorption of front and back and blank control film, such film can significantly improve the adsorbance to metal ion, and right
Special metal has selection characterization of adsorption.
(2) nano fibrous membrane prepared by the present invention and polysulfide structure after oxidation are clear, and property and functionality are controllable, and receive
Rate is higher；Preparation process is simple, can carry out with routine operation and under room temperature, and highly-safe, material post-processing approach is simple and direct,
Test condition and method are simple and easy to get.
(3) present invention be used for water treatment procedure, nano fibrous membrane have facilitate placements, convenient for recycle and not
The advantages of will cause secondary pollution.
Detailed description of the invention
Fig. 1 is the SEM figure of present invention cladding polysulfide Electrospun nano-fibers film.
Fig. 2 be the present invention cladding polysulfide Electrospun nano-fibers film oxidation front and back and blank control sample to three kinds of metals from
The saturated extent of adsorption figure of son.
Specific embodiment
Further detailed description is done to the present invention below with reference to embodiment, embodiments of the present invention are not limited thereto.
Embodiment 1
(1) 0.64g PVDF is added in 10mL serum bottle, 5mL DMAc solvent is added, is stirred well to PVDF and is completely dissolved
Obtain the PVDF solution of concentration 12wt.%；Psf. (polysulfide) 64mg is added in another serum bottle, 2mL DCM, which is added, keeps Psf. complete
Fully dissolved obtains brownish red clear transparent solutions.Psf. solution is slowly added dropwise into the PVDF solution under quick stirring, initially
When Psf. be precipitated in PVDF solution, be sufficiently stirred and be completely dissolved overnight to Psf., mixed solution clear obtains mixing and spins
Silk liquid.
(2) blend spinning liquid obtained by step (1) is added to 15mL dispensing syringe, and folder to electrostatic spinning machine equipment is collected
One layer of reception aluminium foil of roller outer patch, the distance for adjusting roller to syringe needle are 10cm, set spinning voltage 12kV, charging rate 1mL/
H carries out spinning, takes aluminium foil off after spinning, puts to air dry oven the solvent for drying and removing and not volatilizing completely, finally obtain
Coat polysulfide Electrospun nano-fibers film.
(3) cutting out nano fibrous membrane obtained by step (2) is 5 × 5cm2Square tiles youngster, each small block film immerses
20mL concentration is to take out after standing 2h, flushed three times with water and ethyl alcohol in the aqueous hydrogen peroxide solution of 0.05mM, is dried.After drying
Film weigh film quality, each small block film is respectively immersed to 20mL contains (II) three kind of Cr (III), Co (II), Ni metal respectively
In deionized water solution, three metal ion species initial concentrations are 1ppm, are taken out after standing 0.5h, respectively each metal after test absorption
The concentration of ion, and calculate the saturated extent of adsorption of polysulfide.
Concentration of metal ions test method: Cr (III) and Ni (II) uses atomic absorption spectrography (AAS) (AES), and Co (II) is adopted
With inductively coupled plasma mass spectrometry (ICP-MS).
Embodiment 2
(1) 0.82g PVDF is added in 10mL serum bottle, 5mL DMAc solvent is added, is stirred well to PVDF and is completely dissolved
Obtain the PVDF solution of concentration 15wt.%；Psf. 164mg is added in another serum bottle, 2mL DCM, which is added, keeps Psf. completely molten
Solution obtains brownish red clear transparent solutions.Psf. solution is slowly added dropwise into the PVDF solution under quick stirring, when initial
Psf. it is precipitated in PVDF solution, is sufficiently stirred and is completely dissolved overnight to Psf., mixed solution clear obtains blend spinning
Liquid.
