CN102691176A - Method for preparing patterning nanofiber membrane by utilizing insulating receiving template static spinning - Google Patents
Method for preparing patterning nanofiber membrane by utilizing insulating receiving template static spinning Download PDFInfo
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- CN102691176A CN102691176A CN2012101972177A CN201210197217A CN102691176A CN 102691176 A CN102691176 A CN 102691176A CN 2012101972177 A CN2012101972177 A CN 2012101972177A CN 201210197217 A CN201210197217 A CN 201210197217A CN 102691176 A CN102691176 A CN 102691176A
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Abstract
The invention relates to a method for preparing a patterning nanofiber membrane by utilizing insulating receiving template static spinning. The method comprises the following specific steps: (1) dissolving high polymer in a solvent, and stirring until the high polymer is completely dissolved, so as to obtain a spinning solution; and (2) carrying out static spinning on the spinning solution, and taking an insulating substance with a topological structure on the surface as a static spinning receiving device, so as to obtain the patterning nanofiber membrane. According to the preparation method disclosed by the invention, the nanofiber membrane with various patterns can be prepared conveniently and quickly at low cost. Since the patterning nanofiber membrane obtained by the invention is accurate in pattern, controllable and good in repeatability, the patterning nanofiber membrane has good application prospect in the fields of industry and medicine, especially in the field of regenerative medicine based on tissue engineering.
Description
Technical field
The invention belongs to the preparation field of nano fibrous membrane, particularly a kind of method of utilizing insulation reception template electrostatic spinning to be equipped with the patterned nano-fiber film.
Background technology
Electrostatic spinning is a kind of simple and easy to do nanofiber preparation method.The gained nanofiber has a wide range of applications in fields such as sensor, organizational project, catalysis, composite reinforcing material and filtrations owing to have advantages such as porosity height, specific area are big.The nanofibrous structures of patterning has important use and is worth in above-mentioned field.For example in organizational project; To tissues such as picture muscle, nerve, blood vessel, bones; The patterned nano-fiber structure can be simulated its specific structure preferably, thereby promotes the regeneration of sticking, move, breed, breaking up and organize [Dvir, the T. of cell; Et al.Nature Nanotechnology, 2011.6 (1): p.13-22.].But because the unstable whip of electrostatic spinning jet gets rid of, the fiber that obtains is random alignment mostly, is difficult to realize controllably depositing in order of fiber.
In order to address this problem, the whole bag of tricks is used to control the patterning of electrostatic spinning nano fiber in recent years.These methods mainly are through changing electric field, use various gathering-devices and the electrostatic spinning fiber subsequent treatment being obtained patterned nano-fiber.Wherein, using figuratum conduction template to prepare patterned nano-fiber is one of simple, the most the most frequently used method.Xia etc. have prepared the nanofiber of orientations, and have further obtained the tunica fibrosa [Li of braided structure through introducing clearance for insulation in the conduction receiving system; D.; Y.L.Wang, and Y.N.Xia.Advanced Materials, 2004.16 (4): p.361-366.].[Zhang, D.and J.Chang.Advanced Materials, 2007.19 (21): p.3664-3667 such as Zhang; Zhang; D.M.and J.Chang.Nano Letters; 2008.8 (10): p.3283-3287.] reported that the conducted electricity receiving system that utilizes different pattern comes the controlling fiber deposition, thereby obtained the two-dimensional nano tunica fibrosa and the three-dimensional manometer fiber tubular structure of different pattern.Wu etc. [Wu, Y., et al.Polymer, 2010.51 (14): p.3244-3248.] but the metal form electrostatic spinning through different pattern has prepared tunica fibrosa self-supporting, that have different pattern.[Vaquette C such as Vaquette; Cooper-White JJ.Acta Biomaterialia; 2011,7 (6): p.2544-2557.] utilize hollow round metal hole pattern to prepare the macropore fibrous framework, and further studied the growing state of cell on this support as receiving system.
Above-mentioned these methods all are through using figuratum conduction template to prepare the tunica fibrosa of patterning.The formation of the arrangement of fiber, the deposition of fiber and patterning mainly is to be determined by the conduction receiving system with pattern.And, often need a complicacy, meticulous and expensive process in order to obtain these conduction receiving systems (great majority for metal) with pattern.Therefore, be difficult to prepare the nano fibrous membrane of various patterns through processing the conducted electricity receiving system of various patterns.
