CN109731479A - A kind of preparation method and super-hydrophobic nano tunica fibrosa of super-hydrophobic nano tunica fibrosa - Google Patents
A kind of preparation method and super-hydrophobic nano tunica fibrosa of super-hydrophobic nano tunica fibrosa Download PDFInfo
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- CN109731479A CN109731479A CN201811577376.3A CN201811577376A CN109731479A CN 109731479 A CN109731479 A CN 109731479A CN 201811577376 A CN201811577376 A CN 201811577376A CN 109731479 A CN109731479 A CN 109731479A
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Abstract
The invention discloses a kind of preparation method of super-hydrophobic nano tunica fibrosa and super-hydrophobic nano tunica fibrosas, including, monomer bibenzene tetracarboxylic dianhydride and p-phenylenediamine are dissolved in N, in dinethylformamide, reaction synthesis PAA under low temperature, after PAA nano fibrous membrane is made in PAA by electrostatic spinning, imidization is carried out, PI film is obtained；LBL self-assembly is carried out using ferric trichloride and phytic acid and PDMS solution dip-coating is modified obtains the super-hydrophobic nano tunica fibrosa.The present invention realizes the utilization of LBL self-assembly structure, introduces silane coupling agent again on this basis, and the two combines, and has obtained the water-oil separationg film with super-hydrophobic super-oleophylic wetability.Shaggy nanostructure, which has, improves water-oil separating performance, this membrane separation efficiency can reach 99% or more, and verified, is recycled and reuses.
Description
Technical field
The invention belongs to water-oil separationg film preparation technical fields, and in particular to a kind of preparation side of super-hydrophobic nano tunica fibrosa
Method and super-hydrophobic nano tunica fibrosa.
Background technique
Traditional oil-water separation method includes biological treatment, condensation, air bearing, absorption, but these methods have separation effect
The limitation for the problems such as rate is low, and energy consumption is high, complex process, is also easy to produce secondary pollution.Therefore, a kind of effective grease point is developed
It is extremely urgent from technology.
In recent years, membrane separation process is because its is easy to operate, separative efficiency is high, low manufacture cost, flexibility is good, environment is controllable etc.
Advantage is acknowledged as the substitute technology of oil water mixture separation.Therefore, more and more research work are focused on based on polymer
Membrane separation technique, such as polysulfones (PSF), cellulose triacetate (CTA), polyvinylidene fluoride (PVDF), cellulose acetate (CA)
Etc. ultrafiltration and microfiltrations film.Unfortunately, most of traditional ultrafiltration and microfiltration films are still arrived by small throughput and easy fouling tendency
Restriction.
Due to overlapping, separation of single fiber etc., the mechanical property for the tunica fibrosa that electrostatic spinning is prepared is poor, limit
Its practical application in water-oil separating is made.In addition to this, the nano fibrous membrane used in harsh environment at present it is long-term
Durability still has very big challenge.Therefore the nano fibrous membrane that electrospinning is prepared needs before being applied to reality into one
The modification of step, to improve its mechanical property and the scope of application.
Summary of the invention
The purpose of this section is to summarize some aspects of the embodiment of the present invention and briefly introduce some preferable implementations
Example.It may do a little simplified or be omitted to avoid our department is made in this section and the description of the application and the title of the invention
Point, the purpose of abstract of description and denomination of invention it is fuzzy, and this simplification or omit and cannot be used for limiting the scope of the invention.
In view of above-mentioned technological deficiency, the present invention is proposed.
Therefore, as one aspect of the present invention, the present invention overcomes the deficiencies in the prior art, provides a kind of super
The preparation method of hydrophobic nanofiber film.
In order to solve the above technical problems, the present invention provides the following technical scheme that a kind of system of super-hydrophobic nano tunica fibrosa
Preparation Method comprising,
Monomer bibenzene tetracarboxylic dianhydride and p-phenylenediamine are dissolved in n,N-Dimethylformamide, synthesis is reacted under low temperature
PAA after PAA nano fibrous membrane is made in PAA by electrostatic spinning, carries out imidization, obtains PI film；
LBL self-assembly is carried out using ferric trichloride and phytic acid and PDMS solution dip-coating is modified obtains described super-hydrophobic receive
Rice tunica fibrosa.