(2) blend spinning liquid obtained by step (1) is added to 15mL dispensing syringe, and folder to electrostatic spinning machine equipment is collected
One layer of reception aluminium foil of roller outer patch, the distance for adjusting roller to syringe needle are 12cm, set spinning voltage 15kV, charging rate 2mL/
H carries out spinning, takes aluminium foil off after spinning, puts to air dry oven the solvent for drying and removing and not volatilizing completely, finally obtain
Coat polysulfide Electrospun nano-fibers film.
(3) cutting out nano fibrous membrane obtained by step (2) is 5 × 5cm2Square tiles youngster, each small block film immerses
20mL concentration is to take out after standing 8h, flushed three times with water and ethyl alcohol in the aqueous hydrogen peroxide solution of 0.15mM, is dried.After drying
Film weigh film quality, each small block film is respectively immersed to 20mL contains (II) three kind of Cr (III), Co (II), Ni metal respectively
In deionized water solution, three metal ion species initial concentrations are 10ppm, are taken out after standing 4h, respectively each metal after test absorption
The concentration of ion, and calculate the saturated extent of adsorption of polysulfide.
Embodiment 3
(1) 1.03g PVDF is added in 10mL serum bottle, 5mL DMAc solvent is added, is stirred well to PVDF and is completely dissolved
Obtain the PVDF solution of concentration 18wt.%；Psf. 309mg is added in another serum bottle, 2mL DCM, which is added, keeps Psf. completely molten
Solution obtains brownish red clear transparent solutions.Psf. solution is slowly added dropwise into the PVDF solution under quick stirring, when initial
Psf. it is precipitated in PVDF solution, is sufficiently stirred and is completely dissolved overnight to Psf., mixed solution clear obtains blend spinning
Liquid.
(2) blend spinning liquid obtained by step (1) is added to 15mL dispensing syringe, and folder to electrostatic spinning machine equipment is collected
One layer of reception aluminium foil of roller outer patch, the distance for adjusting roller to syringe needle are 15cm, set spinning voltage 18kV, charging rate 3mL/
H carries out spinning, takes aluminium foil off after spinning, puts to air dry oven the solvent for drying and removing and not volatilizing completely, finally obtain
Coat polysulfide Electrospun nano-fibers film.
(3) cutting out nano fibrous membrane obtained by step (2) is 5 × 5cm2Square tiles youngster, each small block film immerses
20mL concentration is to take out after standing 12h, flushed three times with water and ethyl alcohol in the aqueous hydrogen peroxide solution of 0.25mM, is dried.After drying
Film weigh film quality, each small block film is respectively immersed to 20mL contains (II) three kind of Cr (III), Co (II), Ni metal respectively
In deionized water solution, three metal ion species initial concentrations are 100ppm, are taken out after standing 8h, respectively each metal after test absorption
The concentration of ion, and calculate the saturated extent of adsorption of polysulfide.
Embodiment 4
(1) 0.82g PVDF is added in 10mL serum bottle, 5mL DMAc solvent is added, is stirred well to PVDF and is completely dissolved
Obtain the PVDF solution of concentration 15wt.%；Psf.82 mg is added in another serum bottle, 2mL DCM, which is added, is completely dissolved Psf.
Obtain brownish red clear transparent solutions.Psf. solution is slowly added dropwise into the PVDF solution under quick stirring, Psf. when initial
It is precipitated in PVDF solution, is sufficiently stirred and is completely dissolved overnight to Psf., mixed solution clear obtains blend spinning liquid.
(2) blend spinning liquid obtained by step (1) is added to 15mL dispensing syringe, and folder to electrostatic spinning machine equipment is collected
One layer of reception aluminium foil of roller outer patch, the distance for adjusting roller to syringe needle are 10cm, set spinning voltage 20kV, charging rate 4mL/
H carries out spinning, takes aluminium foil off after spinning, puts to air dry oven the solvent for drying and removing and not volatilizing completely, finally obtain
Coat polysulfide Electrospun nano-fibers film.
