CN102787375A - Coaxial electrostatic spinning method of refining fibers by using axis solvents - Google Patents
Coaxial electrostatic spinning method of refining fibers by using axis solvents Download PDFInfo
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- CN102787375A CN102787375A CN2012102465269A CN201210246526A CN102787375A CN 102787375 A CN102787375 A CN 102787375A CN 2012102465269 A CN2012102465269 A CN 2012102465269A CN 201210246526 A CN201210246526 A CN 201210246526A CN 102787375 A CN102787375 A CN 102787375A
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Abstract
The invention discloses a coaxial electrostatic spinning method of refining fibers by using axis solvents. The coaxial electrostatic spinning method comprises the following steps that high-concentration superpolymers are dissolved, ultrasonic degasification is carried out, a shell solution is obtained, then, volatile solvents are used as a core solution, the core solution is subjected to coaxial electrostatic spinning in sealed environment with the temperature being 22 to 35 DEG C and the humidity being 35 to 60 percent, and the concrete conditions of spinning are shown as follows: the voltage is 6 to 18kv, the shell flow velocity is 0.5 to 1.5mL/h, the core flow velocity is 0.1 to 1mL/h, the receiving distance from a needle to an aluminum foil is 10 to 25cm, and nanometer fibrofelt is obtained after drying for one night. The method is continuous and feasible, the operation is simple and convenient, the implementation is easy, the industrialization is easy, and higher simplicity, more time saving and higher speed are realized. The obtained nanometer fibrofelt has the thinner diameter than that of the single-axis nanometer fibers under the same spinning condition, and can be applied to the relevant fields of slow release system implantation, medicine control release, tissue engineering scaffold, bioseparation, protein separation purification, gene transfer and the like.
Description
Technical field
The invention belongs to the high polymer nanometer fiber preparation field, be specially the coaxial electrostatic spinning method of a kind of axle for the refinement fiber of solvent.
Background technology
Nanofiber has that yardstick is little, specific area is big and characteristics such as physical property excellence, has broad application prospects in fields such as microelectronics and biomedicines.Microcyst system with nanometer or submicrometer structure also can play a significant role in food additives, pharmaceutical carrier and special material processing and other fields.
Electrostatic spinning receives extensive concern as a kind of technology of high-efficiency production of nano fiber because of it conveniently obtains continuous nanofiber.1934, Formlals invented first patent about electrostatic spinning technique, detailed preparation technology who refers to method of electrostatic spinning and device for spinning; But up to the eighties in 20th century, because the rapid rising and the development of nano science, this method for preparing nanofiber has just received people's extensive concern; At the beginning of 21 century, the domestic research that has just begun electrostatic spinning, the Chinese Academy of Sciences has made nanoscale polyacrylonitrile fibre felt with method of electrostatic spinning.
In recent years, electrostatic spinning optimization research becomes focus, and after a kind of novel coaxial spinneret occurred, the skin-core structure of acquisition had been expanded the Application Areas of nanofiber.Be applied to the nanofiber of compound nanofiber of coaxial core-skin and core-skin type these biological medical domains such as slow-releasing system, medicine carrying medical dressing and tissue engineering bracket structure, suture of medicine, respond well, prospect is superior.
It is the coaxial electrostatic spinning of shell solution with the neat solvent that surplus lamp extensively waits research, can obtain smooth surface, nanofibrous structures that fibre diameter is thinner.How through more simply, more save time, method obtains thinner nanofiber mats and has also caused concern faster.Expanding thus with the solvent is axle (medicine-carried, protein, growth factor, gene etc.), and high polymer is a shell, can realize the quick preparation of the nanofiber of high concentration high polymeric solution.Coaxial electrically spun also has shortcoming: because spinneret is thicker, syringe needle has drop in the spinning process, makes that the filament that spins is thicker; And the high polymer of high concentration, spinnability is very poor, is difficult to realize the preparation of nanofiber mats.
In view of above reason, the method that this axle is the refinement coaxial electrostatic spinning of solvent prepares nanofiber mats and seems significant, and present research document and patent do not relate to a method of utilizing axle solvent controlling fiber diameter.We utilize continuous, easy relatively axle to prepare nanofiber mats for the coaxial electrostatic spinning method of the refinement fiber of solvent, more simply, more save time, quicker.
Summary of the invention
Technical problem to be solved by this invention provides a kind of axle coaxial electrostatic spinning method for the refinement fiber of solvent, and the inventive method is feasible continuously, and is easy to operation, is easy to industrialization, more simply, more save time, quicker; The nanofiber mats of gained is thinner than single shaft nanofiber diameter under the equal spinning condition, can be used for association areas such as implantation slow release system, medicine control release, tissue engineering bracket, bio-separation, protein separating purifying, gene transmission.