A kind of preferred embodiment of preparation method as super-hydrophobic nano tunica fibrosa of the present invention: anti-under the low temperature
PAA should be synthesized, in -5 DEG C of nitrogen environment, persistently carry out mechanical stirring, to substance in reactor become thick liquid and
There is " rod climbing phenomenon " and terminate reaction afterwards, obtains the PAA.
A kind of preferred embodiment of preparation method as super-hydrophobic nano tunica fibrosa of the present invention: described to pass through electrostatic
PAA nano fibrous membrane is made in PAA by spinning, including, the hexadecyl three of lwt ‰ is added in PAA before electrostatic spinning
First ammonium.
A kind of preferred embodiment of preparation method as super-hydrophobic nano tunica fibrosa of the present invention: described to pass through electrostatic
PAA nano fibrous membrane is made in PAA by spinning, and wherein electrospinning conditions include, the spinning in the high-voltage electrostatic field of 15kV, injection
Device fltting speed is 1.0mL/h, spinning spacing 10cm, drum rotation speed 1500rpm.
A kind of preferred embodiment of preparation method as super-hydrophobic nano tunica fibrosa of the present invention: the carry out imines
Change, for PAA nano fibrous membrane to be placed in tube furnace, is gradually warming up to 350 DEG C of progress imidizations.
A kind of preferred embodiment of preparation method as super-hydrophobic nano tunica fibrosa of the present invention: described to use trichlorine
Change iron and phytic acid carries out LBL self-assembly and the modified water-oil separationg film for obtaining super-hydrophobic super-oleophylic of PDMS solution dip-coating, packet
It includes and the PI film is immersed into FeCl3In solution, positively charged Fe is obtained3+/ PI film.It is more that fiber film surface is removed using distilled water
Remaining FeCl3Solution, by positively charged Fe3+/PI film is immersed in phytic acid, obtains negatively charged PA-Fe3+/ PI film, with steaming
Distilled water cleaning down film to remove extra PA, complete a self assembly circulation, in vacuum drying oven under, solidified and done
It is dry.
A kind of preferred embodiment of preparation method as super-hydrophobic nano tunica fibrosa of the present invention: the tri-chlorination
Iron, concentration 0.01mol/L, the phytic acid, concentration 0.013mol/L.
A kind of preferred embodiment of preparation method as super-hydrophobic nano tunica fibrosa of the present invention: described to use trichlorine
Change iron and phytic acid carries out LBL self-assembly and the modified water-oil separationg film for obtaining super-hydrophobic super-oleophylic of PDMS solution dip-coating, packet
It includes, by PA-Fe after drying3+Solidified in the ethyl acetate solution of/PI film immersion 2wt%PDMS prepolymer, is being dried in vacuo
It is dried in case, obtains the super-hydrophobic nano tunica fibrosa.
As another aspect of the present invention, the present invention overcomes the deficiencies in the prior art, provides described super thin
Super-hydrophobic nano tunica fibrosa made from the preparation method of water nano fibrous membrane.
In order to solve the above technical problems, the present invention provides the following technical scheme that the super-hydrophobic nano tunica fibrosa
Super-hydrophobic nano tunica fibrosa made from preparation method, in which: the separation flow of the super-hydrophobic nano tunica fibrosa is above
7935L·m-2h-1, separative efficiency reaches 99% or more, and hydrophobic angle reaches 150 ° or more.
Beneficial effects of the present invention: the present invention realizes the utilization of LBL self-assembly structure, introduces again on this basis
Silane coupling agent, the two combine, and have obtained the water-oil separationg film with super-hydrophobic super-oleophylic wetability.Shaggy nano junction
Structure, which has, improves water-oil separating performance, this membrane separation efficiency can reach 99% or more, and separation flux is higher than 7935Lm-2·
h-1, hydrophobic angle reaches 150 ° or more, and verified, recyclable reuse.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, required use in being described below to embodiment
Attached drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for this
For the those of ordinary skill of field, without any creative labor, it can also be obtained according to these attached drawings other
Attached drawing.Wherein:
Fig. 1 is building FeCl3The schematic diagram of-PA/PDMSPI nano fibrous membrane.
