CN105544093A - Preparation method and application of functional AOPAN-RC composite nanofiber film - Google Patents
Preparation method and application of functional AOPAN-RC composite nanofiber film Download PDFInfo
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- CN105544093A CN105544093A CN201610070992.4A CN201610070992A CN105544093A CN 105544093 A CN105544093 A CN 105544093A CN 201610070992 A CN201610070992 A CN 201610070992A CN 105544093 A CN105544093 A CN 105544093A
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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
- D04H1/70—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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/74—Natural macromolecular material or derivatives thereof
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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
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/30—Chemical resistance
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Abstract
The invention discloses a preparation method and application of a functional AOPAN-RC composite nanofiber film. The method includes the following steps that firstly, polyacrylonitrile (PAN) and cellulose acetate (CA) are dissolved in a polar organic solvent for electrostatic spinning, and an electrostatic spinning process is adopted for preparing a PAN-CA composite nanofiber film; secondly, a 0.02-0.15 mol/L strong alkaline solution is adopted for carrying out hydrolysis modification on the PAN-CA composite nanofiber film to prepare a PAN-RC composite nanofiber film; a 0.1-0.2 mol/L hydroxylamine hydrochloride solution is adopted for carrying out amidoximation modification on the PAN-RC composite nanofiber film to obtain the functional AOPAN-RC composite nanofiber film. According to the method, as a large number of functional groups such as hydroxyl and amino are instructed in the modification process, the omposite nanofiber film has multifunctionality.
Description
Technical field
The invention belongs to nanofiber technical field of membrane, be specifically related to a kind of preparation method and application thereof of functional AOPAN-RC composite nano-fiber membrane.
Background technology
Polyacrylonitrile (PAN), is a kind of polymer or copolymer prepared through polymerisation by acrylonitrile monemer, is widely used in weaving, the industries such as battery.But, PAN fiber due to intensity not high, the shortcomings such as ABRASION RESISTANCE is poor, and fatigue resistance is also poor, and hydrophily is bad, the also range of application limiting PAN to a certain degree.For these shortcomings, carry out a lot of research both at home and abroad: mainly the PAN of normal dia is hydrolyzed modification, or the composite spinning liquid prepared containing Functional Polymer carries out electrostatic spinning, but above method often just improves the single performance of PAN aspect, effect is also not obvious.
Cellulose acetate (CA), also known as cellulose acetate, is cellulosic acetate, is generally used for Filters, sheet material, sheet material, the fields such as electric thin.Although cellulose acetate membrane has good hydrophilic property, specific area is large, and the advantages such as plasticity is better, because its mechanical strength is not high, be subject to the Application Areas that the features such as bioerosion, not acid and alkali-resistance often also limit it.For the above deficiency of cellulose acetate membrane, the past, people often adopted graft modification, and with the modification of nitromethane gas, the method for modifying such as physical mechanical modification carry out modification to it, but functional effect modification is comparatively single.
Electrostatic spinning and polymeric spray electrostatic stretch spin processes are exactly the special shape of polymeric fluid electrostatic atomization, and now the material is divided in atomization is not fine droplet, but the small jet of polymer, quite long distance can be run, be finally solidified into fiber.Electrostatic spinning is that unique one can be direct at present, the effective and the easiest method of continuous production nanofiber.Electrostatic spinning is a kind of special fiber fabrication process, and polymer solution or melt flow and distortion in highfield, then solidifies, so obtain fibrous material through solvent evaporation or melt cooling.Under electric field action, the drop at syringe needle place can become taper shape (i.e. " taylor cone ") from spherical, and obtains fiber filaments from conical tip extension.This kind of mode can obtain the fiber filaments of nanometer grade diameter.Electrostatic spinning can produce superfine fibre as one, the technology of simple and effective, although the concern just obtaining people in recent years gradually, development speed is very fast.For the polymer with fibre-forming performance, method of electrostatic spinning all can be adopted to prepare nanofiber.