The present invention relates to the coaxial electrostatic spinning method of a kind of axle, comprising for the refinement fiber of solvent:
(1) high polymer is dissolved in the solvent, stirs 1-4h, ultrasonic degas obtains electrostatic spinning solution;
(2) with the spinning solution of step (1) gained as shell solution, easy volatile solvent is an axle solvent, is 22-35 ℃ in temperature, humidity is electrostatic spinning in the enclosed environment of 35-60%, carries out coaxial electrostatic spinning, obtains nanofiber mats after the dried overnight.
High polymer is a polyacrylonitrile in the described step (1), shitosan, and polypyrrole alkane ketone, dissolvings such as PLA or polylactic acid-glycolic guanidine-acetic acid have the high polymer of certain viscosity afterwards.
Solvent is a carrene in the described step (1), acetone, ethanol, formic acid, one or more in N-N dimethyl formamide or the N-N dimethylacetylamide.
The mass volume ratio of high polymer and solvent is 0.08g/mL-0.5g/mL in the described step (1).
Axle solvent in the described step (2) is a carrene, acetone, ethanol, water, formic acid, acetate, one or more in N-N dimethyl formamide or the N-N dimethylacetylamide.
Spinning actual conditions in the described step (2) is voltage: 6-18kv, shell flow velocity: 0.5-1.5mL/h, and axial flow speed: 0.1-1mL/h, syringe needle leaves the receiving range of aluminium foil: 10-25cm,
The external diameter of said syringe needle is 1-2mm, and internal diameter is 0.5-1mm, and two boost pump can be controlled different nucleocapsid flow velocitys in the spinning process.
The present invention obtains solid nanofiber, but because of the difference of shell high polymer, demonstrates the smooth perhaps nanofiber mats of porous surface again because of the volatility of shell solvent and axle solvent is different.
Beneficial effect
(1) used polymer class is originated and is enriched, and cheap, cost is lower;
(2) resulting polymers concentration is higher;
(3) the nanofiber mats diameter of gained is little, and certain toughness and mechanical strength are arranged, and specific area is big.
(4) the present invention saves time, fast, succinctly, is easy to serialization, industrialization, has further reduced cost.
(5) through regulating type of solvent and proportioning, regulating shaft solvent species and flow velocity utilize continuously simple coaxial electrostatic spinning technology, obtain the uniform nanofiber mats of different-diameter.
(6) nanofiber mats of gained is thinner than single shaft nanofiber diameter under the equal spinning condition, can be used for association areas such as implantation slow release system, medicine control release, tissue engineering bracket, bio-separation, protein separating purifying, gene transmission.
Description of drawings
Fig. 1 is the coaxial electrostatic spinning diameter comparison diagram of different solvents for axle of the present invention;
Fig. 2-9 is nanofiber mats under the different solvents of the present invention and diameter Distribution figure thereof, and shell solvent, flow velocity are constant; The axle solvent is the 2-single shaft, 3-carrene, 4-acetone, 5-ethanol, 6-water, 7-formic acid, 8-N, dinethylformamide, 9-N, N-dimethylacetylamide.
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.
With PVPK90 white solid powder 0.1g, be dissolved in the 1mL absolute alcohol, the mass volume ratio of PVPK90 and absolute alcohol is .0.1g:1mL, magnetic agitation 1h, ultrasonic degas 5min makes the single shaft spinning solution, is drawn onto in the 5mL syringe.In temperature is 22 ℃, and humidity is electrostatic spinning in 35% the enclosed environment, the spinning actual conditions: syringe needle diameter 0.9mm, and voltage 10kv, spinning solution flow velocity 1mL/h, syringe needle is 15cm from the receiving range of aluminium foil.Obtain nanofiber mats after the dried overnight.The SEM of gained nanofiber mats such as Fig. 2 a, diameter Distribution such as Fig. 2 b.
With PVPK90 white solid powder 0.1g, be dissolved in the 1mL absolute alcohol, the mass volume ratio of PVPK90 and absolute alcohol is .0.1g:1mL, magnetic agitation 1h, ultrasonic degas 5min makes shell solution, is drawn onto in the 5mL syringe.
To analyze absolute dichloromethane for the axle solvent, be drawn onto in another 5mL syringe.
