CN102776707A - Method for preparing PVP (polyvinyl pyrroloidone)/FF composite nano-fiber film by static spinning preparation - Google Patents
Method for preparing PVP (polyvinyl pyrroloidone)/FF composite nano-fiber film by static spinning preparation Download PDFInfo
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- CN102776707A CN102776707A CN201210238074XA CN201210238074A CN102776707A CN 102776707 A CN102776707 A CN 102776707A CN 201210238074X A CN201210238074X A CN 201210238074XA CN 201210238074 A CN201210238074 A CN 201210238074A CN 102776707 A CN102776707 A CN 102776707A
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Abstract
The invention relates to a static spinning preparation method for a polyvinyl pyrrolidone/biphenylalanine composite nano-fiber film. The method comprises the steps of: (1) slowly adding the polyvinyl pyrrolidon and the biphenylalanine into a mixing solvent of carbinol and N, N-methylacetamide along with agitating, and continuously agitating for 20 to 30 minutes until the mixture is completely swelled; and then vibrating for 15 to 24 hours at 25 plus or minus 2 DEG C until the mixture is dissolved completely so as to obtain the transparent polymer solution, and ultrasonically processing the transparent polymer solution for 15 minutes to degas so as to obtain spinning solution; and (2) statically spinning the obtained spinning solution to obtain a film, and then drying the film in vacuum to obtain the finished product. According to the method, the operation is simple, and less time is consumed, and the raw materials are cheap and easy to obtain; by adopting the method, the film material with diameter and aperture at nanometer level can be obtained; and the method is suitable for large-scale production.
Description
Technical field
The invention belongs to the preparation field of electrostatic spinning nano fiber film, particularly a kind of electro-spinning is equipped with the method for PVP/FF composite nano-fiber membrane.
Background technology
Electrostatic spinning technique is meant that polymer solution or melt are drawn into the process of fiber by injection.It is a kind of new method for preparing polymer nanofiber, and it can prepare diameter is nano level superfine fibre, and minimum diameter can be to 1nm.Polymer fiber than the conventional method preparation; The superfine fibre film that electricity spins that legal system is equipped with polymer nanofiber and has that equipment is simple, processing ease, efficient and electricity consumption spin the method preparation has the big and advantages such as porosity is high, light weight of specific area, and various fields such as organizational project, medicine and catalyst carrier, wound dressing, filtration, sensor, template, armored fabric, nanoelectronic element have potential using value.At present very many through the example that electrostatic spinning technique prepares nanofiber to polymer solution or melt, but the research of relevant micromolecular compound is also rarely found.
(Phe-Phe FF) is the core texture unit that forms the relevant 4 amyloid powder appearance polypeptide of diseases such as Alzheimer's disease and parkinsonism to two phenylalanines.Because two phenylalanines have the π-π effect between hydrogen bond, βZhe Die structure and aromatic rings; Have good self-assembly property, therefore can be in water or organic solvent it can self assembly forms the secondary or the tertiary structure of stable analogous protein through non-covalent bond effect such as the hydrogen bond between the molecule, Van der Waals force, π-π interaction, coordinate bond.In addition, because advantages such as its good degradability, biocompatibility receive much concern it.Since it comes to light, no matter be in medical science or the nanosecond science and technology field has all caused the research interest that people are very big.All the time, many scientists explore and regulate and control its self assembling process with diverse ways.In self assembling process, except the suitable solvent of needs, the proper technique means also are essential.For this reason, scientists attempts utilizing existing various technological means, waits the self assembly that guides fragrant small peptide like electrostatic spinning, ultrasonic wave, externally-applied magnetic field.For example, Singh etc. have carried out electricity and have spun being dissolved in FF monomer among the HFP, have obtained length and can reach millimetre-sized nanotube.But because FF monomer molecule amount is little, characteristic such as solution concentration is low makes the pure more difficult electricity of FF monomer spin.Do not carry out the report that electricity spins at present about FF and other mixture of polymers solution yet.
(polyvinylpyrrolidone is a kind of water miscible high molecular polymer PVP) to PVP, have favorable biological degradability and biocompatibility, and the PVP spinnability is better.Its molecule contains hydrophilic radical and lipophilic group simultaneously, can with multiple material, especially hydroxyl, carboxyl, amino and other contain compound bearing active hydrogen or simple substance forms complex compound, and all have widely in medicine and other fields and use.
Summary of the invention
Technical problem to be solved by this invention provides the method that a kind of electro-spinning is equipped with the PVP/FF composite nano-fiber membrane; This method is quick, easy, cheap, efficient; Prepared in batches and large-scale production; For the research and development of novel nano bioactive materials are offered reference, lay the first stone for further studying FF self assembly behavior.