(3) cutting out nano fibrous membrane obtained by step (2) is 5 × 5cm2Square tiles youngster, each small block film immerses
20mL concentration is to take out after standing 16h, flushed three times with water and ethyl alcohol in the aqueous sodium hypochlorite solution of 0.05mM, is dried.Drying
Film afterwards weighs film quality, and each small block film is respectively immersed to 20mL contains (II) three kind of Cr (III), Co (II), Ni gold respectively
Belong in deionized water solution, three metal ion species initial concentrations are 1ppm, are taken out after standing 12h, respectively each gold after test absorption
Belong to the concentration of ion, and calculates the saturated extent of adsorption of polysulfide.
Embodiment 5
(1) 0.82g PVDF is added in 10mL serum bottle, 5mL DMAc solvent is added, is stirred well to PVDF and is completely dissolved
Obtain the PVDF solution of concentration 15wt.%；Psf. 164mg is added in another serum bottle, 2mL DCM, which is added, keeps Psf. completely molten
Solution obtains brownish red clear transparent solutions.Psf. solution is slowly added dropwise into the PVDF solution under quick stirring, when initial
Psf. it is precipitated in PVDF solution, is sufficiently stirred and is completely dissolved overnight to Psf., mixed solution clear obtains blend spinning
Liquid.
(2) blend spinning liquid obtained by step (1) is added to 15mL dispensing syringe, and folder to electrostatic spinning machine equipment is collected
One layer of reception aluminium foil of roller outer patch, the distance for adjusting roller to syringe needle are 12cm, set spinning voltage 20kV, charging rate 3mL/
H carries out spinning, takes aluminium foil off after spinning, puts to air dry oven the solvent for drying and removing and not volatilizing completely, finally obtain
Coat polysulfide Electrospun nano-fibers film.
(3) cutting out nano fibrous membrane obtained by step (2) is 5 × 5cm2Square tiles youngster, each small block film immerses
20mL concentration is to take out after standing 18h, flushed three times with water and ethyl alcohol in the aqueous sodium hypochlorite solution of 0.15mM, is dried.Drying
Film afterwards weighs film quality, and each small block film is respectively immersed to 20mL contains (II) three kind of Cr (III), Co (II), Ni gold respectively
Belong in deionized water solution, three metal ion species initial concentrations are 10ppm, are taken out after standing 16h, respectively each gold after test absorption
Belong to the concentration of ion, and calculates the saturated extent of adsorption of polysulfide.
Embodiment 6
(1) 0.82g PVDF is added in 10mL serum bottle, 5mL DMAc solvent is added, is stirred well to PVDF and is completely dissolved
Obtain the PVDF solution of concentration 15wt.%；Psf. 246mg is added in another serum bottle, 2mL DCM, which is added, keeps Psf. completely molten
Solution obtains brownish red clear transparent solutions.Psf. solution is slowly added dropwise into the PVDF solution under quick stirring, when initial
Psf. it is precipitated in PVDF solution, is sufficiently stirred and is completely dissolved overnight to Psf., mixed solution clear obtains blend spinning
Liquid.
(2) blend spinning liquid obtained by step (1) is added to 15mL dispensing syringe, and folder to electrostatic spinning machine equipment is collected
One layer of reception aluminium foil of roller outer patch, the distance for adjusting roller to syringe needle are 15cm, set spinning voltage 15kV, charging rate 2mL/
H carries out spinning, takes aluminium foil off after spinning, puts to air dry oven the solvent for drying and removing and not volatilizing completely, finally obtain
Coat polysulfide Electrospun nano-fibers film.
(3) cutting out nano fibrous membrane obtained by step (2) is 5 × 5cm2Square tiles youngster, each small block film immerses
20mL concentration is in the aqueous sodium hypochlorite solution of 0.25mM, and standing is taken out afterwards for 24 hours, is flushed three times with water and ethyl alcohol, is dried.Drying
Film afterwards weighs film quality, and each small block film is respectively immersed to 20mL contains (II) three kind of Cr (III), Co (II), Ni gold respectively
Belong in deionized water solution, three metal ion species initial concentrations are 100ppm, are taken out after standing 20h, each after test absorption respectively
The concentration of metal ion, and calculate the saturated extent of adsorption of polysulfide.
