CN112267300A - Electrostatic spinning fiber-based ultrathin continuous nano spider web fiber material and preparation method thereof - Google Patents
Electrostatic spinning fiber-based ultrathin continuous nano spider web fiber material and preparation method thereof Download PDFInfo
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- 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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- 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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- 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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- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
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- 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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- 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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- D06N3/0043—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by their foraminous structure; Characteristics of the foamed layer or of cellular layers
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- D06N3/0056—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the compounding ingredients of the macro-molecular coating
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- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
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Abstract
The invention relates to an electrostatic spinning fiber-based ultrathin continuous nano-spider web fiber material and a preparation method thereof, which comprises the steps of firstly adding a surfactant into a polymer solution to obtain a mixed solution, then coating the mixed solution on the surface of an electrostatic spinning fiber substrate and spreading the mixed solution to form an ultrathin continuous liquid film, and finally preparing the electrostatic spinning fiber-based ultrathin continuous nano-spider web fiber material which takes electrostatic spinning fibers as the substrate and is covered with an ultrathin continuous nano-spider web structure on the surface layer through non-solvent induced phase separation; the surface tension of the mixed solution is less than or equal to the surface tension of the electrostatic spinning fiber base material; the cobweb in the prepared electrostatic spinning fiber-based ultrathin continuous nano cobweb fiber material is of a uniform continuous net-shaped structure, the average fiber diameter is 20-70 nm, the mesh aperture is 10-500 nm, the porosity is more than or equal to 85%, and the cobweb thickness is 20-70 nm. The method is simple and easy to implement, the prepared product has smaller pore size and more uniform pore size distribution, and the filtering precision of the material can be obviously improved.
Description
Technical Field
The invention belongs to the technical field of fiber materials, and relates to an electrostatic spinning fiber-based ultrathin continuous nano-spider web fiber material and a preparation method thereof.
Background
The electrostatic spinning nanofiber has the advantages of high porosity, good pore canal connectivity and the like, so the electrostatic spinning nanofiber has wide application prospect in the field of filtration and separation. However, the diameter of the conventional electrostatic spinning nano-fiber is more than 100nm at present, so that the aperture of the aggregate is larger than 1 μm, and the high-precision filtration of the pollutants of submicron order is difficult to realize. A method for preparing a functional layer by coating a polymer solution or a mixture of the polymer solution and a nano filler on the surface of electrospun fiber to further reduce the pore diameter of an electrospun nanofiber membrane is reported in the prior patent (CN 201610528343.4; PCT/US 2005/035738). although the pore diameter of the nanofiber membrane can be effectively reduced by the functional layer prepared by the method, the thickness of the functional layer is more than 200nm and the structure is compact, the original high porosity and good pore channel connectivity of the fiber membrane are damaged, and the permeability of the material is sharply reduced.