Fig. 2 is surface topography and element composition figure.(a) SEM image of original PI nano fibrous membrane.(b) five times layer by layer from
PA-Fe after assembling modification3+The SEM image of/PI film.(c) the super-hydrophobic PDMS/PA-Fe after 2wt%PDMS solution modification3+/
The SEM image of PI film.(d)PDMS/PA-Fe3+The EDS spectrogram of/PI nanofiber film surface.
Fig. 3 is phenogram.(a) PI film, PA-Fe3+/ PI film, PDMS/PA-Fe3+The FTIR spectrogram of/PI film.(b) PI film,
PA-Fe3+/ PI film, PDMS/PA-Fe3+The TGA of/PI film schemes.(c) PI film, PA-Fe3+/ PI film, PDMS/PA-Fe3+/ PI film
XPS spectrum figure.(d) PI film, PA-Fe3+/ PI film, PDMS/PA-Fe3+The XRD spectra of/PI film.
Fig. 4 is condition selection figure.(a) the modified PDMS/PA-Fe of various concentration PDMS3+The water contact angle of/PI film.(b)
The PDMS/PA-Fe after different numbers is independently filled layer by layer3+The water contact angle of/PI film.
Fig. 5 is FeCl obtained by the method for the present invention3The grease of-PA/PDMS modified LBL self-assembly structure PI substrate
Separate the test chart of tunica fibrosa contact angle at different conditions.(a) water contact angle test chart in air.(b) organic solvent/salt is molten
The water contact angle test chart of liquid.(c) the water contact angle test chart after ultraviolet irradiation different time.(d) water under different temperatures connects
Feeler test chart.
Fig. 6 is separation process pictorial diagram and evaluation separating effect figure.(a1-a4) photograph of methylene chloride/water separation process
Piece PDMS/PA-Fe3+/ PI nano fibrous membrane.(b) various oil water mixtures pass through PDMS/PA-Fe3+The infiltration of/PI nano fibrous membrane
Saturating flux and separative efficiency.(c) it is recycled 20 times, PDMS/PA-Fe3+The permeation flux and separative efficiency of/PI nano fibrous membrane
Variation.
Specific embodiment
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, right combined with specific embodiments below
A specific embodiment of the invention is described in detail.
In the following description, numerous specific details are set forth in order to facilitate a full understanding of the present invention, but the present invention can be with
Implemented using other than the one described here other way, those skilled in the art can be without prejudice to intension of the present invention
In the case of do similar popularization, therefore the present invention is not limited by the specific embodiments disclosed below.
Secondly, " one embodiment " or " embodiment " referred to herein, which refers to, may be included at least one realization side of the invention
A particular feature, structure, or characteristic in formula." in one embodiment " that different places occur in the present specification not refers both to
The same embodiment, nor the individual or selective embodiment mutually exclusive with other embodiments.
Embodiment 1:
Mechanical agitator, thermometer, N are being housed2In the three neck round bottom for exporting the 100mL of pipe, 0.01mol is added
BPDA and 0.01mol PDA, after evenly mixing.Under conditions of strong mechanical stirring, 40mLDMAc solution is added.Make
It is -5 DEG C with low-temp reaction device control reaction temperature.Then flask is connect with nitrogen cylinder, in N2After being reacted 24 hours under environment,
It was found that occurring rod climbing phenomenon in flask, can reacting exposure, reaction was completed in air, obtains PAA polymer.
The preparation of polyamic acid (PAA) nano fibrous membrane is dissolved into DMAc with by above-mentioned resulting PAA polymer, is obtained
DMAc solution containing 3wt%PAA is added the cetyl trimethylammonium bromide of l ‰ (wt%) to enhance its electric conductivity, is placed on
1h is stirred under magnetic stirring apparatus, obtains uniformly mixed solution.The then spinning in the high-voltage electrostatic field of 15kV, needle point to roller
Distance be about 10cm, collector is the adjustable ground connection flywheel of revolving speed, and revolving speed 1500rpm, the speed of electrospinning is 1.0mL/h.
