CN105714572B - A method of with coating machine layer assembly modified high-molecular micro/nano-fibre film - Google Patents
A method of with coating machine layer assembly modified high-molecular micro/nano-fibre film Download PDFInfo
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- CN105714572B CN105714572B CN201610242991.3A CN201610242991A CN105714572B CN 105714572 B CN105714572 B CN 105714572B CN 201610242991 A CN201610242991 A CN 201610242991A CN 105714572 B CN105714572 B CN 105714572B
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
- D06N3/0015—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using fibres of specified chemical or physical nature, e.g. natural silk
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
- D06N3/0011—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using non-woven fabrics
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0086—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the application technique
- D06N3/0088—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the application technique by directly applying the resin
- D06N3/009—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the application technique by directly applying the resin by spraying components on the web
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N2201/00—Chemical constitution of the fibres, threads or yarns
- D06N2201/04—Vegetal fibres
- D06N2201/042—Cellulose fibres, e.g. cotton
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N2203/00—Macromolecular materials of the coating layers
- D06N2203/02—Natural macromolecular compounds or derivatives thereof
- D06N2203/024—Polysaccharides or derivatives thereof
Abstract
The invention discloses a kind of methods with coating machine layer assembly modified high-molecular micro/nano-fibre film, belong to field of material technology.The method of the present invention includes the following steps: to be coated with one layer of coating material solution using macromolecule micro/nano-fibre film as by painting substrate with coating machine, be dried under vacuum to solvent and volatilize completely, so far to assemble 1 bilayer；Repetitive operation can get the composite micro/nano tunica fibrosa that the double-deck number is the required number of plies.The present invention is using micro/nano-fibre film as by painting substrate, it is modified that layer assembly is carried out to micro/nano-fibre film surface using coating machine, there is no any restrictions to coating material, all synthesis macromolecules that can be dispersed or dissolved in solvent, natural polymer, micro-/ nano particle can be modified through the invention in micro/nano-fibre film surface, the micro/nano-fibre film of functionalization required for preparing.Present invention process is simple, cost of material is low, mild condition, widely applicable etc., is suitable for industrial production.
Description
Technical field
The invention belongs to field of material technology, and in particular to a kind of to use coating machine layer assembly modified high-molecular micro-/ nano
The method of tunica fibrosa.
Background technique
By development in more than 20 years, layer assembly had become a kind of relatively mature skill for preparing multilayer film
Art.Due to its with it is easy to operate, low in cost, almost can be deposited in any substrate, strong applicability and composition and knot
Structure is easy the advantages that regulation and is widely studied, and becomes the most promising preparation for constructing functional membrane material
One of technology.The film forming matter of laminated assembling technology is abundant, including polyelectrolyte, organic and inorganic particles, large biological molecule with
And numerous substances including small organic molecule, oligomer, dendrimer with few charge etc. can be used as and construct primitive
Prepare layer assembly multilayer film.
Traditional layer assembly is widely used as constructing for ultrathin membrane of the thickness less than 100nm.Compared with ultrathin membrane, micron
It is easier to realize high load, the regulation of micro-/ nano composite construction, multifunctional unit with the thick film of sub-micron and assigns film more
High stability.Although scientists based on traditional layer assembly, have developed the quick structure of several layer assembly films
The deriving method built, including by spin coating-layer assembly in conjunction with layer assembly of spin coating, spraying and spraying-laminated assembling technology
And the layer assembly method of the exponential increase based on weak polyelectrolyte, but the functionalization of thick film does not still cause people enough
Attention.Meanwhile the functionalization of thick film still needs to develop the quick constructing method of new layer assembly film.Coating is by one layer or more
There is layer the material of specific function to be attached on substrate surface, and the thickness of coating can be differed from nanoscale to micron order, to change
Kind substrate surface performance or protection substrate assign substrate specific function or directly improve making for product using coating surface characteristic
With value.Coating arts techniques are used for photosensitive industry, paper conversion industry and the fields such as plastics package engineering earliest, at present due to
Coating technique is fast-growth, at low cost and used by various production procedures, and substrate to be coated is also from paper, all kinds of macromolecules
Film expands to aluminium foil, copper foil or even steel plate.