In the open literature [ Ultrathin Cellulose Voronoi-Nanonet Membranes Enable High-Flux and Energy-Saving Water Purification, ACS appl.Mater.Interfaces 2020,12,28, 31852-31862 ] the solution is coated on the surface of the electrospun nanofiber membrane and a nano-spider-web structure is constructed by a non-solvent induced phase separation technology, and the spider-web structure can effectively maintain the porosity and pore channel connectivity of the electrospun nanofiber material, but the method can not form a uniform and continuous mesh structure and seriously limits the further improvement of the filtration precision.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides an electrostatic spinning fiber-based ultrathin continuous nano-spider web fiber material and a preparation method thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for preparing electrostatic spinning fiber-based ultrathin continuous nano-cobweb fiber material comprises the steps of firstly adding a surfactant into a polymer solution to obtain a solution, then coating the mixed solution on the surface of an electrostatic spinning fiber substrate and spreading the solution to form an ultrathin continuous liquid film, and finally preparing the electrostatic spinning fiber-based ultrathin continuous nano-cobweb fiber material which takes electrostatic spinning fibers as the substrate and is covered with an ultrathin continuous nano-cobweb structure on the surface layer through non-solvent induced phase separation, wherein the electrostatic spinning fiber-based ultrathin continuous nano-cobweb fiber material prepared by the invention is internally provided with an electrostatic spinning fiber substrate, and the surface of the electrostatic spinning fiber-based ultrathin continuous nano-cobweb fiber material is in a uniform and continuous ultrathin cobweb structure form;
the reason why the invention takes the electrostatic spinning fiber membrane as the base material is that: (1) the high porosity and the communicated pore structure of the electrostatic spinning fiber membrane are beneficial to mutual diffusion of a solvent and a non-solvent in the phase separation process; (2) the pore size of the electrostatic spinning substrate is in submicron order, thus effectively preventing the solution from permeating, and being beneficial to forming a film on the surface layer of the solution, if the material with larger pore size, such as melt-blown or spun-bonded non-woven fabric, is taken as the substrate, the dilute solution coated on the surface can easily permeate into the material; (3) the electrospun fiber substrate can play a role in supporting the ultrathin cobweb;
the surface tension of the polymer solution is greater than that of the electrostatic spinning fiber base material, and the surface tension of the mixed solution is less than or equal to that of the electrostatic spinning fiber base material;
the polymer is polyacrylonitrile, polyvinylidene fluoride, polyurethane, polyisophthaloyl metaphenylene diamine, polyetherimide, polyethersulfone, cellulose acetate, nitrocellulose or cellulose, the electrostatic spinning fiber substrate is an electrostatic spinning nano-fiber membrane, and the preparation of the electrostatic spinning nano-fiber membrane is a known technology;
the cobweb thickness of the electrospun fiber-based ultrathin continuous nano cobweb fiber material is 20-70 nm.
As a preferred technical scheme:
according to the preparation method of the electrostatic spinning fiber-based ultrathin continuous nano-cobweb fiber material, the surfactant is polyoxyethylene sorbitan monooleate, polyoxyethylene sorbitan monostearate, polyoxyethylene sorbitan monopalmitate, dodecyl trimethyl ammonium bromide, hexadecyl trimethyl ammonium bromide, octadecyl dimethyl benzyl ammonium chloride, tetrabutyl ammonium chloride, sodium dodecyl benzene sulfonate or sodium dodecyl sulfate, the surfactant disclosed by the invention comprises the above types, and other surfactants capable of being dissolved in corresponding solvents are also suitable for the invention; the addition amount of the surfactant is 0.0002-2 wt% of the polymer solution.
The weight-average molecular weight of the polymer is 5 multiplied by 104～100×104g/mol, the concentration of the polymer in the mixed solution is 0.001-5 wt%, and the viscosity of the mixed solution is 50-1000 mPas.
In the method for preparing the electrostatic spinning fiber-based ultrathin continuous nano-spider web fiber material, the solvent of the polymer solution is more than one of N, N-dimethylacetamide, N-dimethylformamide, N-methylpyrrolidone, dimethyl sulfoxide, N-methylmorpholine-N-oxide and acetone.
The method for preparing the electrostatic spinning fiber-based ultrathin continuous nano-spider web fiber material comprises the step of preparing the electrostatic spinning fiber substrate from a polyamide electrostatic spinning nanofiber membrane, a polytetrafluoroethylene electrostatic spinning nanofiber membrane, a polypropylene electrostatic spinning nanofiber membrane, a polyethylene terephthalate electrostatic spinning nanofiber membrane, a cellulose electrostatic spinning nanofiber membrane, an electrostatic spinning carbon nanofiber membrane or SiO2Electrospun nanofiber membranes.