Complexing of metal ion reaction refers to by transition metal ions (such as Fe
3+, Ag
+, Cu
2+deng) and other contain the reaction of the complicated ions that the molecule of two or more lone pair electrons or ion are combined by coordinate bond and formed.In any state, every compound be made up of complex ion or complex molecule, is called complex compound, as complex salt Ag (NH
3)
2cl, complex acid H
2ptCl
6, network alkali Cu (NH
3)
4(OH)
2deng.When forming complex compound, central ion provides unoccupied orbital, and ligand provides lone pair electrons.Complex reaction is widely used in the various isolating and measuring method of analytical chemistry, and as many developers, extractant, precipitating agent, screening agent etc. are all complexing agents, therefore, about the theory and practice knowledge of complex reaction, are one of important contents of analytical chemistry.
Summary of the invention
According to above the deficiencies in the prior art, technical problem to be solved by this invention is the preparation method and the application thereof that propose a kind of functional AOPAN-RC composite nano-fiber membrane, object improves the hydrophilicity of PAN and the brute force of CA and resistance to acids and bases, makes AOPAN-RC composite nano-fiber membrane have multifunctionality.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is:
A preparation method for functional AOPAN-RC composite nano-fiber membrane, the method comprises the steps:
Step one, polyacrylonitrile (PAN) and cellulose acetate (CA) are dissolved in the polar organic solvent for electrostatic spinning, the mass fraction that preparation PAN and CA accounts for gross weight is the electrostatic spinning solution of 10-12%, and adopts electrostatic spinning process to prepare PAN/CA composite nano-fiber membrane; The polyacrylonitrile wherein adopted is polyacrylonitrile powder (PAN, Mw=90000g/mol), and cellulose acetate is celluloseacetate flake (Mw=131900g/mol);
Step 2, adopts the strong base solution of 0.02-0.15mol/L to prepare PAN/RC composite nano-fiber membrane to the modification that is hydrolyzed of PAN/CA composite nano-fiber membrane;
Step 3, adopts the hydroxylamine hydrochloride solution of 0.1-0.2mol/L to carry out amidoxime modification to PAN/RC composite nano-fiber membrane and obtains AOPAN-RC composite nano-fiber membrane.
The mass ratio 4:1-1:1 of PAN and CA described in step one.Adopt this ratio to prepare and all can obtain form PAN/CA composite nano-fiber membrane relatively preferably.
The mass ratio of described PAN and CA is 7:3.The PAN/CA composite nano-fiber membrane form adopting this ratio to be prepared is better, and the modified performance of composite nano-fiber membrane is also more stable.
Described polar organic solvent is DMF, dimethylacetylamide or dimethyl sulfoxide (DMSO).
Electrostatic spinning process described in step one comprises spinning head and receiving system, concrete electrostatic spinning process parameter is: the distance of spinning head and receiving system is 18-20cm, spinning solution flow velocity is 0.5-1.2ml/h, and applying voltage is 18-20kV, receives 10-20 hour by aluminium foil.
The method preparing PAN/RC composite nano-fiber membrane described in step 2 is: the first strong base solution reaction of first PAN/CA composite nano-fiber membrane being put into 0.02-0.06mol/L is spent the night; The second strong base solution reaction of putting into 0.08-0.15mol/L after taking out washing is again spent the night, obtained after washing, drying.Adopt and first react with the strong base solution of low concentration, react with the strong base solution of relatively high concentration again, the PAN/RC composite nano-fiber membrane of preparation is enable better to introduce the functional groups such as-OH, the advantage of further reinforcement PAN and CA, hydrophilicity strengthens, preparation form is better, the composite nano-fiber membrane that performance is more stable.First strong base solution and the second strong base solution are preferably same strong base solution.
The concentration of described first strong base solution is 0.05mol/L, and the concentration of described second strong base solution is 0.1mol/L.Successively the aqueous alkali concentration of twice adopts two above-mentioned concentration, is the solution concentration requirement of the best.
Described in step 3, the preparation method of AOPAN-RC composite nano-fiber membrane is at 65-68 DEG C of temperature, PAN/RC composite nano-fiber membrane being put into pH is 6.5-7, concentration is react in the hydroxylamine hydrochloride solution of 0.1-0.2mol/L, obtained after washing, drying after taking-up.