In micro/nano material field, not yet there is the side using the modified micro/nano-fibre film of coating machine layer assembly
Method.
Chinese patent " utilizing polymer fixed ion liquid " (publication number CN1746196) discloses a kind of utilize and polymerize
The method of object fixed ion liquid.The carrier for utilizing polymers as ionic liquid transfers ionic liquid by amidation process
It is connected on the side chain of polymer；Then by its by the methods of spin coating, layer assembly or electrophoretic deposition be fixed to metal, glass,
On the solid matrixs such as silicon or on metal, semi-conductor nano particles, it can also be fixed on the electrodes such as gold, platinum or glass carbon.This method
Be with difference of the invention, selected matrix is different, what this method was selected be solid matrix, metal semiconductor nanoparticle or
Electrode, and matrix selected by the present invention is micro/nano-fibre film.
Chinese patent " preparation method based on layer assembly hollow multilayer Nano capsule self-healing film " (publication number
CN103755156A a kind of preparation method based on layer assembly hollow multilayer Nano capsule self-healing film) is disclosed.Specifically
Method is as follows: substrate being submerged initially in 15mim in the PEI solution with its oppositely charged, uses distilled water flushing after taking out substrate
Repeatedly be dipped in 15mim in PAA solution again, repeatedly 4 times substrate surface assemble multi-layer polyelectrolyte film, then in multilayer
One layer of hollow microcapsule (revolving speed 5000rad/min) of spin coating on polyelectrolyte film repeats the above process repeatedly thus in obtaining
Empty multi-layer nano capsule self-healing film.It being different from the present invention, selected substrate is glass or silicon wafer in the patent,
And be coated on polyelectrolyte film, it is not on micro/nano-fibre film.
A kind of Chinese patent " preparation method of the self-supporting polymer film of unidirectional drug delivery " (publication number
CN103611194A it) discloses using in polylactic acid-glycollic acid block copolymer (PLGA) interlayer between barrier layer and coating
The method of polyelectrolyte composite layer containing drug be prepared for it is a kind of for unidirectional drug delivery have preferable mechanical strength and
The self-supporting polymer film of flexibility.Equally, although the invention is utilized the method layer assembly of coating, but substrate and this hair
Micro/nano-fibre film in bright is significantly different.
A kind of Chinese patent " LBL self-assembly modified cellulose nanofiber film and its system based on lysozyme and silk-fibroin
It is standby with application " (publication number CN103536958A) disclose it is a kind of modified fine based on the LBL self-assembly of lysozyme and silk-fibroin
Tie up plain nano fibrous membrane and its preparation and application.Although being to be modified on nano fibrous membrane in the invention, not
It is modified to use coating machine layer assembly, there is also a great differences with the present invention.
Document " Nanofibrous mats layer-by-layer assembled via electrospun
The side of EFI is utilized in cellulose acetate and electrosprayed chitosan for cell culture "
It is modified that method carries out LBL self-assembly on acetate fiber nano fibrous membrane, exist from the present invention it is different, this method by EFI with it is electric
Spinning technique combines, and alternately, preferably completes deposition of the chitosan on nano fibrous membrane.The shell that this method is deposited is poly-
Sugar is Nano grade, and negligible amounts, and coating method used in the present invention can reach micron even sub-micron, preferably realize
The fixation of chitosan.For the present invention compared with this method, process is simpler, and time-consuming shorter, effect obtained is also suitable.
Summary of the invention
It is an object of that present invention to provide a kind of methods with coating machine layer assembly modified high-molecular micro/nano-fibre film.
This method can carry out that layer assembly is modified to all macromolecule micro/nano-fibre films, functionalization required for preparing it is micro-/
Nano fibrous membrane.
The purpose of the invention is achieved by the following technical solution:
A method of with coating machine layer assembly modified high-molecular micro/nano-fibre film, include the following steps: with high score
Sub- micro/nano-fibre film is used as by painting substrate, is coated with one layer of coating material solution with coating machine, is dried under vacuum to solvent and waves completely
Hair, so far to assemble 1 bilayer；Repetitive operation can get the composite micro/nano tunica fibrosa that the double-deck number is the required number of plies.It is double-deck
Number is at least 1 layer, does not set the upper limit.