Embodiment 7
(1) 1.03g PVDF is added in 10mL serum bottle, 5mL DMAc solvent is added, is stirred well to PVDF and is completely dissolved
Obtain the PVDF solution of concentration 18wt.%；Psf. 103mg is added in another serum bottle, 2mL DCM, which is added, keeps Psf. completely molten
Solution obtains brownish red clear transparent solutions.Psf. solution is slowly added dropwise into the PVDF solution under quick stirring, when initial
Psf. it is precipitated in PVDF solution, is sufficiently stirred and is completely dissolved overnight to Psf., mixed solution clear obtains blend spinning
Liquid.
(2) blend spinning liquid obtained by step (1) is added to 15mL dispensing syringe, and folder to electrostatic spinning machine equipment is collected
One layer of reception aluminium foil of roller outer patch, the distance for adjusting roller to syringe needle are 15cm, set spinning voltage 15kV, charging rate 3mL/
H carries out spinning, takes aluminium foil off after spinning, puts to air dry oven the solvent for drying and removing and not volatilizing completely, finally obtain
Coat polysulfide Electrospun nano-fibers film.
(3) cutting out nano fibrous membrane obtained by step (2) is 5 × 5cm2Square tiles youngster, each small block film immerses
20mL concentration is in the aqueous hydrogen peroxide solution of 0.15mM, and standing is taken out afterwards for 24 hours, is flushed three times with water and ethyl alcohol, is dried.After drying
Film weigh film quality, each small block film is respectively immersed to 20mL contains (II) three kind of Cr (III), Co (II), Ni metal respectively
In deionized water solution, three metal ion species initial concentrations are 100ppm, and standing is taken out afterwards for 24 hours, respectively each gold after test absorption
Belong to the concentration of ion, and calculates the saturated extent of adsorption of polysulfide.
Embodiment 8
(1) 0.64g PVDF is added in 10mL serum bottle, 5mL DMAc solvent is added, is stirred well to PVDF and is completely dissolved
Obtain the PVDF solution of concentration 12wt.%；Psf. 192mg is added in another serum bottle, 2mL DCM, which is added, keeps Psf. completely molten
Solution obtains brownish red clear transparent solutions.Psf. solution is slowly added dropwise into the PVDF solution under quick stirring, when initial
Psf. it is precipitated in PVDF solution, is sufficiently stirred and is completely dissolved overnight to Psf., mixed solution clear obtains blend spinning
Liquid.
(2) blend spinning liquid obtained by step (1) is added to 15mL dispensing syringe, and folder to electrostatic spinning machine equipment is collected
One layer of reception aluminium foil of roller outer patch, the distance for adjusting roller to syringe needle are 15cm, set spinning voltage 15kV, charging rate 3mL/
H carries out spinning, takes aluminium foil off after spinning, puts to air dry oven the solvent for drying and removing and not volatilizing completely, finally obtain
Coat polysulfide Electrospun nano-fibers film.
(3) nano fibrous membrane obtained by step (2) is cut out to the square tiles youngster for being 5 × 5cm, each small block film immerses 20mL
Concentration is in the aqueous sodium hypochlorite solution of 0.15mM, and standing is taken out afterwards for 24 hours, is flushed three times with water and ethyl alcohol, is dried.After drying
Film weigh film quality, each small block film respectively immerse to 20mL contain respectively Cr (III), Co (II), (II) three kind of metal of Ni from
In sub- aqueous solution, three metal ion species initial concentrations are 100ppm, and standing is taken out afterwards for 24 hours, respectively each metal after test absorption
The concentration of ion, and calculate the saturated extent of adsorption of polysulfide.