A kind of electro-spinning of the present invention is equipped with the method for PVP/FF composite nano-fiber membrane, comprising:
(1) polyvinylpyrrolidone (PVP) and two phenylalanines (FF) powder are under agitation slowly joined in the mixed solvent of methyl alcohol and DMAc, continue to stir 20～30min to complete swelling; At 25 ± 2 ℃, vibration 15～24h is to dissolving fully then, and the polymer solution that obtains is transparence, and sonicated 15min outgases, and obtains spinning solution;
(2) adopt above-mentioned spinning solution to carry out electrostatic spinning and obtain film, last vacuumize promptly gets the PVP/FF composite nano-fiber membrane.
The volume ratio of methyl alcohol and DMAc in the described mixed solvent of step (1) (volumetric concentration>98%) is 85:15.
The mass ratio of FF and PVP is at 1:100～50:100 in the spinning solution that step (1) obtains.
The syringe specification is 5mL in the described electrostatic spinning of step (2), and the syringe needle internal diameter is 0.4 ~ 0.7mm, and receiving screen adopts the reception of aluminium foil ground connection, and the distance of syringe needle and receiving screen is 20～25cm.
The ejection flow velocity is 0.1～1.0mL/h in the described electrostatic spinning process of step (2).
Method of the present invention is quick, easy, cheap, efficient, is fit to prepared in batches PVP-FF composite nano-fiber membrane.
The present invention is main spinning material with PVP, and mix contain hydrophily functional group-COOH ,-NH
2Two phenylalanines, through the quality when relevant spinning condition parameter of FF with PVP, successful realization blending, for further research FF self assembly behavior lays the first stone.
The fibre diameter of the PVP/FF composite nano-fiber membrane that the present invention obtains is along with the mass ratio of FF and PVP increases and reduces earlier afterwards to increase; Increase along with the increase of flow velocity.
Beneficial effect
(1) the inventive method is simple to operate, and is consuming time less, can obtain diameter and aperture at nano level membrane material, is applicable to large-scale production;
(2) raw material used in the present invention are cheap and easy to get, have good degradability and biocompatibility, have to use the potentiality that it does follow-up related experiment analysis.
Description of drawings
Fig. 1 is 10% (w/v) for fixing PVP content, and spinning voltage is 16kv, and receiving range is 25cm, and when the injection flow velocity was 1ml/h, different FF/PVP quality were than the electromicroscopic photograph of electrostatic spinning gained and to the influence of fibre diameter;
Fig. 2 is the diameter Distribution of different FF/PVP quality than electro spinning nano fiber;
Fig. 3 is 10% (w/v) for fixing PVP content, and the FF/PVP mass ratio is 50:100, and fixedly spinning voltage is 16kv, and receiving range is 25cm, the electromicroscopic photograph of different in flow rate electrostatic spinning gained and to the influence of fibre diameter;
The diameter Distribution of the nanofiber that Fig. 4 spins for the different in flow rate electricity;
Fig. 5 is FF, PVP and the different FF/PVP quality X diffraction pattern than electro spinning nano fiber;
Fig. 6 is FF, PVP and the different FF/PVP quality infrared spectrogram than electro spinning nano fiber: (a) FF, (b) PVP, (c) 4:100, (d) 6:100, (e) 20:100 and (f) 50:100;
Fig. 7 is FF, PVP and the different FF/PVP quality TG curve than electro spinning nano fiber: (a) PVP, (b) 4:100, (c) 6:100, (d) 20:100, (e) 50:100 and (f) FF.
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.
(1) be that 85:15 methyl alcohol and DMAC N,N (DMAc) mixed liquor are put into reaction vessel with volume ratio;
(2) load weighted PVP and FF powder are slowly added in the above-mentioned reaction vessel under stirring condition, continue to stir 20～30min to complete swelling; Wherein, the content of PVP in methyl alcohol and DMAc mixed liquor is fixed as 10% (w/w), and the mass ratio of FF and PVP is followed successively by: 0:100,4:100,6:100,20:100,50:100;
(3) conical flask is placed in the shaking table, at 25 ± 2 ℃, vibration 15～24h is to dissolving fully, and polymer solution is transparence, and sonicated 15min outgases, and makes spinning solution;
(4) (the syringe needle internal diameter is 0.4 ~ 0.7mm) extraction FF/PVP spinning solution, is fixed on the electrostatic spinning apparatus, and fixedly electrostatic pressure is 16kv with the 5ml syringe; Receiving range is 25cm; The injection flow velocity is 1mL/h, carries out electricity and spins, and obtains the PVP-FF composite nano-fiber membrane;
(5) film of collecting is put into more than the dry 24h of vacuum desiccator, subsequent use.
According to the nano fibrous membrane electromicroscopic photograph of the resultant different FF of above step and PVP mass ratio and as shown in Figure 1 to the influence of fibre diameter.
The diameter Distribution of the nanofiber of different FF and PVP mass ratio is as shown in Figure 2.
Resulting PVP/FF composite nano-fiber membrane is carried out XRD, FTIR and thermogravimetric (TG) characterize, the result is like Fig. 5,6, shown in 7.