In N2In the tube furnace of protection, by the good PAA tunica fibrosa imidization of electrospinning, the imidization are as follows: PAA nano fibrous membrane is according to 1
DEG C/heating rate of min is heated to 150 DEG C of heat preservation 1h, 200 DEG C of heat preservation 1h are then heated to, then be warming up to 250 DEG C of heat preservation 1h,
300 DEG C of heat preservation 1h are then raised temperature to, 350 DEG C of heat preservation 0.5h are finally warming up to, imidization obtains polyimide nanofiber membrane (PI
Film) and remove low molecular weight residue therein (water and organic solvent).
Embodiment 2:
(1) PI film (2cm × 2cm) prepared by embodiment 1 is placed in ethyl alcohol and deionized water solution at successively ultrasound
It manages 30min and removes surface impurity.
(2) 2.7029g Iron(III) chloride hexahydrate solid is accurately weighed, with deionized water dissolving, constant volume obtains 0.01mol/L
FeCl3Solution.
(3) the PI film after cleaning is immersed into FeCl32min in solution obtains positively charged Fe3+/ PI film, then with steaming
Distilled water removes the extra FeCl of film surface3。
(4) the positively charged Fe that will be obtained3+/ PI film immerses 2min in 0.013mol/L phytic acid (PA) solution, obtains band
The PA-Fe of negative electrical charge3+Then/PI film removes extra PA solution with distilled water cleaning down film.By it is above-mentioned it is this in a manner of,
A self assembly circulation is completed, and repeats the process to obtain required self assembly cycle-index on PI nano fibrous membrane.
(5) after above-mentioned gained sample is 2 hours dry at 60 DEG C, the acetic acid second containing 2wt%PDMS prepolymer is immersed
Ester solution 2min.Drying 2 hours under vacuum (80 DEG C) are finally placed on, the PDMS/PA- of super-hydrophobicity and super-oleophilic is obtained
Fe3+/ PI film, whole process are as shown in Figure 1.
Embodiment 3:
Using field emission scanning electron microscope (S-4800, Japanese Hitachi electronics corporation), observes embodiment 2 and prepare
Obtained PI film, PA-Fe3+/ PI film, PDMS/PA-Fe3+The configuration of surface of/PI film is clear that the three-dimensional on fiber is more
Pore structure is combined with the protrusion of micro-/ nano scale, forms a kind of and closely similar dual coarse structure of lotus leaf surface.This
The secondary field emission scanning electron microscope utilized has the function of analytical element, is analyzed to identify film surface member by the EDS of outfit
Element, it was demonstrated that membrane modifying success, as shown in Figure 2.
PI film prepared by embodiment 2, PA-Fe are identified using Nicolet 360FT-IR spectrometer respectively3+/ PI film, PDMS/
PA-Fe3+/ PI film functional group and membrane structure property, as shown in Figure 3a.One of adsorption peak of PI fiber is 1771cm-1, can belong to
In the stretching vibration of-CONH functional group, this has turned out PAA fiber imidization success.In addition, 1717cm-1,1356cm-1Place
Adsorption peak respectively corresponds-COOH and C-N functional group, they are all the characteristic peaks of polyimides.By FeCl3With phytic acid processing
Afterwards, in 1652cm-1And 1100cm-1There is new characteristic peak in place, be respectively belonging to P=O functional group stretching vibration and-
HPO43-Characteristic peak.PA-Fe3+After/PI film is immersed in PDMS solution, in 1261cm-1and 810cm-1Place occurs new
Characteristic peak is respectively belonging to Si-CH3The bending vibration of key and the stretching vibration of Si-O-Si key.
Using thermogravimetric analyzer (TGA Q5000-IR), TA company, the U.S. characterizes the thermal stability of film, heating speed
Degree per minute, rises to 800 DEG C of cut-offs from room temperature for 1 DEG C.Curve, which is varied with temperature, from quality knows method therefor system in the present invention
Standby superhydrophobic fibers film has thermal stability, and 500 DEG C or more still keep stable, as shown in Figure 3b.