Test case
As shown in Figure 1, the fiber size of cladding polysulfide Electrospun nano-fibers film prepared by the present invention 100~
200nm has very big specific surface area advantage.
As shown in Fig. 2, comparative analysis coats polysulfide Electrospun nano-fibers film (Psf.), polysulfide oxygen before polysulfide oxidation
After change (O.Psf.) and blank control sample (PVDF) to Cr (III), Co (II), (II) three metal ion species of Ni saturated extent of adsorption.
The study found that the cladding polysulfide Electrospun nano-fibers film after oxidation obviously increases metal ion saturated extent of adsorption, it is seen then that
Cladding polysulfide Electrospun nano-fibers film after oxidation has apparent characterization of adsorption to metal ion, and to Co's (II)
Adsorbance is maximum.
Table 1 is that polysulfide Electrospun nano-fibers film is coated after aoxidizing obtained by each embodiment to the saturation of three metal ion species
Adsorbance summarizes.According to test result, the cladding polysulfide Electrospun nano-fibers films of different degree of oxidation to three kinds of metals from
Son has certain adsorption capacity, and has significant saturated extent of adsorption for Co (II).As it can be seen that surface coats polysulfide nanofiber
Film has the feasibility used as adsorbent in the case where aoxidizing stimuli responsive completely.
Table 1 aoxidize after cladding polysulfide Electrospun nano-fibers film to the saturated extent of adsorption of three metal ion species
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (9)
1. a kind of preparation method for coating polysulfide Electrospun nano-fibers film, it is characterised in that: be that polysulfide is dissolved in dichloromethane
Polysulfide solution is obtained in alkane, is then instilled in Kynoar solution and is formed homogeneous blend spinning liquid, then with the side of electrostatic spinning
Cladding polysulfide Electrospun nano-fibers film is prepared in method.
2. the preparation method of cladding polysulfide Electrospun nano-fibers film according to claim 1, it is characterised in that: described
Kynoar solution is that Kynoar is dissolved in the solution of dimethyl acetamide, the concentration of Kynoar solution is 12~
18wt.%.
3. the preparation method of cladding polysulfide Electrospun nano-fibers film according to claim 1, it is characterised in that: polysulfide
Dosage be Kynoar quality 10~30%.
4. the preparation method of cladding polysulfide Electrospun nano-fibers film according to claim 1, it is characterised in that: described
The operating parameter of electrostatic spinning are as follows: 12~20kV of voltage, 1~4mL/h of speed, 10~15cm of receiver sheet distance.
5. a kind of application for coating polysulfide Electrospun nano-fibers film, it is characterised in that: being will be any in Claims 1 to 4
The cladding polysulfide Electrospun nano-fibers film that the method is prepared be used in the case where aoxidizing stimuli responsive adsorbing metal from
Son.
6. the application of cladding polysulfide Electrospun nano-fibers film according to claim 5, it is characterised in that: first will cladding
Polysulfide Electrospun nano-fibers film, which is infiltrated to the aqueous solution containing oxidant, to be aoxidized, and is taken out to clean after a certain period of time and is dried
It is dry, it is then immersed in the aqueous solution containing metal ion and carries out adsorbing metal ions.
7. the application of cladding polysulfide Electrospun nano-fibers film according to claim 6, it is characterised in that: the oxidation
Agent is the aqueous solution of hydrogen peroxide or sodium hypochlorite, and oxidant concentration is 0.05~0.25mmol/L.
8. the application of cladding polysulfide Electrospun nano-fibers film according to claim 6, it is characterised in that: the oxidation
Time be 2~for 24 hours, clean and embathed more than three times using distilled water and dehydrated alcohol, the time of absorption is 0.5~for 24 hours.
9. the application of cladding polysulfide Electrospun nano-fibers film according to claim 6, it is characterised in that: the metal
Ion is one of Cr (III), Co (II), Ni (II).
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