The method for preparing the electrostatic spinning fiber-based ultrathin continuous nano-cobweb fiber material comprises the steps of enabling the surface tension of an electrostatic spinning fiber base material to be 22-47 mN/m (when the selected electrostatic spinning base material is a polyamide electrostatic spinning nano-fiber film, the surface tension is 33 mN/m; when the electrostatic spinning base material is a polytetrafluoroethylene electrostatic spinning base material, the surface tension is 22 mN/m; when the electrostatic spinning base material is a polypropylene electrostatic spinning nano-fiber film, the surface tension is 31 mN/m; when the electrostatic spinning base material is a polyethylene glycol terephthalate electrostatic spinning nano-fiber film, the surface tension is 41 mN/m; when the electrostatic spinning base material is a cellulose electrostatic spinning nano-fiber film, the surface tension is 44 mN/m; when the electrostatic spinning base material is an electrostatic spinning carbon nano-fiber film, the surface tension is 36 mN/m; and the electrostatic spinning base material is SiO2When the nanofiber membrane is electrostatically spun, the surface tension is 47mN/m), and the surface tension of the polymer solution after the surfactant is added is 15-45 mN/m; the coating amount of the mixed solution on the surface of the electrostatic spinning fiber substrate is 3-15 ul cm-2。
In the method for preparing the electrospun fiber-based ultrathin continuous nano-spider web fiber material, the non-solvent used for inducing phase separation (the non-solvent is mutually miscible with the solvent used for the polymer solution but can not dissolve the polymer) is more than one of water, methanol, ethanol, propanol, isopropanol and acetone.
According to the preparation method of the electrostatic spinning fiber-based ultrathin continuous nano-spider web fiber material, the non-solvent used for inducing phase separation is a mixture of more than one of water, methanol, ethanol, propanol and isopropanol and a solvent used for a polymer solution (the solvent accounts for less than or equal to 30 wt%); the non-solvent may be present in liquid or gaseous form during phase separation, and if the non-solvent is present in gaseous form in the phase separation, the concentration of non-solvent in the environment is 80 v/v% or more.
According to the preparation method of the electrostatic spinning fiber-based ultrathin continuous nano-spider web fiber material, the phase separation temperature is 20-50 ℃, and the phase separation time is 20-120 min.
The invention also provides an electrostatic spinning fiber-based ultrathin continuous nano-cobweb fiber material prepared by adopting the method, wherein the surface of the electrostatic spinning fiber-based ultrathin continuous nano-cobweb fiber material is of a uniform continuous net-shaped structure; the average fiber diameter of the spider web in the electrostatic spinning fiber-based ultrathin continuous nano spider web fiber material is 20-70 nm, the aperture of the mesh is 10-500 nm, and the porosity is more than or equal to 85%.
The principle of the invention is as follows:
because the polymer solution has certain viscosity and surface tension, when the polymer solution is coated on the surface of the electrostatic spinning fiber substrate, the polymer solution tends to shrink rather than spread due to the self-tension, so that the polymer solution is difficult to be uniformly distributed on the surface of the electrostatic spinning fiber, a complete ultrathin liquid film cannot be formed, and the finally obtained net structure is not uniform and discontinuous, and the non-uniform and discontinuous spider-web structure causes the material to have large pore size and wide pore size distribution range.
The invention controls the surface tension to be matched with the surface tension of the electrostatic spinning fiber substrate by adding the surfactant into the polymer solution, namely, the surface tension of the polymer solution is controlled to be less than or equal to the surface tension of the electrostatic spinning fiber substrate, when the electrostatic spinning fiber substrate is selected, the surface tension is a fixed value (the surface tension is defined in the way that solid surface atoms have more energy than internal atoms of a substance, so the surface atoms can generate a spontaneous inward force, the solid surface tension is mainly related to surface elements and groups of the material, so the surface tension can be considered to be a fixed value when the electrostatic spinning substrate is selected), therefore, the surface tension of the solution can be regulated and controlled by adding the surfactant into the solution to be less than or equal to the surface tension of the substrate, so that the polymer solution can be rapidly spread into a complete and uniform layer of ultra-thin liquid film on the surface of the electrostatic spinning fiber substrate, and the uniform and continuous ultra-thin nano-thin cobweb knot can be formed on The structure of the nanometer spider-web structure (the aperture of the mesh is 10-500 nm) can effectively reduce the aperture of the material and simultaneously enable the pore structure to be more uniform, and in addition, the ultrathin thickness (the thickness is 20-70 nm) of the nanometer spider-web can further optimize the porosity of the material.
Has the advantages that:
(1) the ultrathin continuous nano-cobweb material can obviously reduce the aperture of the electrospun nano-fiber membrane, and can keep the pore connectivity and porosity of the electrospun nano-fiber membrane;
(2) compared with the existing nano-cobweb material, the ultrathin continuous nano-cobweb material has the advantages of more optimized pore structure, smaller pore diameter and more uniform pore diameter distribution, and can remarkably improve the filtering precision of the material.