Described pH is 7, and the concentration of described hydroxylamine hydrochloride is 0.15mol/L.The amidoxime carried out under this condition is modified as optimum condition, through experiment draw can with above-mentioned steps in better act synergistically, while strengthening composite nano-fiber membrane performance, make its form better.
Accordingly, the present invention's application of AOPAN-RC composite nano-fiber membrane in separating and purifying serum albumin and adsorbing metal ions of also providing the preparation method of functional AOPAN-RC composite nano-fiber membrane to prepare.
Beneficial effect of the present invention is: the AOPAN-RC composite nano-fiber membrane that the present invention utilizes electrostatic spinning and chemical modification to prepare, not only improve the hydrophily of PAN greatly, and well play the advantage of cellulose acetate, strengthen the resistance to acids and bases of cellulose acetate and the performance such as powerful; AOPAN/RC composite nano-fiber membrane prepared by the present invention, because in the process of modification, fiber introduces the functional groups such as numerous hydroxyls, amino, composite nano fiber is made to possess multifunctionality, there is better absorption property compared with the PAN nanofiber membrane of routine, can be used as the nano-filtration membrane of catching heavy metal ion and organic pollution in molecular filter or wastewater treatment, and large molecule milipore filter, thus well expand the Application Areas of PAN tunica fibrosa, and be easy to reclaim use.
Accompanying drawing explanation
Below the content expressed by this Figure of description and the mark in figure are briefly described:
Fig. 1 is the SEM figure that the present invention prepares the composite nano-fiber membrane in each step of functional AOPAN-RC composite nano-fiber membrane;
Wherein a is that PAN/CA composite nano fiber SEM schemes; B is that PAN/RC composite nano fiber SEM schemes; C is that AOPAN/RC composite nano fiber SEM schemes;
Fig. 2 is that functional AOPAN/RC composite nano fiber EDX of the present invention schemes;
Fig. 3 is the EDX figure of functional AOPAN/RC composite nano fiber absorbing copper ion of the present invention;
Fig. 4 is the EDX figure of functional AOPAN/RC composite nano fiber absorption iron ion of the present invention;
Fig. 5 is the EDX figure of functional AOPAN/RC composite nano fiber Adsorption of Cadmium of the present invention.
Detailed description of the invention
Contrast accompanying drawing below, by the description to embodiment, the specific embodiment of the present invention is as the effect of the mutual alignment between the shape of involved each component, structure, each several part and annexation, each several part and operation principle, manufacturing technique and operation using method etc., be described in further detail, have more complete, accurate and deep understanding to help those skilled in the art to inventive concept of the present invention, technical scheme.
Embodiment 1
1. first, the 1.32g cellulose acetate section accurately taken and 3.08gPAN powder put into 50ml conical flask, then 35.6gDMF solvent is added, under being put in the water bath with thermostatic control of 40 DEG C, magnetic agitation 6 is little of abundant dissolving, and obtained gross mass mark is the PAN/CA composite spinning solution (wherein the mass ratio of PAN and CA is 7:3) of 11%.
2. the even spinning solution of PAN/CA of preparation in step 1 is loaded in the syringe of 10ml, polish flat with the syringe needle that internal diameter is 0.7mm by abrasive machine.The positive pole of high voltage source is connected on the needle point of the syringe being horizontally fixed on syringe pump.At room temperature, regulate spinning solution flow to be 0.5ml/h, the voltage 18kv applied, and needle point is to the distance 20cm of colelctor electrode.One piece of aluminium foil covers the receiving system of fixing rectangle copper mesh collector as nanofiber of a ground connection, receives 20h.The nano fibrous membrane prepared by electrostatic spinning is dry 2h in 40 DEG C of vacuum drying chambers, prepares functionalized polypropylene nitrile/cellulose acetate composite nano fiber.