The preparation method of the macromolecule micro/nano-fibre film include but is not limited to wet spinning process, method of electrostatic spinning,
Pulling method, template synthesis method, phase separation method, self-assembly method, the spinning of molecule spinneret, confinement synthetic method, fabric of island-in-sea type bi-component are multiple
Close spin processes and molecular engineering the preparation method and biological the preparation method etc..
The component of the macromolecule micro/nano-fibre film is unlimited, can be one or more, including synthesis macromolecule
And natural polymer, such as polyacrylonitrile, cellulose acetate, fibroin albumen, collagen, polylactic acid, according to methacrylate,
Polyoxyethylene, polyaniline, polystyrene, polyvinylpyrrolidone etc..
The type of the coating machine is unlimited, and the method for coating is also unlimited, including the coating of pressure roller class, scraper class are coated with, squeeze
Coating, curtain coating, rotary coating and spraying coating etc. out.
The coating material can be one or more, including all can be dispersed or dissolved in water or organic molten
Synthesis macromolecule, natural polymer and micro-/ nano particle in agent.
Below by taking cellulose acetate micro/nano-fibre film (substrate) and chitosan (coating material) as an example, illustrate with coating
The method of machine layer assembly modified high-molecular micro/nano-fibre film, includes the following steps:
(1) cellulose acetate is dissolved in acetone and the mixed solution of dimethyl acetamide, it is molten obtains cellulose acetate
Liquid；Then cellulose acetate micro/nano-fibre film is prepared by electrostatic spinning technique.
(2) Chitosan powder is added in acetic acid solution and prepares chitosan solution.
(3) it is coated with one layer of chitosan solution on dried cellulose acetate micro/nano-fibre film using coating machine, puts
Enter in vacuum oven drying to volatilize completely to solvent, so far to assemble 1 bilayer；It is institute that repetitive operation, which can get the double-deck number,
Need the composite micro/nano tunica fibrosa of the number of plies.
Preferably, the above method includes the following steps:
(1) cellulose acetate is dissolved in acetone and the mixed solution of dimethyl acetamide (mass ratio 2:1), is obtained
The cellulose acetate solution of 16wt%.Then cellulose acetate micro/nano-fibre film, parameter packet are prepared by electrostatic spinning technique
Include: temperature and relative humidity are respectively 25 DEG C and 50%, and for electrostatic spinning voltage between 1-16kV, solution flow velocity is 1mL/h, are connect
Receiving distance is 15cm.Then resulting cellulose acetate micro/nano-fibre film is dried in vacuo at 60 DEG C, so that solvent is abundant
Volatilization.
(2) Chitosan powder is added in the acetic acid solution of 0.5wt%, it is molten is configured to the chitosan that mass fraction is 3%
Liquid.
(3) a layer thickness is coated on the resulting cellulose acetate micro/nano-fibre film of step (1) using coating machine is 1-
Then obtained composite membrane is put into 60 DEG C of vacuum ovens dryings and volatilizees completely to solvent by 1000 μm of chitosan solution,
It so far is to assemble 1 bilayer；Repetitive operation can get the composite micro/nano tunica fibrosa that the double-deck number is the required number of plies.
The present invention for the first time using micro/nano-fibre film as by painting substrate, using coating machine to micro/nano-fibre film surface into
Row layer assembly is modified, does not have any restrictions, all synthesis high scores that can be dispersed or dissolved in solvent to coating material
Son, natural polymer, micro-/ nano particle can be modified through the invention in micro/nano-fibre film surface, prepare institute
The micro/nano-fibre film of the functionalization needed.The present invention has many advantages, such as, including simple process, cost of material are low, condition temperature
With it is widely applicable etc., be suitable for industrial production, and at home and abroad all still belong to the first time.
Detailed description of the invention
Fig. 1 is that the chitosan/acetic acid cellulose composite micro/nano tunica fibrosa that the double-deck number prepared by embodiment 1 is 1.5 is cut
Surface scan electron microscope.