Detailed Description
The invention will be further illustrated with reference to specific embodiments. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example 1
A process for preparing the electrostatic spinning fibre-base ultra-thin continuous nano cobweb fibre material includes such steps as providing a weight-average molecular weight of 10104Adding a surfactant (lauryl sodium sulfate) into a g/mol polymer (cotton cellulose) solution to obtain a mixed solution, enabling the surface tension of the mixed solution to be less than or equal to that of an electrostatic spinning fiber base material (polyamide electrostatic spinning nanofiber membrane), then coating the mixed solution on the surface of the electrostatic spinning fiber base material and spreading the mixed solution to form an ultrathin continuous liquid membrane, and finally preparing the electrostatic spinning fiber base ultrathin continuous nano spider web fiber material by non-solvent induced phase separation; wherein the solvent of the polymer solution is N-methylmorpholine-N-oxide; the addition amount of the surfactant was 0.002 wt% of the polymer solution, the concentration of the polymer in the mixed solution was 0.001 wt%, the viscosity of the mixed solution was 150 mPas, and the surface tension was 25 mN/m; the surface tension of the electrostatic spinning fiber base material is 33mN/m, and the coating amount of the mixed solution on the surface of the electrostatic spinning fiber base material is 15ul cm-2(ii) a The non-solvent used for inducing phase separation is a mixture of water and N-methylmorpholine-N-oxide in a mass ratio of 9: 1; the temperature of the phase separation was 50 ℃ and the phase separation time was 20 min.
The surface of the finally prepared electrostatic spinning fiber-based ultrathin continuous nano-cobweb fiber material is of a uniform continuous network structure; the average fiber diameter of the spider web in the electrostatic spinning fiber-based ultrathin continuous nano spider web fiber material is 30nm, the thickness of the spider web is 30nm, the aperture of the mesh is 10-100 nm, and the porosity is 85%.
Example 2
A method for preparing electrostatic spinning fiber-based ultrathin continuous nanometer cobweb fiber material comprises firstly adding water to a solution with a weight average molecular weight of 42 × 104Adding a surfactant (sodium dodecyl benzene sulfonate) into a g/mol polymer (nitrocellulose) solution to obtain a mixed solution, so that the surface tension of the mixed solution is less than or equal to that of an electrostatic spinning fiber base material (a polyamide electrostatic spinning nanofiber membrane), then coating the mixed solution on the surface of the electrostatic spinning fiber base material and spreading the electrostatic spinning fiber base material into an ultrathin continuous liquid membrane, and finally preparing the electrostatic spinning fiber base ultrathin continuous nano spider web fiber material by non-solvent induced phase separation; wherein the solvent of the polymer solution is acetone; the amount of the surfactant added was 1.5 wt% of the polymer solution, the concentration of the polymer in the mixed solution was 2.5 wt%, and the viscosity of the mixed solution was250 mPa.s, the surface tension is 30 mN/m; the surface tension of the electrostatic spinning fiber base material is 33mN/m, and the coating amount of the mixed solution on the surface of the electrostatic spinning fiber base material is 12ul cm-2(ii) a The non-solvent used for inducing phase separation is a mixture of propanol and acetone in a mass ratio of 8: 1; the temperature of the phase separation was 50 ℃ and the phase separation time was 20 min.
The surface of the finally prepared electrostatic spinning fiber-based ultrathin continuous nano-cobweb fiber material is of a uniform continuous network structure; the average fiber diameter of the spider web in the electrostatic spinning fiber-based ultrathin continuous nano spider web fiber material is 20nm, the thickness of the spider web is 20nm, the aperture of the mesh is 50-200 nm, and the porosity is 90%.