3. the NaOH powder accurately taking 2g puts it in the distilled water of 1L, obtained concentration is the NaOH solution of 0.05mol/L, the PAN/CA composite nano-fiber membrane prepared is put into the NaOH solution of 0.05mol/L, after being placed on shady and cool ventilation place reaction 24h, take out tunica fibrosa, clean 3 times with distilled water.And then the NaOH powder accurately taking 4g puts it in the distilled water of 1L, obtained concentration is the NaOH solution of 0.1mol/L, tunica fibrosa after cleaning is put into the NaOH solution that concentration is 0.1mol/L again, after being placed on shady and cool ventilation place reaction 24h, again tunica fibrosa is taken out, after cleaning 3 times with distilled water, put into the baking oven that temperature is 40 DEG C, dry 2h, obtains PAN/RC composite nano-fiber membrane.
4. accurately take hydroxylamine hydrochloride, be dissolved in distilled water, obtained concentration is the hydroxylamine hydrochloride solution of 0.15mol/L, and putting it into temperature is in the water-bath of 65 DEG C, and the pH value of solution is adjusted to 7.Accurately take the PAN/RC tunica fibrosa that quality is 1g, PAN/RC composite nano-fiber membrane is put into solution and paves as much as possible, reaction 2h, takes out tunica fibrosa, cleans 3 times with distilled water.Nano fibrous membrane is put in the drying box of 40 DEG C, drying 2h, preparation AOPAN/RC composite nano-fiber membrane.
5. accurately take tunica fibrosa quality before and after PAN/RC composite nano-fiber membrane amidoxime modified-reaction, calculate its amidoxime conversion ratio according to correlation formula.
Embodiment 2
1. first, the cellulose acetate section and the 2.80gPAN powder that accurately take 1.20g put into 50ml conical flask, then 36.0gDMF solvent is added, under being put in the water bath with thermostatic control of 40 DEG C, magnetic agitation 6 is little of abundant dissolving, and obtained gross mass mark is the PAN/CA composite spinning solution (wherein the mass ratio of PAN and CA is 7:3) of 10%.
2. the even spinning solution of PAN/CA of preparation in step 1 is loaded in the syringe of 10ml, polish flat with the syringe needle that internal diameter is 0.7mm by abrasive machine.The positive pole of high voltage source is connected on the needle point of the syringe being horizontally fixed on syringe pump.At room temperature, regulate spinning solution flow to be 0.8ml/h, the voltage 19kv applied, and needle point is to the distance 20cm of colelctor electrode.One piece of aluminium foil covers the receiving system of fixing rectangle copper mesh collector as nanofiber of a ground connection, receives 20h.The nano tunica fibrosa prepared by electrostatic spinning dry 2h in 40 DEG C of vacuum drying chambers, prepares functionalized polypropylene nitrile/cellulose acetate composite nano fiber.
3. the NaOH powder accurately taking 2g puts it in the distilled water of 1L, obtained concentration is the NaOH solution of 0.05mol/L, the PAN/CA composite nano-fiber membrane prepared is put into the NaOH solution of 0.05mol/L, after being placed on shady and cool ventilation place reaction 24h, take out tunica fibrosa, clean 3 times with distilled water.And then the NaOH powder accurately taking 4g puts it in the distilled water of 1L, obtained concentration is the NaOH solution of 0.1mol/L, tunica fibrosa after cleaning is put into the NaOH solution that concentration is 0.1mol/L again, after being placed on shady and cool ventilation place reaction 24h, again tunica fibrosa is taken out, after cleaning 3 times with distilled water, put into the baking oven that temperature is 40 DEG C, dry 2h, obtains PAN/RC composite nano-fiber membrane.
4. accurately take hydroxylamine hydrochloride, be dissolved in distilled water, obtained concentration is the hydroxylamine hydrochloride solution of 0.15mol/L, and putting it into temperature is in the water-bath of 67 DEG C, and the pH value of solution is adjusted to 7.Accurately take the PAN/RC tunica fibrosa that quality is 0.8g, PAN/RC composite nano-fiber membrane is put into above-mentioned hydroxylamine hydrochloride solution, reaction 2h, takes out tunica fibrosa, cleans 3 times with distilled water.Nano fibrous membrane is put in the drying box of 40 DEG C, drying 2h, preparation AOPAN/RC composite nano-fiber membrane.