Fig. 2 is the shape appearance figure of the cellulose acetate micro/nano-fibre film of the preparation of embodiment 1, composite micro/nano tunica fibrosa.a
It is cellulose acetate micro/nano-fibre film surface scanning electron microscope (SEM) photograph, b is that the chitosan/acetic acid cellulose that the double-deck number is 2 is compound
Micro/nano-fibre film surface scanning electron microscope (SEM) photograph.
Fig. 3 be embodiment 1 with composite micro/nano tunica fibrosa prepared by comparative example 1 to the antibacterial of staphylococcus aureus
Effect diagram.
Fig. 4 is the shape appearance figure of the polycaprolactone micro/nano-fibre film of the preparation of embodiment 3, composite micro/nano tunica fibrosa.A is
Polycaprolactone micro/nano-fibre film surface scanning electron microscope (SEM) photograph, b are that the sodium alginate/bovine serum albumin/that the double-deck number is 4 gathers in oneself
Ester composite micro/nano tunica fibrosa surface scan electron microscope.
Fig. 5 is the shape appearance figure of the polystyrene micro/nano-fibre film of the preparation of embodiment 4, composite micro/nano tunica fibrosa.A is
Polystyrene micro/nano-fibre film surface scanning electron microscope (SEM) photograph, b are poly-N-vinyl pyrrolidones/polyphenyl second that the double-deck number is 4
Alkene composite micro/nano tunica fibrosa surface scan electron microscope.
Specific embodiment
Below by specific embodiment, technical scheme is described further, and its object is to help preferably
Understand the contents of the present invention, but these specific embodiments are not in any way limit the scope of the present invention.
Embodiment 1
(1) prepare cellulose acetate micro/nano-fibre film using electrostatic spinning technique: cellulose acetate be dissolved in acetone and
In the mixed solution of dimethyl acetamide (mass ratio 2:1), the cellulose acetate solution of 16wt% is obtained.Then pass through Static Spinning
Silk technology prepares cellulose acetate micro/nano-fibre film, and parameter includes: temperature and relative humidity is respectively 25 DEG C and 50%, electrostatic
Spinning voltage is 16kV, and solution flow velocity is 1mL/h, and receiving distance is 15cm.It is then that resulting cellulose acetate micro-/ nano is fine
Dimension film is dried in vacuo at 60 DEG C, so that solvent sufficiently volatilizees, it is at this time 0.5 bilayer.
(2) Chitosan powder is dissolved in the acetic acid solution of 0.5wt%, is slowly stirred at room temperature for 24 hours, obtains quality point
The chitosan solution that number is 3%.
(3) the cellulose acetate micro/nano-fibre film after drying is paved on coating machine, the thickness of adjustment coating machine coating
Degree is 10 μm, speed 50mm/s, and chitosan solution is coated on cellulose acetate micro/nano-fibre film, obtained chitosan/
Cellulose acetate composite micro/nano tunica fibrosa, 60 DEG C of 12 hours (solvent are made to volatilize completely) of vacuum drying obtain 1 pair since then
Layer.Continue Static Spinning cellulose acetate deposition on the duplicature, after vacuum drying, that is, obtains 1.5 bilayers；Then it applies
Cloth chitosan solution after vacuum drying, that is, obtains 2 bilayers.It repeats electrospinning cellulose acetate and is coated with the operation of chitosan, it can
Obtaining the double-deck number is required number of plies composite micro/nano tunica fibrosa.
The pattern of gained composite micro/nano tunica fibrosa is shown in that Fig. 1,2, Fig. 1 are chitosan/vinegar that the double-deck number prepared is 1.5
Acid cellulose composite micro/nano tunica fibrosa cross-sectional scans electron microscope.Fig. 2-a is cellulose acetate micro/nano-fibre, and Fig. 2-b is
The chitosan/acetic acid cellulose composite micro/nano tunica fibrosa that the double-deck number is 2.The composite Nano for being 5 by the obtained double-deck number is fine
Film is tieed up for the bacteriostatic experiment to staphylococcus aureus, fungistatic effect such as Fig. 3.