Example 3
A method for preparing electrostatic spinning fiber-based ultrathin continuous nanometer cobweb fiber material comprises firstly adding a solvent to a solution containing a polar solvent and a solvent to obtain a solution with a weight average molecular weight of 27 × 104Adding surfactant (tetrabutylammonium chloride) into g/mol polymer (cellulose acetate) solution to obtain mixed solution, and making the surface tension of the mixed solution be less than or equal to that of electrostatic spinning fiber base material (SiO)2Electrostatic spinning nanofiber membrane), then coating the mixed solution on the surface of an electrostatic spinning fiber base material and spreading the electrostatic spinning fiber base material into a layer of ultrathin continuous liquid membrane, and finally preparing the electrostatic spinning fiber base ultrathin continuous nano spider web fiber material by non-solvent induced phase separation; wherein, the solvent of the polymer solution is N, N-dimethylformamide and dimethyl sulfoxide with the volume ratio of 1: 1; the addition amount of the surfactant is 1 wt% of the polymer solution, the concentration of the polymer in the mixed solution is 2 wt%, the viscosity of the mixed solution is 400 mPa.s, and the surface tension is 40 mN/m; the surface tension of the electrostatic spinning fiber base material is 47mN/m, and the coating amount of the mixed solution on the surface of the electrostatic spinning fiber base material is 12ul cm-2(ii) a The non-solvent used for inducing phase separation is methanol; the temperature of the phase separation was 45 ℃ and the phase separation time was 50 min.
The surface of the finally prepared electrostatic spinning fiber-based ultrathin continuous nano-cobweb fiber material is of a uniform continuous network structure; the average fiber diameter of the spider web in the electrostatic spinning fiber-based ultrathin continuous nano spider web fiber material is 38nm, the spider web thickness is 40nm, the mesh aperture is 10-300 nm, and the porosity is 88%.
Example 4
A method for preparing electrostatic spinning fiber-based ultrathin continuous nanometer cobweb fiber material comprises firstly adding water to obtain a mixture with a weight average molecular weight of 7.9 × 104Adding a surfactant (octadecyl dimethyl benzyl ammonium chloride) into a g/mol polymer (polyether sulfone) solution to obtain a mixed solution, so that the surface tension of the mixed solution is less than or equal to that of an electrostatic spinning fiber substrate (electrostatic spinning carbon nanofiber membrane), then coating the mixed solution on the surface of the electrostatic spinning fiber substrate and spreading the electrostatic spinning fiber substrate into an ultrathin continuous liquid membrane, and finally preparing the electrostatic spinning fiber-based ultrathin continuous nano spider web fiber material by non-solvent induced phase separation; wherein the solvent of the polymer solution is dimethyl sulfoxide; the addition amount of the surfactant was 0.25% by weight of the polymer solution, the concentration of the polymer in the mixed solution was 1.5% by weight, the viscosity of the mixed solution was 270 mPas, and the surface tension was 33 mN/m; the surface tension of the electrostatic spinning fiber base material is 36mN/m, and the coating amount of the mixed solution on the surface of the electrostatic spinning fiber base material is 10ul cm-2(ii) a The non-solvent used for inducing phase separation is acetone; the temperature of the phase separation was 40 ℃ and the phase separation time was 85 min.
The surface of the finally prepared electrostatic spinning fiber-based ultrathin continuous nano-cobweb fiber material is of a uniform continuous network structure; the average fiber diameter of a spider web in the electrostatic spinning fiber-based ultrathin continuous nano spider web fiber material is 25nm, the thickness of the spider web is 25nm, the aperture of a mesh is 200-500 nm, and the porosity is 95%.
Example 5
A method for preparing electrostatic spinning fiber-based ultrathin continuous nanometer cobweb fiber material comprises firstly adding a solvent to obtain a mixture with a weight average molecular weight of 2.5 × 104Adding a surfactant (cetyl trimethyl ammonium bromide) into a g/mol polymer (polyetherimide) solution to obtain a mixed solution, so that the surface tension of the mixed solution is less than or equal to that of an electrostatic spinning fiber base material (a cellulose electrostatic spinning nanofiber membrane), then coating the mixed solution on the surface of the electrostatic spinning fiber base material and spreading the electrostatic spinning fiber base material into an ultrathin continuous liquid membrane, and finally carrying out non-solvent induced phase separation to prepare the electrostatic spinning fiber base ultrathin continuous nano spider web fiber material; wherein the solvent of the polymer solution is N, N-dimethylacetamide;the addition amount of the surfactant was 0.12 wt% of the polymer solution, the concentration of the polymer in the mixed solution was 3 wt%, the viscosity of the mixed solution was 300 mPas, and the surface tension was 40 mN/m; the surface tension of the electrospun fiber substrate was 44mN/m, and the coating amount of the mixed solution on the surface of the electrospun fiber substrate was 10ul cm-2(ii) a The non-solvent used for inducing phase separation is isopropanol; the temperature of the phase separation was 40 ℃ and the phase separation time was 85 min.