(1) be 85:15 methyl alcohol and N with volume ratio, N-methylacetamide (DMAc) mixed liquor is put into reaction vessel;
(2) load weighted PVP and FF powder are slowly added in the above-mentioned reaction vessel under stirring condition, continue to stir 20～30min to complete swelling; Wherein, the content of PVP in methyl alcohol and DMAc mixed liquor is fixed as 10% (w/w), and the mass ratio of FF and PVP is 50:100;
(3) conical flask is placed in the shaking table, at 25 ± 2 ℃, vibration 15～24h is to dissolving fully, and polymer solution is transparence, and sonicated 15min outgases, and makes spinning solution;
(4) (the syringe needle internal diameter is 0.4 ~ 0.7mm) extraction FF/PVP spinning solution with the 5ml syringe; Be fixed on the electrostatic spinning apparatus; Fixedly electrostatic pressure is 16kv, and receiving range is 25cm, sprays flow velocity and is respectively 0.1mL/h, 0.2mL/h, 0.4mL/h, 0.8mL/h, 1.0mL/h; Carry out electricity and spin, obtain the PVP-FF composite nano-fiber membrane;
(5) film of collecting is put into more than the dry 24h of vacuum desiccator, subsequent use.
The electromicroscopic photograph of PVP/FF composite nano-fiber membrane and flow velocity are as shown in Figure 3 to the influence of fibre diameter.The diameter Distribution of the PVP/FF composite nano fiber that makes under the different in flow rate is as shown in Figure 4.
Claims (5)
1. an electro-spinning is equipped with the method for polyvinylpyrrolidone/two phenylalanine composite nano-fiber membranes, comprising:
(1) polyvinylpyrrolidone and two phenylalanines are under agitation slowly joined methyl alcohol and N, in the mixed solvent of N-methylacetamide, continue to stir 20～30min to complete swelling; At 25 ± 2 ℃, vibration 15～24h is to dissolving fully then, and the polymer solution that obtains is transparence, and sonicated 15min outgases, and obtains spinning solution;
(2) adopt above-mentioned spinning solution to carry out electrostatic spinning, obtain film, last vacuumize promptly gets.
2. a kind of electro-spinning according to claim 1 is equipped with the method for polyvinylpyrrolidone/two phenylalanine composite nano-fiber membranes, it is characterized in that: methyl alcohol and N in the described mixed solvent of step (1), the volume ratio of N-methylacetamide is 85:15.
3. a kind of electro-spinning according to claim 1 is equipped with the method for polyvinylpyrrolidone/two phenylalanine composite nano-fiber membranes, it is characterized in that: the mass ratio of two phenylalanines and polyvinylpyrrolidone is at 1:100～50:100 in the spinning solution that step (1) obtains.
4. a kind of electro-spinning according to claim 1 is equipped with the method for polyvinylpyrrolidone/two phenylalanine composite nano-fiber membranes; It is characterized in that: the syringe specification is 5mL in the described electrostatic spinning of step (2); The syringe needle internal diameter is 0.4 ~ 0.7mm; Receiving screen adopts the reception of aluminium foil ground connection, and the distance of syringe needle and receiving screen is 20～25cm.
5. a kind of electro-spinning according to claim 1 is equipped with the method for polyvinylpyrrolidone/two phenylalanine composite nano-fiber membranes, it is characterized in that: the ejection flow velocity is 0.1～1.0mL/h in the described electrostatic spinning process of step (2).
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070272901A1 (en) * | 2005-12-09 | 2007-11-29 | Pelagia-Irene Gouma | Poly-vinylpyrrolidone electrospun composites and Bio-composite sensing materials |
| CN101327182A (en) * | 2008-07-25 | 2008-12-24 | 东华大学 | Preparation of nano crystal fibre felt of water-insoluble medicament |
| CN101703493A (en) * | 2009-12-03 | 2010-05-12 | 东华大学 | Electrospinning composite nanofiber membrane of medicament ferulic acid, preparation method and application thereof |
| JP2010126856A (en) * | 2008-11-28 | 2010-06-10 | Sumitomo Seika Chem Co Ltd | Iodine-containing microfiber |
| CN102068339A (en) * | 2010-12-03 | 2011-05-25 | 北京化工大学 | Preparation method of biodegradable nanofiber medical dressing loaded with medicine |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070272901A1 (en) * | 2005-12-09 | 2007-11-29 | Pelagia-Irene Gouma | Poly-vinylpyrrolidone electrospun composites and Bio-composite sensing materials |
| CN101327182A (en) * | 2008-07-25 | 2008-12-24 | 东华大学 | Preparation of nano crystal fibre felt of water-insoluble medicament |
| JP2010126856A (en) * | 2008-11-28 | 2010-06-10 | Sumitomo Seika Chem Co Ltd | Iodine-containing microfiber |
| CN101703493A (en) * | 2009-12-03 | 2010-05-12 | 东华大学 | Electrospinning composite nanofiber membrane of medicament ferulic acid, preparation method and application thereof |
| CN102068339A (en) * | 2010-12-03 | 2011-05-25 | 北京化工大学 | Preparation method of biodegradable nanofiber medical dressing loaded with medicine |
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