CN103088442A - Preparation method of hollow fiber in coaxial electrostatic spinning - Google Patents
Preparation method of hollow fiber in coaxial electrostatic spinning Download PDFInfo
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- CN103088442A CN103088442A CN2013100243422A CN201310024342A CN103088442A CN 103088442 A CN103088442 A CN 103088442A CN 2013100243422 A CN2013100243422 A CN 2013100243422A CN 201310024342 A CN201310024342 A CN 201310024342A CN 103088442 A CN103088442 A CN 103088442A
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Abstract
The invention discloses a preparation method of hollow fiber in coaxial electrostatic spinning. The method includes a first step of selecting synthetic macromolecule and enabling the synthetic macromolecule to be solved in solution and stirred until the synthetic macromolecule is completely solved according to prepared final fiber, and a second step of using the solution obtained in the first step as outer pipe spinning liquid which is injected into an outer pipe of a coaxial spinning nozzle, ventilating air into an inner pipe and conducting the coaxial electrostatic spinning under the condition of room temperature. The prepared fiber is in an obvious hollow structure and can be applied to the medical field of drug carriers, artificial dialysis and the like. The preparation method of the hollow fiber in the coaxial electrostatic spinning has the advantages of being simple and convenient to operate, temperate in reaction condition, low in cost, and capable of being completed just by one step without need of using inner layer materials and subsequent processing, greatly saving time and material cost, meanwhile avoiding influences of the remained inner layer materials on the hollow fiber and having good application prospect.
Description
Technical field
The present invention relates to the preparation method in doughnut field, particularly, what relate to is a kind of method that coaxial electrostatic spinning prepares doughnut.
Background technology
Electrostatic spinning technique can prepare diameter at the fiber of tens nanometers to several microns, fibre diameter is controlled, has larger specific area, show good functional characteristic, and due to its simple experimental provision, lower cost, higher output, be easy to the advantages such as control, caused for many years researchers' very big interest.
Compare with the solid fibers of single structure, the one dimension fibre with hollow structure has unique advantage in many aspects, as drug targeting release, catalysis, separation, sensing and microfluid pipeline etc.Therefore, the preparation of doughnut is significant.The researcher utilizes the method for electrostatic spinning to prepare doughnut mainly by the fibrous template method before, utilize the fiber that electrostatic spinning makes to be template, at fiber surface self-assembling function material, then the stratum nucleare material is removed, obtain corresponding doughnut, but this method is comparatively loaded down with trivial details, pass through the processes such as electrostatic spinning, self assembly, removing template.Therefore, people have developed the coaxial electrostatic spinning method with the preparation doughnut.
2002, Loscertales etc. proposed a kind of a kind of coaxial electrostatic sprayer unit that jointly is comprised of two different capillaries of thickness, can step preparation microcapsules.(Loscertales I, Barrero A, Guerrero I, et al.Science, 2002,295:1695) subsequently, some seminar arrive the electrostatic spinning system with this technological expansion, be called coaxial electrostatic spinning (coaxial electrospinning), carried out a series of activities in this brand-new field, prepared micro-nano mitron and the core-shell structure fiber of various different materials.
After making the nucleocapsid structure fiber with the coaxial electrostatic spinning method, optionally remove the stratum nucleare material by the method for extraction or high-temperature calcination, can obtain corresponding doughnut.
Dan Li etc. the earliest with coaxial electrostatic spinning prepared doughnut (Li D, Xia Y N.Nano Lett, 2004,4:933).They adopt the ethanolic solution of PVP (PVP) and metatitanic acid isopropyl alcohol ester as outer fluid, mineral oil is as inner fluid, obtained the nucleocapsid structure fiber by coaxial electrostatic spinning, the mineral oil of stratum nucleare is removed in extraction through octane, obtain containing the composite hollow fibre of PVP and metatitanic acid isopropyl alcohol ester, pass through again high-temperature calcination, remove PVP and mineral oil composition in composite fibre, obtain diameter less than the titanium dioxide hollow fiber of 500 nanometers.
Application number is that the Chinese invention patent of CN201210172307.0 discloses a kind of method that coaxial electrostatic spinning prepares polyacrylonitrile-radical porous hollow carbon fiber, and the method comprises the following steps: with polyacrylonitrile and additives mixed, be outer solution; Getting internal layer polymer is internal layer solution; Outer solution and internal layer solution are input to respectively skin and the internal layer of coaxial syringe needle with constant flow velocity and velocity ratio, carry out electrostatic spinning, obtain PAN base core-skin composite fiber; After the washing of PAN base core-skin composite fiber, pre-oxidation and carbonization, obtain hole, PAN Quito hollow carbon fiber.