The fiber shape that embodiment 2 is film-made using X-ray powder diffraction (XRD) (Ultima IV, Rigaku, Japan)
State is studied.All samples all show similar XRD diagram case, are nearby respectively provided with wide diffraction at 18 °, 21 ° and 25 °
Peak.This means that film PDMS/PA-Fe3+The micro/nano structure of/PI film is amorphous, and is remained during surface is modified
Fibre structure, as shown in Figure 3c.
Detect the table that embodiment 2 is film-made respectively using x-ray photoelectron spectroscopy (XPS) (AXIS Ultra DLD, UK)
Face difference element, XPS measuring spectrum show PI film by Elements C1s(285eV), N1s(399eV) and O1s(532eV) composition.Layer by layer
After self assembly, in 745eV (Fe2p) at there is new peak, show N1sSignal strength reduce, it is meant that PI nano fibrous membrane quilt
PA-Fe3+It is completely covered, further modified by PDMS, for new peak present in 100.4eV and 167.7eV, this belongs to hydridization
Track Si2sAnd Si2pCharacteristic, further demonstrate that PDMS is successfully covered on PI nano fibrous membrane, as shown in Figure 3d.
Using contact-angle measurement instrument (JC2000D1), Chinese Shanghai Zhong Chen company, PDMS solution to various concentration and
The modified nano fibrous membrane wettability of the surface of different numbers is independently filled layer by layer to be tested.Film is laid on testboard, is taken the photograph
At camera alignment stage, it is ensured that complete picture can be captured, sample introduction needle is filled into deionized water, every time release 2 microlitres go from
Sub- water, makes drop rest on film surface, artificial to determine drop and film surface point of contact and drop highest using " three-point circle " principle
Point, measuring instrument automatically generate contact angle angle i.e. and can determine the wetability of film surface, and contact angle reaches 153.64 ± 11.6 °, surveys
Test result is as shown in Figure 4.
Embodiment 4:
The environmental resistance for the nano fibrous membrane that for further evaluation prepared by example 2.We select LBL self-assembly 5
Secondary, 2wt%PDMS modified PI nano fibrous membrane makes further research.Using contact-angle measurement instrument (JC2000D1), China
Upper marine occasion company, to the aqueous solution under different pH value, strong acid/base/high concentration salt solutions (CaCl2, KCl, Zn (NO3)2With
MgSO4) in, in organic solvent (n-hexane, acetone, toluene, ether, dimethyl sulfoxide and chloroform), different time of ultraviolet irradiation
PDMS/PA-Fe under lower and different temperatures3+The water contact angle of/PI film is tested, the results showed that the contact angle of film is above
150 °, to confirm that nano fibrous membrane prepared by example 2 has good tolerance, as shown in Figure 5.
Embodiment 5:
Oil water mixture is separated using cylinder type filter, front and back liquid quality is separated by record, calculates and divides
From efficiency and circulation.By the mixed liquor of water and methylene chloride (DCM) (50%v/v, with methyl blue and oil red respectively to water and
DCM dyes in order to observe) it pours into upper tube.It is observed that DCM can infiltrate through film and drop into following beaker.
Meanwhile water is trapped within above film.After separation, almost all of DCM be all collected in lower section, show excellent oil/
Water separable performance energy.Other four kinds of oil water mixtures (chloroform-water, dichloroethanes-water, bromobenzene-water and carbon tetrachloride-water)
It is successfully separated, the separative efficiency of all these products is above 99%.Meanwhile after separating various oil water mixtures, the film exhibition
Reveal good recuperability and durability.Such as after 20 separation, the separation flux and separation effect of DCM- aqueous mixtures
Rate varies less in repetitive process, and separation flux is always above 7935Lm-2·h-1, separative efficiency is above 99%, as schemed
Shown in 6.
The present invention realizes the utilization of LBL self-assembly structure, introduces silane coupling agent, the two knot again on this basis
It closes, has obtained the water-oil separationg film with super-hydrophobic super-oleophylic wetability.Shaggy nanostructure, which has, improves grease
Separating property, this membrane separation efficiency can reach 99% or more, and verified, are recycled and reuse.