The above two are placed on respectively under the different boost pumps, are 22 ℃ in temperature, and humidity is electrostatic spinning in 35% the enclosed environment, the spinning actual conditions: voltage 6kv, and shell flow velocity 0.5mL/h, axial flow speed 0.1mL/h, syringe needle is 10cm from the receiving range of aluminium foil.Obtain nanofiber mats after the dried overnight.
The SEM of gained nanofiber mats such as Fig. 3 a, diameter Distribution such as Fig. 3 b.
Embodiment 3
With PVPK90 white solid powder 0.1g, be dissolved in the 1mL absolute alcohol, the mass volume ratio of PVPK90 and absolute alcohol is .0.1g:1mL, magnetic agitation 2h, ultrasonic degas 5min makes shell solution, is drawn onto in the 5mL syringe.
To analyze pure acetone for the axle solvent, be drawn onto in another 5mL syringe.
The above two are placed on respectively under the different boost pumps, are 26 ℃ in temperature, and humidity is electrostatic spinning in 44% the enclosed environment, the spinning actual conditions: voltage 10kv, and shell flow velocity 0.8mL/h, axial flow speed 0.4mL/h, syringe needle is 15cm from the receiving range of aluminium foil.Obtain nanofiber mats after the dried overnight.
The SEM of gained nanofiber mats such as Fig. 4 a, diameter Distribution such as Fig. 4 b.
With PVPK90 white solid powder 0.1g, be dissolved in the 1mL absolute alcohol, the mass volume ratio of PVPK90 and absolute alcohol is .0.1g:1mL, magnetic agitation 3h, ultrasonic degas 5min makes shell solution, is drawn onto in the 5mL syringe.
To analyze straight alcohol for the axle solvent, be drawn onto in another 5mL syringe.
The above two are placed on respectively under the different boost pumps, are 30 ℃ in temperature, and humidity is electrostatic spinning in 53% the enclosed environment, the spinning actual conditions: voltage 14kv, and shell flow velocity 1.1mL/h, axial flow speed 0.7mL/h, syringe needle is 20cm from the receiving range of aluminium foil.Obtain nanofiber mats after the dried overnight.
The SEM of gained nanofiber mats such as Fig. 5 a, diameter Distribution such as Fig. 5 b.
To gather (lactic-co-glycolic acid) PLGA white solid powder 0.2g, and be dissolved in the 1ml absolute alcohol, the mass volume ratio of PVPK90 and absolute alcohol is .0.2g:1mL, magnetic agitation 4h, and ultrasonic degas 5min makes shell solution, is drawn onto in the 5mL syringe.
With distilled water is the axle solvent, is drawn onto in another 5mL syringe.
The above two are placed on respectively under the different boost pumps, are 35 ℃ in temperature, and humidity is electrostatic spinning in 60% the enclosed environment, the spinning actual conditions: voltage 18kv, and shell flow velocity 1.5mL/h, axial flow speed 1mL/h, syringe needle is 25cm from the receiving range of aluminium foil.Obtain nanofiber mats after the dried overnight.
The SEM of gained nanofiber mats such as Fig. 6 a, diameter Distribution such as Fig. 6 b.
To gather (lactic-co-glycolic acid) PLGA white solid powder 0.2g, and be dissolved in the 1ml absolute alcohol, the mass volume ratio of PVPK90 and absolute alcohol is .0.2g:1mL, magnetic agitation 4h, and ultrasonic degas 5min makes shell solution, is drawn onto in the 5mL syringe.
To analyze pure formic acid for the axle solvent, be drawn onto in another 5mL syringe.
The above two are placed on respectively under the different boost pumps, are 35 ℃ in temperature, and humidity is electrostatic spinning in 60% the enclosed environment, the spinning actual conditions: voltage 18kv, and shell flow velocity 1.5mL/h, axial flow speed 1mL/h, syringe needle is 25cm from the receiving range of aluminium foil.Obtain nanofiber mats after the dried overnight.
The SEM of gained nanofiber mats such as Fig. 7 a, diameter Distribution such as Fig. 7 b.
Embodiment 7
To gather (lactic-co-glycolic acid) PLGA white solid powder 0.2g, and be dissolved in the 1ml absolute alcohol, the mass volume ratio of PVPK90 and absolute alcohol is .0.2g:1mL, magnetic agitation 4h, and ultrasonic degas 5min makes shell solution, is drawn onto in the 5mL syringe.
To analyze pure N, dinethylformamide is the axle solvent, is drawn onto in another 5mL syringe.