But, about obtaining pattern template (like non-conductive templates such as paper, plastics) through being prone to substances processed, and then the preparation patterned nano-fiber, then rarely have bibliographical information.[Cho, S.J., et al.Langmuir, 2010.26 (18): p.14395-14399.] reported the preservative film that on conductive electrode, covers one deck insulation, on preservative film, deposited the tunica fibrosa the same such as Cho with the conductive electrode pattern.But this method still utilizes the conduction template to form the patterning fiber in fact.[Dempsey such as David; D.K.; Et al.Macromolecular Materials and Engineering; 2010.295 (11): the p.990-994.] deposition of the silica gel gathering-device controlling fiber through having pattern, electro-spinning is provided figuratum polyurethane fiber film fully, but its used silica gel template then is covered with copper base conductive layer.[A.Zucchelli such as Zucchelli; D.Fabiani; C.Gualandi and M.L.Focarete, Journal of Materials Science, 2009.44 (18): p.4969-4975.] prepare tunica fibrosa with pattern through the enamel coating on the metal.But these methods are the deposition of controlling fiber accurately, more can't prepare the nano fibrous membrane with various complicacies, exquisite patterning.
Summary of the invention
Technical problem to be solved by this invention provides a kind of method of utilizing insulation reception template electrostatic spinning to be equipped with the patterned nano-fiber film; The patterned nano-fiber film of this method preparation is because accurate, the controlled and good reproducibility of its pattern has extraordinary application prospect in industry and field of medicaments.
A kind of method of utilizing insulation reception template electrostatic spinning to be equipped with the patterned nano-fiber film of the present invention, concrete steps comprise:
(1) high molecular polymer is dissolved in the solvent, is stirred to dissolving fully, obtain spinning solution;
(2) carry out electrostatic spinning with above-mentioned spinning solution, the megohmite insulant that has topological structure with the surface promptly obtains and receiving system pattern nano fibrous membrane closely similar, that have patterning as the electrostatic spinning receiving system.
High molecular polymer described in the step (1) is a poly; PPTA; Cellulose acetate; Polyaniline; PEO; Polylactide; Polystyrene; Polyacrylonitrile; Polycaprolactone; Polyvinylpyrrolidone; Polymethyl methacrylate; Polyethylene glycol oxalate; Merlon; Nylon 6; Polyvinyl alcohol; PLA; Poly butyric ester; Gather the valeric acid butyrate; Gather 3-hydroxybutyric acid and 3-hydroxycaproic acid copolymer; Shitosan; Cellulose; Hyaluronic acid; Fibroin; Gelatin; In the collagen one or more.
Solvent described in the step (1) is trifluoroethanol, water, acetate, N, one or more in dinethylformamide, dimethylacetylamide, formic acid, sulfuric acid, ethanol, methyl alcohol, carrene, chloroform, acetone, oxolane, ether, methyl-sulfoxide, trifluoroacetic acid and the hexafluoroisopropanol.
The concentration of high molecular polymer is 2~20% in the spinning solution described in the step (1).
The megohmite insulant that surface described in the step (2) has a topological structure is paper, the cloth with decorative pattern with decorative pattern, have the glass of decorative pattern or have the plastics of decorative pattern.
The megohmite insulant that surface described in the step (2) has topological structure is polystyrene foam, toilet paper, napkin paper or mesh cloth.
The spinning condition of the electrostatic spinning described in the step (2) is preferably following: voltage is 1~100kV; Electric field or receiving range are 0.02~2m, and spinnerette diameters is 1 μ m~2mm, and the spinning solution delivery rate is 0.1~10mL/h; Environment temperature is 20~60 ℃, and envionmental humidity is 20~80%.
The present invention prepares the nano fibrous membrane with various complicacies, exquisite patterning through the patterning of non-conductive template control electrostatic spinning fiber; The present invention with non-conductive materials such as polystyrene foam, toilet paper, mesh cloth as receiving system; High molecular polymer is dissolved in obtains spinning solution in the solvent; Obtained with the receiving system pattern closely similarly through electrostatic spinning, had the nano fibrous membrane of pattern structure.
Used receiving system is non-conductive material among the present invention, and the surface has rough topological structure, and the deposition of the topological morphology control nanofiber on surface forms the nano fibrous membrane with pattern structure.
The present invention is a deposition of controlling nanofiber through the topological pattern that utilizes non-conductive receiving system surface; Obtain a cover and can accurately control the process of the patterning of electrostatic spinning fiber, and then prepare nano fibrous membrane with various complicacies, exquisite patterning.Therefore, the present invention can promote greatly that static spins the development and application of patterned nano-fiber film, further paves the way for realizing its effective application in industry and medicine and other fields.
Beneficial effect
(1) template with pattern that the present invention is used is dirt cheap, is easy to get, and need not complicated processing.Thereby the receiving system through various patterns, can prepare the nano fibrous membrane of various patterns easily and fast, at an easy rate.For example, can be through paper be carried out the paper that embossing obtains various patterns, and then prepare the nano fibrous membrane of various patterns.
(2) the present invention can prepare the nano fibrous membrane (20cm * 20cm), can accurately control the patterning of nanofiber simultaneously of larger area patterning.