The surface of the finally prepared electrostatic spinning fiber-based ultrathin continuous nano-cobweb fiber material is of a uniform continuous network structure; the average fiber diameter of the spider web in the electrostatic spinning fiber-based ultrathin continuous nano spider web fiber material is 50nm, the thickness of the spider web is 50nm, the aperture of the mesh is 50-300 nm, and the porosity is 88%.
Example 6
A method for preparing electrostatic spinning fiber-based ultrathin continuous nanometer cobweb fiber material comprises firstly adding water to a solution of a solvent with a weight average molecular weight of 88 × 104Adding a surfactant (dodecyl trimethyl ammonium bromide) into a g/mol polymer (poly (m-phenylene isophthalamide)) solution to obtain a mixed solution, so that the surface tension of the mixed solution is less than or equal to that of an electrostatic spinning fiber base material (polyethylene glycol terephthalate electrostatic spinning nanofiber membrane), then coating the mixed solution on the surface of the electrostatic spinning fiber base material and spreading the electrostatic spinning fiber base material into an ultrathin continuous liquid membrane, and finally preparing the electrostatic spinning fiber base ultrathin continuous nano spider web fiber material by non-solvent induced phase separation; wherein the solvent of the polymer solution is N, N-dimethylformamide; the addition amount of the surfactant was 0.01 wt% of the polymer solution, the concentration of the polymer in the mixed solution was 0.005 wt%, the viscosity of the mixed solution was 600 mPas, and the surface tension was 40 mN/m; the surface tension of the electrostatic spinning fiber base material is 41mN/m, and the coating amount of the mixed solution on the surface of the electrostatic spinning fiber base material is 8ul cm-2(ii) a The non-solvent used for inducing phase separation is propanol; the temperature of the phase separation was 30 ℃ and the phase separation time was 100 min.
The surface of the finally prepared electrostatic spinning fiber-based ultrathin continuous nano-cobweb fiber material is of a uniform continuous network structure; the average fiber diameter of the spider web in the electrostatic spinning fiber-based ultrathin continuous nano spider web fiber material is 55nm, the spider web thickness is 55nm, the mesh aperture is 30-200 nm, and the porosity is 91%.
Example 7
A process for preparing the electrostatic spinning fibre-base ultra-thin continuous nano cobweb fibre material includes such steps as providing the superfine fibre material with weight-average molecular weight of 18X 104Adding a surfactant (polyoxyethylene sorbitan monopalmitate) into a g/mol polymer (polyurethane) solution to obtain a mixed solution, enabling the surface tension of the mixed solution to be less than or equal to that of an electrostatic spinning fiber base material (polypropylene electrostatic spinning nanofiber membrane), then coating the mixed solution on the surface of the electrostatic spinning fiber base material and spreading the electrostatic spinning fiber base material into a layer of ultrathin continuous liquid membrane, and finally preparing the electrostatic spinning fiber base ultrathin continuous nano spider web fiber material by non-solvent induced phase separation; wherein the solvent of the polymer solution is N, N-dimethylacetamide; the addition amount of the surfactant was 1 wt% of the polymer solution, the concentration of the polymer in the mixed solution was 1 wt%, the viscosity of the mixed solution was 120 mPas, and the surface tension was 28 mN/m; the surface tension of the electrostatic spinning fiber base material is 31mN/m, and the coating amount of the mixed solution on the surface of the electrostatic spinning fiber base material is 6ul cm-2(ii) a The non-solvent used for inducing phase separation is ethanol; the temperature of the phase separation was 30 ℃ and the phase separation time was 100 min.