Although this method can prepare doughnut, but its operating procedure is relatively complicated, need two kinds of different solution of preparation respectively as shell solution and stratum nucleare solution, also need the steps such as follow-up washing, extraction, calcining to remove the stratum nucleare material through after coaxial electrostatic spinning, to obtain the fiber of hollow structure.The material of stratum nucleare can not be removed sometimes fully simultaneously, and remaining stratum nucleare material may exert an influence to the performance of doughnut.
Summary of the invention
For defective of the prior art, the purpose of this invention is to provide a kind of method that coaxial electrostatic spinning prepares doughnut, the method is easy and simple to handle, and reaction condition is gentle, and is with low cost; The fiber of gained has hollow structure, can be applicable to the fields such as pharmaceutical carrier and hemodialysis.
A kind of coaxial electrostatic spinning of the present invention prepares the method for doughnut, comprises the steps:
(1) choose synthetic high polymer according to the final fiber of preparation and be dissolved in solvent, be stirred to dissolving fully, obtain the uniform solution that mass fraction is 2%-20%;
(2) solution that above-mentioned steps (1) is made injects the outer tube of coaxial spinning head as the outer tube spinning solution, and blowing air enters inner tube, carries out at ambient temperature coaxial electrostatic spinning.
Preferably, described coaxial electrostatic spinning, spinning parameter is: diameter of inner pipe is 0.2-1mm, and outer tube diameter is 1-2mm, and the flow velocity of inner tube air is 0.2-1mL/h, and the flow velocity of outer tube solution is 0.5-1.5mL/h, and voltage is 7-30kV, and receiving range is 5-30cm.
Synthetic high polymer of the present invention is that the needs of final fiber according to preparation design, to coordinate specific function.The present invention utilize synthetic high polymer have physicochemical property adjustable controlled, quality stability good, low price, in biomedical sector application preferably.Preferably, the synthetic high polymer in described step (1) is one or more the mixture in polyglycolic acid, PLA, polycaprolactone, aliphatic polyester copolymer, poly-para-dioxanone, poly-beta-hydroxyalkanates, polyamide, Merlon, polyurethane, poly phosphazene, polyethylene glycol oxide, polyvinyl alcohol, polyacrylic acid, polyacrylamide, PVP, hydroxypropyl cellulose.
Preferably, the solvent in described step (1) is one or more the mixture in carrene, chloroform, oxolane, DMF, trifluoroethanol, hexafluoroisopropanol, formic acid, acetic acid, methyl alcohol, ethanol, acetone, water.
The fiber of the present invention's preparation is the synthetic high polymer fiber with hollow structure.
The fibre diameter of the present invention's preparation is 100-3000nm.
Coaxial spinning head of the present invention is assembled in the sleeve pipe mode by two different metal-made capillaries of inside and outside footpath.
The present invention's method for preparing doughnut with coaxial electrostatic spinning different from the past can a step prepare doughnut, need to not carry out subsequent treatment after spinning.In the process of spinning, do not add any solution in inner layer pipe, but allow syringe pump promote the interior air movement of pipe with constant speed, under the double action of air draught and high voltage electric field, make the liquid that sprays from outer jet pipe form concentrically ringed structure, through processes such as injection, stretching, splitting, curing, solvent evaporates, form at last doughnut in electrostatic field.
The present invention is by passing into air at internal layer, can solve the problem that spinning head stops up, play the effect of stablizing volatile polymer solution, by controlling gas flow rate, can control the spinning pattern from fiber to catenate conversion in the situation that do not change other parameters simultaneously.This fiber that has simultaneously hollow and a beading pattern has good application prospect in the pharmaceutical carrier field.By adjustments of gas temperature and flow velocity, can also realize the electrostatic spinning of the polymer that some viscositys are larger.
Compared with prior art, the present invention has following beneficial effect:
(1) preparation method of the present invention is easy and simple to handle, reaction condition is gentle, with low cost;
(2) doughnut of the present invention's preparation only needs can complete once going on foot, and does not need to use inner layer material, also need not subsequent treatment, has greatly saved the time and materials cost, has also avoided residual inner layer material on the impact of doughnut simultaneously;
(3) doughnut of the present invention's preparation can regulate and control its structure and size easily, can be suitable in various field.