(3) the patterned nano-fiber film of the present invention's preparation is because accurate, the controlled and good reproducibility of its pattern; In industry and field of medicaments, especially extraordinary application prospect is arranged in regenerative medicine field (as: as bionic nano fibrous framework) with macroporous structure based on organizational project.
Description of drawings
Fig. 1 is that the present invention prepares the used device of patterning fiber;
Fig. 2 is to be the enlarged drawing of the patterning tunica fibrosa that obtains of receiving system with the polystyrene foam;
Fig. 3 be the present invention prepare closely similar with the receiving system pattern, by the resulting tunica fibrosa of nanofiber selective deposition with patterning.Wherein a is with a kind of pictorial diagram with napkin paper of decorative pattern as receiving device; The nano fibrous membrane with pattern of b for obtaining with this receiving system;
Fig. 4 is to be the light microscopic enlarged drawing of the patterning fiber that obtains of receiving system with a kind of napkin paper with decorative pattern;
Fig. 5 is the ESEM enlarged drawing of toilet paper;
Fig. 6 is to be the light microscopic enlarged drawing of the patterning tunica fibrosa that obtains of receiving system with the toilet paper;
Fig. 7 is to be the ESEM enlarged drawing of the patterning tunica fibrosa that obtains of receiving system with the toilet paper;
Fig. 8 is a kind of light microscopic enlarged drawing of mesh cloth;
Fig. 9 is to be the light microscopic enlarged drawing of the patterning tunica fibrosa that obtains of receiving system with mesh cloth;
Figure 10 is the nano fibrous membrane of the different pattern that obtains as receiving system with other different megohmite insulants.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in the restriction scope of the present invention.Should be understood that in addition those skilled in the art can do various changes or modification to the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
0.5g gelatin and 0.5g polycaprolactone are dissolved in the trifluoroethanol of 10ml, in solution, add 20ul acetate, stir 24h to dissolving fully, obtaining concentration is the gelatin/polycaprolactone spinning solution of 10% (grams per milliliter).Select the syringe of 10ml for use, the syringe needle of 1.2mm internal diameter extracts gelatin/polycaprolactone spinning solution, is fixed on the micro-injection pump.Carry out electricity through electrostatic spinning apparatus as shown in Figure 1 and spin, parameter is: voltage 16kv, accept apart from 14cm, and injection rate 1ml/h, environment temperature is 26 ℃, envionmental humidity is 55%.Adopt a kind of thickness be the polystyrene foam of 25mm as receiving system, obtained having the nano fibrous membrane of patterning.The polystyrene electrical conductivity is (σ) 10
-16S/m is a kind of typical insulating materials.Therefore, can think surface topology pattern, i.e. the deposition of the concaveconvex structure of material surface control electrospinning fibre, rather than the deposition of electric field force controlling fiber owing to receiving system.Fig. 2 is the nano fibrous membrane that obtains as receiving system with polystyrene foam.
0.7g gelatin and 0.3g polycaprolactone are dissolved in the trifluoroethanol of 10ml, in solution, add 20ul acetate, stir 24h to dissolving fully, obtaining concentration is the gelatin/polycaprolactone spinning solution of 10% (grams per milliliter).Select the syringe of 10ml for use, the syringe needle of 1.2mm internal diameter extracts gelatin/polycaprolactone spinning solution, is fixed on the micro-injection pump.Carry out electricity through electrostatic spinning apparatus as shown in Figure 1 and spin, parameter is: voltage 12kv, accept apart from 11cm, and injection rate 2ml/h, environment temperature is 28 ℃, envionmental humidity is 45%.Adopt a kind of napkin paper as receiving system with decorative pattern, obtained with its picture on surface closely similar, the nano fibrous membrane with patterning.As shown in Figure 3, wherein a is receiving device (a kind of napkin paper with decorative pattern), the tunica fibrosa of b for obtaining with this receiving system.Fig. 4 is the enlarged drawing that spins the patterning fiber that obtains with the napkin paper for receiving system static.
Embodiment 3
0.6g gelatin and 0.4g polycaprolactone are dissolved in the trifluoroethanol of 10ml, in solution, add 20ul acetate, stir 24h to dissolving fully, obtaining concentration is the gelatin/polycaprolactone spinning solution of 10% (grams per milliliter).Select the syringe of 10ml for use, the syringe needle of 1.2mm internal diameter extracts gelatin/polycaprolactone spinning solution, is fixed on the micro-injection pump.Carry out electricity through electrostatic spinning apparatus as shown in Figure 1 and spin, parameter is: voltage 15kv, accept apart from 12cm, and injection rate 2ml/h, environment temperature is 23 ℃, envionmental humidity is 54%.Adopt toilet paper commonly used in the daily life as receiving system, it is closely similar to have obtained pattern of indentations surperficial with it, has the nano fibrous membrane of patterning.Fig. 5 is the Electronic Speculum enlarged drawing of toilet paper; Fig. 6 is the enlarged drawing that spins the patterning fiber that obtains with the toilet paper for receiving system static.Fig. 7 is to be the ESEM enlarged drawing of the 3D macropore support that obtains of receiving system with the toilet paper.Can know that from Fig. 7 the 3D macropore support of this method preparation is to be about the fibrous of 500 nanometers by smooth, nothing bonding, average diameter.