5. accurately take tunica fibrosa quality before and after PAN/RC composite nano-fiber membrane amidoxime modified-reaction, calculate its amidoxime conversion ratio according to correlation formula.
Embodiment 3
1. first, the 1.44g cellulose acetate section accurately taken and 3.36gPAN powder put into 50ml conical flask, then 35.2gDMF solvent is added, under being put in the water bath with thermostatic control of 40 DEG C, magnetic agitation 6 is little of abundant dissolving, and obtained gross mass mark is the PAN/CA composite spinning solution (wherein the mass ratio of PAN and CA is 7:3) of 12%.
2. the even spinning solution of PAN/CA of preparation in step 1 is loaded in the syringe of 10ml, polish flat with the syringe needle that internal diameter is 0.7mm by abrasive machine.The positive pole of high voltage source is connected on the needle point of the syringe being horizontally fixed on syringe pump.At room temperature, regulate spinning solution flow to be 0.7ml/h, the voltage 18.5kv applied, and needle point is to the distance 19cm of colelctor electrode.One piece of aluminium foil covers the receiving system of fixing rectangle copper mesh collector as nanofiber of a ground connection, receives 20h.The nano tunica fibrosa prepared by electrostatic spinning dry 2h in 45 DEG C of vacuum drying chambers, prepares functionalized polypropylene nitrile/cellulose acetate composite nano fiber.
3. the NaOH powder accurately taking 2g puts it in the distilled water of 1L, obtained concentration is the NaOH solution of 0.05mol/L, the PAN/CA composite nano-fiber membrane prepared is put into the NaOH solution of 0.05mol/L, after being placed on shady and cool ventilation place reaction 24h, take out tunica fibrosa, clean 3 times with distilled water.And then the NaOH powder accurately taking 4g puts it in the distilled water of 1L, obtained concentration is the NaOH solution of 0.1mol/L, tunica fibrosa after cleaning is put into the NaOH solution that concentration is 0.1mol/L again, after being placed on shady and cool ventilation place reaction 24h, again tunica fibrosa is taken out, after cleaning 3 times with distilled water, put into the baking oven that temperature is 40 DEG C, dry 2h, obtains PAN/RC composite nano-fiber membrane.
4. accurately take hydroxylamine hydrochloride, be dissolved in distilled water, obtained concentration is the hydroxylamine hydrochloride solution of 0.15mol/L, and putting it into temperature is in the water-bath of 65 DEG C, and the pH value of solution is adjusted to 7.Accurately take the PAN/RC tunica fibrosa that quality is 1.2g, PAN/RC composite nano-fiber membrane is put into solution and paves as much as possible, reaction 2h, takes out tunica fibrosa, cleans 3 times with distilled water.Nano fibrous membrane is put in the drying box of 45 DEG C, drying 2h, preparation AOPAN/RC composite nano-fiber membrane.
5. accurately take tunica fibrosa quality before and after PAN/RC composite nano-fiber membrane amidoxime modified-reaction, calculate its amidoxime conversion ratio according to correlation formula.
Embodiment 4
The difference of the present embodiment and embodiment 1 is, in step 3, first add 0.04mol/L NaOH solution reaction, after add 0.12mol/L NaOH solution reaction.
Embodiment 5
The difference of the present embodiment and embodiment 1 is, in step 4, the concentration of hydroxylamine hydrochloride solution is 0.2mol/L.
Embodiment 6
The difference of the present embodiment and embodiment 1 is, in step 4, the concentration of hydroxylamine hydrochloride solution is 0.1mol/L.
Embodiment 7
The difference of the present embodiment and embodiment 1 is, the mass ratio of PAN and the CA that step 1 adopts is 8:2.
Embodiment 8
The difference of the present embodiment and embodiment 1 is, the mass ratio of PAN and the CA that step 1 adopts is 5:5.