The specific embodiment
The present invention is described in detail below in conjunction with specific embodiment.Following examples will help those skilled in the art further to understand the present invention, but not limit in any form the present invention.Should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, can also make some distortion and improvement.These all belong to protection scope of the present invention.
Embodiment 1
(1) polycaprolactone of molecular weight 150,000 being dissolved in volume ratio is in the carrene, DMF mixed solvent of 4: 1, is made into mass fraction and is 8% solution;
(2) solution that above-mentioned steps (1) is made injects the outer tube of coaxial spinning head as the outer tube spinning solution, and blowing air enters inner tube, carries out at ambient temperature coaxial electrostatic spinning.Spinning parameter is: the flow velocity of inner tube air is 0.2mL/h, and the flow velocity of outer tube solution is 1mL/h, and voltage is 15kV, and receiving range is 15cm.
In the present embodiment, the inside/outside footpath of the inner tube of coaxial spinning head is respectively 0.5/0.7mm, and the inside/outside footpath of outer tube is respectively 1.2/2mm.
Prepared fibre diameter is the polycaprolactone nanofiber with hollow structure of 130-370nm.
Embodiment 2
(1) with the PLGA(50/50 of molecular weight 70,000) to be dissolved in volume ratio be in the oxolane/DMF mixed solvent of 3: 1, is made into mass fraction and is 18% solution;
(2) solution that above-mentioned steps (1) is made injects the outer tube of coaxial spinning head as the outer tube spinning solution, and blowing air enters inner tube, carries out at ambient temperature coaxial electrostatic spinning.Spinning parameter is: the flow velocity of inner tube air is 0.2mL/h, and the flow velocity of outer tube solution is 0.8mL/h, and voltage is 15kV, and receiving range is 15cm.
In the present embodiment, the inside/outside footpath of the inner tube of coaxial spinning head is respectively 0.5/0.7mm, and the inside/outside footpath of outer tube is respectively 1.2/2mm.
Prepared fibre diameter is the PLGA nanofiber with hollow structure of 150-225nm.
Embodiment 3
(1) PVP with molecular weight 300,000 is dissolved in alcohol solvent, is made into mass fraction and is 10% solution;
(2) solution that above-mentioned steps (1) is made injects the outer tube of coaxial spinning head as the outer tube spinning solution, and blowing air enters inner tube, carries out at ambient temperature coaxial electrostatic spinning.Spinning parameter is: the flow velocity of inner tube air is 0.4mL/h, and the flow velocity of outer tube solution is 1mL/h, and voltage is 15kV, and receiving range is 10cm.
In the present embodiment, the inside/outside footpath of the inner tube of coaxial spinning head is respectively 0.5/0.7mm, and the inside/outside footpath of outer tube is respectively 1.2/2mm.
Prepared fibre diameter is the PVP micrometer fibers with hollow structure of 2000-3000nm.
Embodiment 4
(1) PLLA of molecular weight 100,000 being dissolved in volume ratio is in the carrene/DMF mixed solvent of 1: 4, is made into mass fraction and is 9% solution;
(2) solution that above-mentioned steps (1) is made injects the outer tube of coaxial spinning head as the outer tube spinning solution, and blowing air enters inner tube, carries out at ambient temperature coaxial electrostatic spinning.Spinning parameter is: the flow velocity of inner tube air is 0.2mL/h, and the flow velocity of outer tube solution is 0.5mL/h, and voltage is 30kV, and receiving range is 30cm.
In the present embodiment, the inside/outside footpath of the inner tube of coaxial spinning head is respectively 0.5/0.7mm, and the inside/outside footpath of outer tube is respectively 1.2/2mm.
Prepared fibre diameter is the PLLA micro nanometer fiber with hollow structure of 700-1400nm.
Embodiment 5
(1) poly-para-dioxanone is dissolved in the hexafluoroisopropanol solvent, is made into mass fraction and is 2.55% solution;
(2) solution that above-mentioned steps (1) is made injects the outer tube of coaxial spinning head as the outer tube spinning solution, and blowing air enters inner tube, carries out at ambient temperature coaxial electrostatic spinning.Spinning parameter is: the flow velocity of inner tube air is 0.5mL/h, and the flow velocity of outer tube solution is 0.8mL/h, and voltage is 10kV, and receiving range is 15cm.