Comparative example 1
The chitosan solution of cellulose acetate micro/nano-fibre film and 3% is prepared according to the method in embodiment 1.
The chitosan solution that mass fraction is 3% is sprayed on dried cellulose acetate micro-/ nano using the method for EFI
On tunica fibrosa, the EFI time is 4 hours, voltage 20kV；Then to get to 1 bilayer after being dried in vacuo 48 hours；In this pair
Continue Static Spinning cellulose acetate deposition on tunic, after vacuum drying, that is, obtains 1.5 bilayers；Then EFI chitosan
Solution after vacuum drying, that is, obtains 2 bilayers.The operation of electrospinning cellulose acetate and EFI chitosan is repeated, can get double points
Sublayer number is the chitosan/acetic acid cellulose composite micro-nano rice tunica fibrosa of the required number of plies.By the obtained double-deck number be 5 it is compound
Nano fibrous membrane is used for the bacteriostatic experiment to staphylococcus aureus, fungistatic effect such as Fig. 3.
As shown, sample obtained by embodiment 1 and comparative example 1 has certain inhibition to make staphylococcus aureus
With wherein the average diameter of inhibition zone of embodiment 1 is 13.7mm, and the average diameter of inhibition zone of comparative example 1 is 11.3mm, this explanation
The fungistatic effect of the modified composite nano-fiber membrane obtained of layer assembly is more preferable by the method for the invention.The main reason is that right
The chitosan that the method for ratio 1 is deposited is Nano grade, negligible amounts；And embodiment 1 passes through coating method Dichlorodiphenyl Acetate fiber
Plain micro/nano-fibre film carries out layer assembly and is modified, and the amount for the chitosan fixed is more, can reach micron even sub-micron.
In addition, compared with Example 1, taking a long time in comparative example 1, technique is simple and convenient not as good as embodiment 1.
Embodiment 2
(1) cellulose acetate micro/nano-fibre film is prepared using electrostatic spinning technique: cellulose acetate is dissolved in acetone
In the mixed solution of dimethyl acetamide (mass ratio 2:1), the cellulose acetate solution of 16wt% is obtained.Then pass through electrostatic
Spining technology prepares cellulose acetate micro/nano-fibre film, and parameter includes: temperature and relative humidity is respectively 25 DEG C and 50%, quiet
Electrospinning filament voltage is 16kV, and solution flow velocity is 1mL/h, and receiving distance is 15cm.Then by resulting cellulose acetate it is micro-/receive
Rice tunica fibrosa is dried in vacuo at 60 DEG C, so that solvent sufficiently volatilizees.
Cellulose acetate micro/nano-fibre film after drying is placed in 0.05mol/L sodium hydroxide solution and hydrolyzes 7d, room
Temperature is dried, i.e. acquisition cellulose micro/nano-fibre bottom plate.
(2) chitosan is made into the solution of 1mg/L using the acetic acid solution of 0.002mol/L as solvent, fibroin albumen is made into
The aqueous solution of 1mg/L.
(3) the cellulose micro/nano-fibre film after drying being laid on coating machine, adjustment coating speed is 200mm/s,
Coating thickness is 1 μm, using cellulose micro/nano-fibre film as bottom plate, is coated with chitosan solution, after vacuum drying removes solvent,
Obtain 0.5 bilayer；It is coated with silk fibroin protein solution, after vacuum drying removes solvent, that is, obtains 1 bilayer.On the bilayer
Continue to be coated with chitosan solution, after vacuum drying, that is, obtains 1.5 bilayers；Then it is coated with silk fibroin protein solution, is dried in vacuo
Afterwards, that is, 2 bilayers are obtained.Alternately coating chitosan solution and silk fibroin protein solution are repeated, can get bilayer number is the required number of plies
Chitosan/fibroin albumen/cellulose composite micro/nano tunica fibrosa.