Go out from the experimental results, the functional AOPAN-RC composite nano-fiber membrane form that functional AOPAN-RC composite nano-fiber membrane prepared by embodiment 1-3 is prepared than embodiment 4-8 is better, and performance is more stable.
Now optical contact angle measuring instrument (DSA25) is used to carry out hydrophilicity test the functional AOPAN-RC composite nano-fiber membrane prepared in embodiment 1-3.
As can be seen from Table 1, functional AOPAN-RC composite nano-fiber membrane (static contact angle is 10.87 °) prepared by embodiment 1-3 compares with PAN nanofiber membrane (static contact angle is 118.60 °), and known hydrophilicity improves a lot.
Static contact angle (°) test result of functional AOPAN-RC nanofiber prepared by table 1 embodiment 1-3
| Static contact angle (θ) | |
| Embodiment 1 | 11.40 |
| Embodiment 2 | 10.30 |
| Embodiment 3 | 10.90 |
The functional AOPAN-RC composite nano-fiber membrane prepared in embodiment 1-3 is put in the Fe that concentration is 100mmol/L respectively
3+and Cu
2+and Cd
2+in ionic metal solion, after 24h concussion, take out and dry.As shown in Fig. 2 to 5, functional AOPAN-RC composite nano-fiber membrane is to Fe
3+and Cu
2+and Cd
2+the absorption EDX of ion schemes.And calculate nanofiber adsorbing metal ions amount in table 2 (the metal ion quality representation that the composite nano fiber of adsorption of metal ions amount unit grammes per square metre adsorbs).Then Fe will be adsorbed with
3+and Cu
2+and Cd
2+ion composite nano fiber is put in the hydrochloric acid solution of 0.1mol/L, after 2h vibration, takes out dry.Calculate the desorption efficiency of nanofiber in table 2 (desorption efficiency accounts for the metal ion of composite nano fiber desorb the percentage adsorbing total metal ion and represents).AOPAN/RC composite nano fiber can Fe in efficient adsorption industrial wastewater as shown in Table 2
3+, Cu
2+and Cd
2+deng metal ion, and have and reuse ability preferably.
Functional AOPAN-RC composite nano-fiber membrane adsorption of metal ions amount prepared by table 2 embodiment 1-3 and desorption efficiency
By the functional AOPAN-RC composite nano-fiber membrane prepared in embodiment 1-3 for separating of purified serum albumin solution, be 0.1Mpa at operating pressure, processing time is under 90min condition, the rate and protein retention of calculating nano fibrous membrane and the permeation flux of solution are in table 3 (wherein, rate and protein retention refers to the ratio of total amount in the amount and shared solution that in solution, seralbumin tunicle retains, solution permeation flux also claims membrane flux, refers to representing flux by the serum albumin solution volume of per membrane area in the unit interval).AOPAN/RC composite nano-fiber membrane can efficient separation of serum albumin solution as shown in Table 3.
Functional AOPAN-RC composite nano-fiber membrane rate and protein retention prepared by table 3 embodiment 1-3 and membrane flux
Above by reference to the accompanying drawings to invention has been exemplary description; obvious specific implementation of the present invention is not subject to the restrictions described above; as long as have employed the improvement of the various unsubstantialities that method of the present invention is conceived and technical scheme is carried out; or design of the present invention and technical scheme directly applied to other occasion, all within protection scope of the present invention without to improve.The protection domain that protection scope of the present invention should limit with claims is as the criterion.
Claims (10)
1. a preparation method for functional AOPAN-RC composite nano-fiber membrane, it is characterized in that, the method comprises the steps:
Step one, polyacrylonitrile (PAN) and cellulose acetate (CA) are dissolved in the polar organic solvent for electrostatic spinning, the mass fraction that preparation PAN and CA accounts for gross weight is the electrostatic spinning solution of 10-12%, and adopts electrostatic spinning process to prepare PAN/CA composite nano-fiber membrane;
Step 2, adopts the strong base solution of 0.02-0.15mol/L to prepare PAN/RC composite nano-fiber membrane to the modification that is hydrolyzed of PAN/CA composite nano-fiber membrane;
Step 3, adopts the hydroxylamine hydrochloride solution of 0.1-0.2mol/L to carry out amidoxime modification to PAN/RC composite nano-fiber membrane and obtains AOPAN-RC composite nano-fiber membrane.