The surface of the finally prepared electrostatic spinning fiber-based ultrathin continuous nano-cobweb fiber material is of a uniform continuous network structure; the average fiber diameter of a spider web in the electrostatic spinning fiber-based ultrathin continuous nano spider web fiber material is 25nm, the thickness of the spider web is 25nm, the aperture of a mesh is 200-500 nm, and the porosity is 93%.
Example 8
A method for preparing electrostatic spinning fiber-based ultrathin continuous nanometer cobweb fiber material comprises firstly adding a solvent to a solution containing a polar solvent and a solvent to obtain a solution with a weight average molecular weight of 68 × 104Adding surfactant (polyoxyethylene sorbitan monostearate) into g/mol polymer (polyvinylidene fluoride) solution to obtain mixed solution, making the surface tension of the mixed solution be less than or equal to that of electrostatic spinning fiber base material (polytetrafluoroethylene electrostatic spinning nanofiber membrane), then coating the mixed solution on the surface of the electrostatic spinning fiber base material and spreading it to form a layer of ultrathin continuous liquid membrane, finally making it pass through non-solvent induced phase separationPreparing an electrostatic spinning fiber-based ultrathin continuous nano-spider web fiber material; wherein the solvent of the polymer solution is N, N-dimethylformamide; the addition amount of the surfactant is 1 wt% of the polymer solution, the concentration of the polymer in the mixed solution is 2 wt%, the viscosity of the mixed solution is 450mPa & s, and the surface tension is 18 mN/m; the surface tension of the electrostatic spinning fiber base material is 22mN/m, and the coating amount of the mixed solution on the surface of the electrostatic spinning fiber base material is 4ul cm-2(ii) a The non-solvent used for inducing phase separation is methanol; the temperature of the phase separation was 25 ℃ and the phase separation time was 100 min.
The surface of the finally prepared electrostatic spinning fiber-based ultrathin continuous nano-cobweb fiber material is of a uniform continuous network structure; the average fiber diameter of the spider web in the electrostatic spinning fiber-based ultrathin continuous nano spider web fiber material is 35nm, the spider web thickness is 35nm, the mesh aperture is 20-200 nm, and the porosity is 94%.
Example 9
A method for preparing electrostatic spinning fiber-based ultrathin continuous nanometer cobweb fiber material comprises firstly adding water to a solution with a weight average molecular weight of 5 × 104Adding a surfactant (polyoxyethylene sorbitan monooleate) into a g/mol polymer (polyacrylonitrile) solution to obtain a mixed solution, so that the surface tension of the mixed solution is less than or equal to that of an electrostatic spinning fiber base material (a polyamide electrostatic spinning nanofiber membrane), then coating the mixed solution on the surface of the electrostatic spinning fiber base material and spreading the electrostatic spinning fiber base material into an ultrathin continuous liquid membrane, and finally preparing the electrostatic spinning fiber base ultrathin continuous nano spider web fiber material by non-solvent induced phase separation; wherein the solvent of the polymer solution is N-methyl pyrrolidone; the addition amount of the surfactant was 0.5% by weight of the polymer solution, the concentration of the polymer in the mixed solution was 1.5% by weight, the viscosity of the mixed solution was 280 mPas, and the surface tension was 30 mN/m; the surface tension of the electrostatic spinning fiber base material is 33mN/m, and the coating amount of the mixed solution on the surface of the electrostatic spinning fiber base material is 3ul cm-2(ii) a The non-solvent used for inducing phase separation is water; the temperature of the phase separation was 20 ℃ and the phase separation time was 120 min.
The surface of the finally prepared electrostatic spinning fiber-based ultrathin continuous nano-cobweb fiber material is of a uniform continuous network structure; the average fiber diameter of a spider web in the electrostatic spinning fiber-based ultrathin continuous nano spider web fiber material is 33nm, the thickness of the spider web is 33nm, the aperture of a mesh is 50-400 nm, and the porosity is 91%.