Embodiment 3
(1) polycaprolactone micro/nano-fibre film is prepared using electrostatic spinning technique: 8g polycaprolactone being taken to be dissolved into 92g third
In ketone, it is configured to the polycaprolactone solution that mass fraction is 8%.Then polycaprolactone micro-/ nano is prepared by electrostatic spinning technique
Tunica fibrosa, parameter includes: temperature and relative humidity is respectively 25 DEG C and 40%, and electrostatic spinning voltage is between 15kV, solution flow velocity
For 1mL/h, receiving distance is 12cm.Then resulting polycaprolactone micro/nano-fibre film is dried in vacuo at 60 DEG C, so that
Solvent sufficiently volatilizees, and is so far 0.5 bilayer.
(2) sodium alginate and bovine serum albumin are the ratio mixing of 1:1 in mass ratio, are dissolved in water, being made into solute is
3wt%(, that is, sodium alginate and each sodium alginate/bovine serum albumen solution 3%) of bovine serum albumin.
(3) the polycaprolactone micro/nano-fibre film after drying is laid on coating machine, the thickness of adjustment coating machine coating
It is 1 μm, speed 100mm/s, sodium alginate/bovine serum albumen solution is coated on polycaprolactone micro/nano-fibre film, is obtained
To sodium alginate/bovine serum albumin/polycaprolactone composite micro/nano tunica fibrosa, it is dried in vacuo 12 hours, obtains 1 pair since then
Layer.On the bilayer, continues electrospinning polycaprolactone micro/nano-fibre deposition and obtained after vacuum drying removes solvent
1.5 bilayers；Then it is coated with sodium alginate/bovine serum albumen solution, after vacuum drying removes solvent, that is, obtains 2 bilayers.Weight
Multiple operation can get the composite micro/nano tunica fibrosa that the double-deck number is the required number of plies.
Pattern such as Fig. 4, Fig. 4-a polycaprolactone micro/nano-fibre of gained composite micro/nano tunica fibrosa, Fig. 4-b are double-deck
Sodium alginate/bovine serum albumin/polycaprolactone composite micro/nano tunica fibrosa that number is 4.
Embodiment 4
(1) polyethylene micro/nano-fibre film is prepared using electrostatic spinning technique: polyethylene being taken to be dissolved into dimethylformamide
In the mixed solution of tetrahydrofuran (mass ratio 4:6), it is configured to the polyethylene solution that mass fraction is 16%；Then by quiet
Electrospinning prepares polystyrene micro/nano-fibre film, and parameter includes: temperature and relative humidity is respectively 25 DEG C and 40%, quiet
For electrospinning filament voltage between 15-20kV, solution flow velocity is 1mL/h, and receiving distance is 10cm.Then by resulting polystyrene
Micro/nano-fibre film is dried in vacuo at 60 DEG C, so that solvent sufficiently volatilizees, it is so far 0.5 bilayer.
(2) poly-N-vinyl pyrrolidones is taken water as a solvent to the solution for being made into 8wt%.
(3) the polystyrene micro/nano-fibre film after drying is laid on coating machine, the thickness of adjustment coating machine coating
It is 1 μm, speed 100mm/s, poly-N-vinyl pyrrolidone solution is coated on polystyrene micro/nano-fibre film, is obtained
To poly-N-vinyl pyrrolidones/polystyrene composite micro/nano tunica fibrosa, it is dried in vacuo 12 hours, obtains 1 pair since then
Layer.On the bilayer, continues electrospinning polystyrene micro/nano-fibre deposition and obtained after vacuum drying removes solvent
1.5 bilayers；Then it is coated with poly-N-vinyl pyrrolidone solution, after vacuum drying removes solvent, that is, obtains 2 bilayers.Weight
Multiple operation can get the composite micro/nano tunica fibrosa that the double-deck number is the required number of plies.
Pattern such as Fig. 5, Fig. 5-a of gained composite micro/nano tunica fibrosa are polystyrene micro/nano-fibres, and Fig. 5-b is double
Poly-N-vinyl pyrrolidones/polystyrene composite micro/nano tunica fibrosa that the number of plies is 4.