2. the preparation method of functional AOPAN-RC composite nano-fiber membrane according to claim 1, is characterized in that: the mass ratio 4:1-1:1 of PAN and CA described in step one.
3. the preparation method of functional AOPAN-RC composite nano-fiber membrane according to claim 2, is characterized in that: the mass ratio of described PAN and CA is 7:3.
4. the preparation method of functional AOPAN-RC composite nano-fiber membrane according to claim 1, is characterized in that: described polar organic solvent is DMF, dimethylacetylamide or dimethyl sulfoxide (DMSO).
5. the preparation method of functional AOPAN-RC composite nano-fiber membrane according to claim 1, it is characterized in that, electrostatic spinning process described in step one comprises spinning head and receiving system, concrete electrostatic spinning process parameter is: the distance of spinning head and receiving system is 18-20cm, spinning solution flow velocity is 0.5-1.2ml/h, applying voltage is 18-20kV, receives 10-20 hour by aluminium foil.
6. the preparation method of functional AOPAN-RC composite nano-fiber membrane according to claim 1, it is characterized in that, the method preparing PAN/RC composite nano-fiber membrane described in step 2 is: the first strong base solution reaction of first PAN/CA composite nano-fiber membrane being put into 0.02-0.06mol/L is spent the night; The second strong base solution reaction of putting into 0.08-0.15mol/L after taking out washing is again spent the night, obtained after washing, drying.
7. the preparation method of functional AOPAN-RC composite nano-fiber membrane according to claim 6, it is characterized in that: the concentration of described first strong base solution is 0.05mol/L, the concentration of described second strong base solution is 0.1mol/L.
8. the preparation method of functional AOPAN-RC composite nano-fiber membrane according to claim 1, it is characterized in that: the preparation method of AOPAN-RC composite nano-fiber membrane described in step 3 is at 65-68 DEG C of temperature, PAN/RC composite nano-fiber membrane being put into pH is 6.5-7, concentration is react in the hydroxylamine hydrochloride solution of 0.1-0.2mol/L, obtained after washing, drying after taking-up.
9. the preparation method of functional AOPAN-RC composite nano-fiber membrane according to claim 8, it is characterized in that: described pH is 7, the concentration of described hydroxylamine hydrochloride is 0.15mol/L.
10. the application of AOPAN-RC composite nano-fiber membrane in separating and purifying serum albumin prepared of the preparation method of functional AOPAN-RC composite nano-fiber membrane described in any one of claim 1-9.
Priority Applications (1)
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| CN106350946A (en) * | 2016-10-17 | 2017-01-25 | 安徽工程大学 | Preparation method of functional PU-RC (Poly Urethane-Regenerated Cellulose) composite nanofiber membrane and application thereof |
| CN106480710A (en) * | 2016-09-23 | 2017-03-08 | 安徽工程大学 | A kind of preparation method of feature PU AOPAN composite nano-fiber membrane |
| CN108103662A (en) * | 2018-01-25 | 2018-06-01 | 天津工业大学 | For the amino acid engrafted nanometer fiber membrane preparation method of bilirubin adsorption |
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| CN112127011A (en) * | 2020-09-28 | 2020-12-25 | 湘潭大学 | Polyacrylonitrile/cellulose composite fiber membrane and preparation method and application thereof |
| CN112127011B (en) * | 2020-09-28 | 2023-01-03 | 湘潭大学 | Polyacrylonitrile/cellulose composite fiber membrane and preparation method and application thereof |
| CN112726028A (en) * | 2020-12-28 | 2021-04-30 | 中南大学 | Super-hydrophilic composite nanofiber membrane with coarse structure and preparation and application thereof |
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| CN113206260A (en) * | 2021-04-25 | 2021-08-03 | 西安电子科技大学 | Self-supporting M-N/C oxygen reduction catalyst and preparation method and application thereof |
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