Embodiment 4
0.7g gelatin and 0.3g PLA are dissolved in the trifluoroethanol of 10ml, in solution, add 20ul acetate, stir 24h to dissolving fully, obtaining concentration is the gelatin/polycaprolactone spinning solution of 10% (grams per milliliter).Select the syringe of 10ml for use, the syringe needle of 1.2mm internal diameter extracts gelatin/polycaprolactone spinning solution, is fixed on the micro-injection pump.Carry out electricity through electrostatic spinning apparatus as shown in Figure 1 and spin, parameter is: voltage 14kv, accept apart from 13cm, and injection rate 1ml/h, environment temperature is 22 ℃, envionmental humidity is 55%.Adopt a kind of mesh cloth as receiving system, obtained with its picture on surface closely similar, the nano fibrous membrane with patterning.Fig. 8 is the enlarged drawing of mesh cloth; Fig. 9 is to be the enlarged drawing that receiving system static spins the patterning fiber that obtains with mesh cloth.Can find out that from above two figure the protruding part of mesh cloth is prone to deposit fiber, the part of depression is difficult for deposit fiber, thereby makes the tunica fibrosa that receives form patterning.
Therefore, this method can be prepared the nano fibrous membrane of various pattern easily with the insulating materials (like the paper of various patterns) that is dirt cheap, is easy to get and have various patterns as template.Further use other various non-conductive materials as template, prepared the nano fibrous membrane of various pattern equally, shown in figure 10.
Claims (7)
1. one kind is utilized insulation to receive the method that the template electrostatic spinning is equipped with the patterned nano-fiber film, and concrete steps comprise:
(1) high molecular polymer is dissolved in the solvent, is stirred to dissolving fully, obtain spinning solution;
(2) carry out electrostatic spinning with above-mentioned spinning solution, the megohmite insulant that has topological structure with the surface promptly gets the patterned nano-fiber film as the electrostatic spinning receiving system.
2. according to claim 1ly a kind ofly utilize insulation to receive the method that the template electrostatic spinning is equipped with the patterned nano-fiber film, it is characterized in that: the high molecular polymer described in the step (1) is poly, PPTA, cellulose acetate, polyaniline, PEO, polylactide, polystyrene, polyacrylonitrile, polycaprolactone, polyvinylpyrrolidone, polymethyl methacrylate, polyethylene glycol oxalate, Merlon, nylon 6, polyvinyl alcohol, PLA, poly butyric ester, gather the valeric acid butyrate, gather 3-hydroxybutyric acid and 3-hydroxycaproic acid copolymer, in the shitosan, cellulose, hyaluronic acid, fibroin, gelatin, collagen one or more.
3. a kind of method of utilizing insulation reception template electrostatic spinning to be equipped with the patterned nano-fiber film according to claim 1; It is characterized in that: the solvent described in the step (1) is trifluoroethanol, water, acetate, N, one or more in dinethylformamide, dimethylacetylamide, formic acid, sulfuric acid, ethanol, methyl alcohol, carrene, chloroform, acetone, oxolane, ether, methyl-sulfoxide, trifluoroacetic acid and the hexafluoroisopropanol.
4. a kind of method of utilizing insulation reception template electrostatic spinning to be equipped with the patterned nano-fiber film according to claim 1, it is characterized in that: the concentration of high molecular polymer is 2~20% in the spinning solution described in the step (1).
5. according to claim 1ly a kind ofly utilize insulation to receive the method that the template electrostatic spinning is equipped with the patterned nano-fiber film, it is characterized in that: the megohmite insulant that described surface has a topological structure is paper, the cloth with decorative pattern with decorative pattern, have the glass of decorative pattern or have the plastics of decorative pattern.
6. a kind of method of utilizing insulation reception template electrostatic spinning to be equipped with the patterned nano-fiber film according to claim 1, it is characterized in that: the megohmite insulant that described surface has topological structure is polystyrene foam, toilet paper, napkin paper or mesh cloth.
7. a kind of method of utilizing insulation reception template electrostatic spinning to be equipped with the patterned nano-fiber film according to claim 1; It is characterized in that: the spinning condition of the electrostatic spinning described in the step (2) is following: voltage is 1~100kV; Electric field or receiving range are 0.02~2m, and spinnerette diameters is 1 μ m~2mm, and the spinning solution delivery rate is 0.1~10mL/h; Environment temperature is 20~60 ℃, and envionmental humidity is 20~80%.
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