In the present embodiment, the inside/outside footpath of the inner tube of coaxial spinning head is respectively 0.5/0.7mm, and the inside/outside footpath of outer tube is respectively 1.2/2mm.
Prepared fibre diameter is the poly-para-dioxanone nanofiber with hollow structure of 100-450nm.
Embodiment 6
(1) the biconjugate methylenedioxy phenoxy is replaced poly phosphazene and be dissolved in chloroform solvent, be made into mass fraction and be 8% solution;
(2) solution that above-mentioned steps (1) is made injects the outer tube of coaxial spinning head as the outer tube spinning solution, and blowing air enters inner tube, carries out at ambient temperature coaxial electrostatic spinning.Spinning parameter is: the flow velocity of inner tube air is 1mL/h, and the flow velocity of outer tube solution is 1.5mL/h, and voltage is 20kV, and receiving range is 20cm.
In the present embodiment, the inside/outside footpath of the inner tube of coaxial spinning head is respectively 0.5/0.7mm, and the inside/outside footpath of outer tube is respectively 1.2/2mm.
Prepared fibre diameter is the biconjugate methylenedioxy phenoxy substituted polyphosphazene with hollow structure of 1400-1600nm.
As can be seen from the above embodiments, coaxial electrostatic spinning of the present invention prepares the method for doughnut, by preparation synthetic high polymer solution, synthetic high polymer solution is injected the outer tube of coaxial spinning head, blowing air enters inner tube, carries out at ambient temperature coaxial electrostatic spinning.As outflow, air can a step prepare the fiber with hollow structure as interior stream with synthetic high polymer solution in the present invention, do not need to use inner layer material, need not subsequent treatment, can greatly save time and material cost, also avoid residual inner layer material on the impact of doughnut simultaneously.The present invention is easy and simple to handle, and reaction condition is gentle, and is with low cost; The synthetic high polymer fiber of gained has hollow structure, can be applicable to the fields such as pharmaceutical carrier and hemodialysis.
Above specific embodiments of the invention are described.It will be appreciated that, the present invention is not limited to above-mentioned specific implementations, and those skilled in the art can make various distortion or modification within the scope of the claims, and this does not affect flesh and blood of the present invention.
Claims (6)
1. a coaxial electrostatic spinning prepares the method for doughnut, it is characterized in that comprising the steps:
(1) choose synthetic high polymer according to the final fiber of preparation and be dissolved in solvent, be stirred to dissolving fully, obtain the uniform solution that mass fraction is 2%-20%;
(2) solution that above-mentioned steps (1) is made is as the outer tube spinning solution, inject the outer tube of coaxial spinning head, blowing air enters inner tube, carry out at ambient temperature coaxial electrostatic spinning, spinning parameter is: diameter of inner pipe is 0.2-1mm, and outer tube diameter is 1-2mm, the flow velocity of inner tube air is 0.2-1mL/h, the flow velocity of outer tube solution is 0.5-1.5mL/h, and voltage is 7-30kV, and receiving range is 5-30cm.
2. a kind of coaxial electrostatic spinning according to claim 1 prepares the method for doughnut, it is characterized in that: the synthetic high polymer in described step (1) is one or more the mixture in polyglycolic acid, PLA, polycaprolactone, aliphatic polyester copolymer, poly-para-dioxanone, poly-beta-hydroxyalkanates, polyamide, Merlon, polyurethane, poly phosphazene, polyethylene glycol oxide, polyvinyl alcohol, polyacrylic acid, polyacrylamide, PVP, hydroxypropyl cellulose.
3. a kind of coaxial electrostatic spinning according to claim 1 and 2 prepares the method for doughnut, it is characterized in that: the solvent in described step (1) is one or more the mixture in carrene, chloroform, oxolane, DMF, trifluoroethanol, hexafluoroisopropanol, formic acid, acetic acid, methyl alcohol, ethanol, acetone, water.
4. a kind of coaxial electrostatic spinning according to claim 1 and 2 prepares the method for doughnut, it is characterized in that: the fiber of preparation is the synthetic high polymer fiber with hollow structure.
5. a kind of coaxial electrostatic spinning according to claim 4 prepares the method for doughnut, it is characterized in that: described fibre diameter is 100nm-3000nm.
6. a kind of coaxial electrostatic spinning according to claim 1 and 2 prepares the method for doughnut, it is characterized in that: described coaxial spinning head is assembled in the sleeve pipe mode by two different metal-made capillaries of inside and outside footpath.
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Application publication date: 20130508 |