It should be noted that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although referring to preferable
Embodiment describes the invention in detail, those skilled in the art should understand that, it can be to technology of the invention
Scheme is modified or replaced equivalently, and without departing from the spirit and scope of the technical solution of the present invention, should all be covered in this hair
In bright scope of the claims.
Claims (9)
1. a kind of preparation method of super-hydrophobic nano tunica fibrosa, it is characterised in that: including,
Monomer bibenzene tetracarboxylic dianhydride and p-phenylenediamine are dissolved in n,N-Dimethylformamide, reaction synthesis PAA, leads under low temperature
It crosses after PAA nano fibrous membrane is made in PAA by electrostatic spinning, carries out imidization, obtain PI film；
The super-hydrophobic nano fibre is obtained using ferric trichloride and phytic acid progress LBL self-assembly and PDMS solution dip-coating are modified
Tie up film.
2. the preparation method of super-hydrophobic nano tunica fibrosa as described in claim 1, it is characterised in that: react and close under the low temperature
At PAA, persistently to carry out mechanical stirring, becoming thick liquid and appearance to substance in reactor in -5 DEG C of nitrogen environment
" rod climbing phenomenon " terminates reaction afterwards, obtains the PAA.
3. the preparation method of super-hydrophobic nano tunica fibrosa as claimed in claim 1 or 2, it is characterised in that: described to pass through electrostatic
PAA nano fibrous membrane is made in PAA by spinning, including, the hexadecyl three of lwt ‰ is added in PAA before electrostatic spinning
First ammonium.
4. the preparation method of super-hydrophobic nano tunica fibrosa as claimed in claim 1 or 2, it is characterised in that: described to pass through electrostatic
PAA nano fibrous membrane is made in PAA by spinning, and wherein electrospinning conditions include, the spinning in the high-voltage electrostatic field of 15kV, injection
Device fltting speed is 1.0mL/h, spinning spacing 10cm, drum rotation speed 1500rpm.
5. the preparation method of super-hydrophobic nano tunica fibrosa as claimed in claim 1 or 2, it is characterised in that: the carry out imines
Change, for PAA nano fibrous membrane to be placed in tube furnace, is gradually warming up to 350 DEG C of progress imidizations.
6. the preparation method of super-hydrophobic nano tunica fibrosa as claimed in claim 1 or 2, it is characterised in that: described to use trichlorine
Change iron and phytic acid carries out LBL self-assembly and the modified water-oil separationg film for obtaining super-hydrophobic super-oleophylic of PDMS solution dip-coating, packet
It includes and the PI film is immersed into FeCl3In solution, positively charged Fe is obtained3+/ PI film.It is more that fiber film surface is removed using distilled water
Remaining FeCl3Solution, by positively charged Fe3+/PI film is immersed in phytic acid, obtains negatively charged PA-Fe3+/ PI film, with steaming
Distilled water cleaning down film to remove extra PA, complete a self assembly circulation, in vacuum drying oven under, solidified and done
It is dry.
7. the preparation method of super-hydrophobic nano tunica fibrosa as claimed in claim 1 or 2, it is characterised in that: the ferric trichloride,
Concentration is 0.01mol/L, the phytic acid, concentration 0.013mol/L.
8. the preparation method of super-hydrophobic nano tunica fibrosa as claimed in claim 6, it is characterised in that: described to use ferric trichloride
LBL self-assembly and the modified water-oil separationg film for obtaining super-hydrophobic super-oleophylic of PDMS solution dip-coating are carried out with phytic acid, including,
By PA-Fe after drying3+Solidified in the ethyl acetate solution of/PI film immersion 2wt%PDMS prepolymer, in a vacuum drying oven
Drying, obtains the super-hydrophobic nano tunica fibrosa.
9. super-hydrophobic nano tunica fibrosa made from the preparation method of any super-hydrophobic nano tunica fibrosa of claim 1~8,
It is characterized by: the separation flow of the super-hydrophobic nano tunica fibrosa is above 7935Lm-2h-1, separative efficiency reaches 99%
More than, hydrophobic angle reaches 150 ° or more.
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