Claims (10)
1. A method for preparing an electrostatic spinning fiber-based ultrathin continuous nano spider web fiber material is characterized by comprising the following steps: firstly, adding a surfactant into a polymer solution to obtain a mixed solution, then coating the mixed solution on the surface of an electrostatic spinning fiber substrate and spreading the mixed solution to form an ultrathin continuous liquid film, and finally preparing the electrostatic spinning fiber-based ultrathin continuous nano-spider web fiber material which takes electrostatic spinning fibers as the substrate and is covered with an ultrathin continuous nano-spider web structure on the surface layer through non-solvent induced phase separation;
the surface tension of the mixed solution is less than or equal to the surface tension of the electrostatic spinning fiber base material;
the polymer is polyacrylonitrile, polyvinylidene fluoride, polyurethane, polyisophthaloyl metaphenylene diamine, polyetherimide, polyethersulfone, cellulose acetate, nitrocellulose or cellulose, and the electrostatic spinning fiber substrate is an electrostatic spinning nano-fiber membrane;
the cobweb thickness of the electrospun fiber-based ultrathin continuous nano cobweb fiber material is 20-70 nm.
2. The method for preparing the electrospun fiber-based ultrathin continuous nano-spider web fiber material of claim 1, wherein the surfactant is polyoxyethylene sorbitan monooleate, polyoxyethylene sorbitan monostearate, polyoxyethylene sorbitan monopalmitate, dodecyltrimethylammonium bromide, hexadecyltrimethylammonium bromide, octadecyldimethylbenzylammonium chloride, tetrabutylammonium chloride, sodium dodecylbenzenesulfonate or sodium dodecylsulfate, and the addition amount of the surfactant is 0.0002-2 wt% of the polymer solution.
3. The method for preparing the electrospun fiber-based ultrathin continuous nano-spider web fiber material according to claim 2, wherein the weight average molecular weight of the polymer is 5 x 104～100×104g/mol, the concentration of the polymer in the mixed solution is 0.001-5 wt%, and the viscosity of the mixed solution is 50-1000 mPas.
4. The method for preparing an electrospun fiber-based ultrathin continuous nano-spider web fiber material according to claim 3, characterized in that the solvent of the polymer solution is one or more of N, N-dimethylacetamide, N-dimethylformamide, N-methylpyrrolidone, dimethyl sulfoxide, N-methylmorpholine-N-oxide and acetone.
5. The method for preparing the electrospun fiber-based ultrathin continuous nano-spider web fiber material according to claim 4, wherein the electrospun fiber substrate is a polyamide electrospun nanofiber membrane, a polytetrafluoroethylene electrospun nanofiber membrane, a polypropylene electrospun nanofiber membrane, a polyethylene terephthalate electrospun nanofiber membrane, a cellulose electrospun nanofiber membrane, an electrospun carbon nanofiber membrane, or an SiO2Electrospun nanofiber membranes.
6. The method for preparing the electrospun fiber-based ultrathin continuous nano-spider web fiber material according to claim 5, wherein the surface tension of the electrospun fiber base material is 22-47 mN/m, and the surface tension of the mixed solution is 15-45 mN/m; the coating amount of the mixed solution on the surface of the electrostatic spinning fiber substrate is 3-15 ul cm-2。
7. The method for preparing the electrospun fiber-based ultrathin continuous nano-spider web fiber material according to claim 1, wherein the non-solvent used for the non-solvent induced phase separation is one or more of water, methanol, ethanol, propanol, isopropanol and acetone.
8. The method for preparing an electrospun fiber-based ultrathin continuous nano-spider web fiber material according to claim 1, characterized in that the non-solvent used for non-solvent induced phase separation is a mixture of more than one of water, methanol, ethanol, propanol and isopropanol with the solvent used for the polymer solution.
9. The method for preparing the electrospun fiber-based ultrathin continuous nano-spider web fiber material according to claim 7 or 8, characterized in that the temperature of phase separation is 20-50 ℃ and the time of phase separation is 20-120 min.
10. The electrospun fiber-based ultrathin continuous nano-spider web fiber material prepared by the method of any one of claims 1 to 9, which is characterized in that: the surface is a uniform continuous network structure; the average fiber diameter of the spider web in the electrostatic spinning fiber-based ultrathin continuous nano spider web fiber material is 20-70 nm, the aperture of the mesh is 10-500 nm, and the porosity is more than or equal to 85%.
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