Embodiment 5
(1) polyacrylonitrile micro/nano-fibre film is prepared using electrostatic spinning technique: polyacrylonitrile is dissolved in tetrahydrofuran
In, obtain the polyacrylonitrile solution of 15wt%.Then polyacrylonitrile micro/nano-fibre film, parameter are prepared by electrostatic spinning technique
Include: temperature and relative humidity is respectively 25 DEG C and 50%, electrostatic spinning voltage is 20kV, and solution flow velocity is 1mL/h, receive away from
From for 15cm.Then resulting polyacrylonitrile micro/nano-fibre film is dried in vacuo at 60 DEG C, so that solvent sufficiently volatilizees.
(2) titanium dioxide is poured into water, and is handled 15 minutes by cell pulverization instrument, enable titanium dioxide uniform
Ground is dispersed in solvent, and polyvinyl alcohol is then added, and is slowly stirred at room temperature for 24 hours, and the final total concentration of solutes that obtains is 5wt%'s
Titanium dioxide/polyvinyl alcohol (w/w, 3:5) aqueous solution.
(3) the polyacrylonitrile micro/nano-fibre film after drying is laid on coating machine, the thickness of adjustment coating machine coating
It is 3 μm, speed 50mm/s, titanium dioxide/poly-vinyl alcohol solution is coated on polyacrylonitrile micro/nano-fibre film, is obtained
Composite micro/nano tunica fibrosa is dried in vacuo 12 hours, obtains 1 bilayer since then.On the bilayer, continue electrospinning poly- third
Alkene nitrile micro/nano-fibre deposition after vacuum drying removes solvent, that is, obtains 1.5 bilayers；Then it is coated with titanium dioxide/poly- second
Enolate solution after vacuum drying removes solvent, that is, obtains 2 bilayers.Repetitive operation can get the double-deck number be the required number of plies it is micro-/
Composite nano-fiber membrane.The composite micro/nano tunica fibrosa of acquisition is impregnated into 72 hours removal polyvinyl alcohol in water, is after dry
It can get titanium dioxide/polyacrylonitrile composite micro/nano tunica fibrosa.
Claims (6)
1. a kind of method with coating machine layer assembly modified high-molecular micro/nano-fibre film, it is characterised in that including walking as follows
It is rapid: using macromolecule micro/nano-fibre film as by painting substrate, to be coated with one layer of coating material solution with coating machine, be dried under vacuum to
Solvent volatilizees completely, so far to assemble 1 bilayer；Repetitive operation can get the composite micro/nano that the double-deck number is the required number of plies
Tunica fibrosa；
The coating method is that blade coating or pressure roller are coated with；
The coating material is synthesis macromolecule or natural polymer.
2. according to the method described in claim 1, it is characterized by: the group of the macromolecule micro/nano-fibre film is divided into one
Kind is a variety of.
3. according to the method described in claim 1, it is characterized by: the macromolecule includes synthesis macromolecule and natural polymer
Son.
4. according to the method described in claim 1, it is characterized by: the coating material solution is a kind of the molten of coating material
The solution of liquid or a variety of coating materials.
5. according to the method described in claim 1, it is characterized by: the coating material further includes micro-/ nano particle.
6. according to the method described in claim 1, it is characterized by: substrate is cellulose acetate micro/nano-fibre film, coating material
When material is chitosan, include the following steps:
(1) cellulose acetate is dissolved in acetone and the mixed solution of dimethyl acetamide, obtains cellulose acetate solution；So
Cellulose acetate micro/nano-fibre film is prepared by electrostatic spinning technique afterwards, is at this time 0.5 bilayer；
(2) Chitosan powder is added in acetic acid solution and prepares chitosan solution；
(3) it is coated with one layer of chitosan solution on dried cellulose acetate micro/nano-fibre film using coating machine, is put into true
Drying is volatilized completely to solvent in empty drying box, so far to assemble 1 bilayer；It is required layer that repetitive operation, which can get the double-deck number,
Several composite micro/nano tunica fibrosas.
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| CN103755156A (en) * | 2014-01-14 | 2014-04-30 | 东南大学 | Preparation method of self-healing thin film of hollow multi-layered nano capsule based on layer by layer assembly |
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| CN103755156A (en) * | 2014-01-14 | 2014-04-30 | 东南大学 | Preparation method of self-healing thin film of hollow multi-layered nano capsule based on layer by layer assembly |
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