The above two are placed on respectively under the different boost pumps, are 35 ℃ in temperature, and humidity is electrostatic spinning in 60% the enclosed environment, the spinning actual conditions: voltage 18kv, and shell flow velocity 1.5mL/h, axial flow speed 1mL/h, syringe needle is 25cm from the receiving range of aluminium foil.Obtain nanofiber mats after the dried overnight.
The SEM of gained nanofiber mats such as Fig. 8 a, diameter Distribution such as Fig. 8 b.
To gather (lactic-co-glycolic acid) PLGA white solid powder 0.2g, and be dissolved in the 1ml absolute alcohol, the mass volume ratio of PVPK90 and absolute alcohol is .0.2g:1mL, magnetic agitation 4h, and ultrasonic degas 5min makes shell solution, is drawn onto in the 5mL syringe.
To analyze pure DMAC N,N for the axle solvent, be drawn onto in another 5mL syringe.
The above two are placed on respectively under the different boost pumps, are 35 ℃ in temperature, and humidity is electrostatic spinning in 60% the enclosed environment, the spinning actual conditions: voltage 18kv, and shell flow velocity 1.5mL/h, axial flow speed 1mL/h, syringe needle is 25cm from the receiving range of aluminium foil.Obtain nanofiber mats after the dried overnight.
The SEM of gained nanofiber mats such as Fig. 9 a, diameter Distribution such as Fig. 9 b.
The nanofiber mats diameter contrast of implementing 1-8 is as shown in table 1.
Table 1
Claims (8)
1. the present invention relates to the coaxial electrostatic spinning method of a kind of axle, comprising for the refinement fiber of solvent:
(1) high polymer is dissolved in the solvent, stirs 1-4h, ultrasonic degas obtains electrostatic spinning solution;
(2) with the spinning solution of step (1) gained as shell solution, easy volatile solvent is an axle solvent, is 22-35 ℃ in temperature, humidity is electrostatic spinning in the enclosed environment of 35-60%, carries out coaxial electrostatic spinning, obtains nanofiber mats after the dried overnight.
2. a kind of axle according to claim 1 is the coaxial electrostatic spinning method of the refinement fiber of solvent, and it is characterized in that: high polymer is polyacrylonitrile, shitosan, polypyrrole alkane ketone, PLA or polylactic acid-glycolic guanidine-acetic acid in the described step (1).
3. a kind of axle according to claim 1 is the coaxial electrostatic spinning method of the refinement fiber of solvent; It is characterized in that: solvent is a carrene in the described step (1), acetone, ethanol; Formic acid, one or more in N-N dimethyl formamide or the N-N dimethylacetylamide.
4. a kind of axle according to claim 1 is the coaxial electrostatic spinning method of the refinement fiber of solvent, and it is characterized in that: the mass volume ratio of high polymer and solvent is 0.08g/mL-0.5g/mL in the described step (1).
5. a kind of axle according to claim 1 is the coaxial electrostatic spinning method of the refinement fiber of solvent, it is characterized in that: the axle solvent in the described step (2) is a carrene, acetone; Ethanol, water, formic acid; Acetate, one or more in N-N dimethyl formamide or the N-N dimethylacetylamide.
6. a kind of axle according to claim 1 is the coaxial electrostatic spinning method of the refinement fiber of solvent; It is characterized in that: the spinning actual conditions in the described step (2) is voltage: 6-18kv; Shell flow velocity: 0.5-1.5mL/h; Axial flow speed: 0.1-1mL/h, syringe needle is from the receiving range of aluminium foil: 10-25cm.
7. a kind of axle according to claim 6 is the coaxial electrostatic spinning method of the refinement fiber of solvent, and it is characterized in that: the external diameter of said syringe needle is 1-2mm, and internal diameter is 0.5-1mm.
8. a kind of axle according to claim 1 is the coaxial electrostatic spinning method of the refinement fiber of solvent, and it is characterized in that: boost pump is two in the spinning process.
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| CN106498508A (en) * | 2016-10-05 | 2017-03-15 | 桂林理工大学 | A kind of preparation method of PLA electrostatic spinning solution |
| CN108148209A (en) * | 2017-12-14 | 2018-06-12 | 浙江大学 | Based on shell pure solvent coaxial electrical spray for the method for polymer beads of the size less than 100nm |
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| CN101187093A (en) * | 2007-11-28 | 2008-05-28 | 吉林大学 | Coaxial spinning method for preparing hollow molecular sieve fiber possessing grade structure |
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| CN106498508B (en) * | 2016-10-05 | 2019-06-07 | 桂林理工大学 | A kind of preparation method of polylactic acid electrostatic spinning solution |
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Application publication date: 20121121 |