CN104213331A - Preparation method of electrostatic spinning polylactic acid nano-pore fiber membrane - Google Patents

Preparation method of electrostatic spinning polylactic acid nano-pore fiber membrane Download PDF

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Publication number
CN104213331A
CN104213331A CN201410468060.6A CN201410468060A CN104213331A CN 104213331 A CN104213331 A CN 104213331A CN 201410468060 A CN201410468060 A CN 201410468060A CN 104213331 A CN104213331 A CN 104213331A
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China
Prior art keywords
polylactic acid
preparation
fiber membrane
syringe
spinning
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Pending
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CN201410468060.6A
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Chinese (zh)
Inventor
徐志伟
李显华
吴腾飞
钱晓明
田旭
滕堃玥
买巍
单明景
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Tianjin Polytechnic University
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Tianjin Polytechnic University
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Priority to CN201410468060.6A priority Critical patent/CN104213331A/en
Publication of CN104213331A publication Critical patent/CN104213331A/en
Pending legal-status Critical Current

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Abstract

The invention discloses a preparation method of a polylactic acid nano-pore fiber membrane. The method comprises the following steps: dissolving polylactic acid particles for use in electrostatic spinning into a single-component solvent; receiving the fiber membrane by adopting a water bath receiving groove; preparing the polylactic acid fiber membrane having a nano-pore structure by means of a phase conversion principle. The preparation method is easy to operate, is low in cost, is mild in implementation condition, and can be implemented at the conventional humidity. A single fiber of the polylactic acid nano-pore fiber membrane can present a porous structure of which the pore diameter ranges from dozens of nanometers to hundreds of nanometers. The nano-pore fiber membrane has the characteristics of high porosity and large specific surface area, so that the application range of the polylactic acid fiber membrane is expanded greatly.

Description

The preparation method of a kind of Static Spinning polylactic acid nano hole tunica fibrosa
Technical field
The invention belongs to electrostatic spinning technique field, particularly the preparation method of a kind of Static Spinning polylactic acid nano hole tunica fibrosa.
Background technology
Electrostatic spinning technique is proposed first in 1934 by Formhals.This technology is sprayed from spout under the effect of high-voltage electrostatic field polymer solution or melt, form stable thread, then solvent evaporates or melt cooling, fiber is tapered, finally collect on the reception device and solidify, forming the thin layer of the disorderly and unsystematic arrangement of superfine fibre.Its core makes the flow deformation drawing-off in the electric field of charged polymer solution or melt, and then cooling curing, obtains fibrous material.
In recent years, existing many scholars use electrostatic spinning technique successfully to prepare the nanofiber of various structures, especially achieve remarkable result preparing in porous fibre.But the method preparing Static Spinning porous fibre is at present roughly divided into two kinds: a kind of method is under the condition of higher levels of humidity, the difference of two component solvent evaporates speed is utilized to produce porous: another kind of method two kinds of polymer is dissolved in same solvent carry out spinning, washes wherein a kind of composition after film forming again off.Though these two kinds of methods are simple, come with some shortcomings, such as, first method is higher to humidity requirement, and humidity is crossed conference to spinning effect and produced certain influence, therefore often cannot spin the good porous fibre of pattern.Two part solvent or double focusing compound is selected to carry out spinning, the dissolubility of double focusing compound in same solvent (or polymer is at two part solvent) should be considered, also to consider each material rate of volatilization in spinning process simultaneously, otherwise many kinds of substance can be caused to disperse inequality in the solution, and then affect fibre fineness and become silk effect.
Summary of the invention
In order to solve the problem, the preparation method of the Static Spinning polylactic acid nano hole tunica fibrosa of one-component solvent is used under the object of the present invention is to provide a kind of normal humidity environment, the method can spin the good porous fibre of pattern in the environment of traditional humidity, and operation is simple.
The present invention is the preparation method of a kind of Static Spinning polylactic acid nano hole fiber, comprise: the particles of polylactic acid being used for electrostatic spinning is dissolved in the solvent of one-component, then adopt water-bath receiving slit to receive tunica fibrosa, it is the tens Static Spinning polylactic acid nano hole tunica fibrosas arriving hundreds of nano aperture structure that final dependence inversion of phases principle successfully prepares aperture.Its concrete operation step is as follows:
(1) in syringe, add the certain density PLA spinning solution prepared;
(2) be connected with syringe needle by high-voltage power cathode, negative pole connects with one end of water-bath receiving slit, simultaneously by water-bath receiving slit ground connection;
(3) open high voltage source, in addition appropriate voltage, open syringe pump simultaneously, with suitable speed, spinning solution is extruded, form tunica fibrosa.
Solvent in described PLA spinning solution is selected from the one in chloroform, carrene.
The mass concentration of described PLA spinning solution is 8 ~ 10%.
The voltage that described high voltage source applies is 10 ~ 30kV, and the fltting speed of syringe pump is 1 ~ 5ml/h.
Advantage of the present invention: (1) adopts water-bath receiving slit to receive tunica fibrosa, can realize the uncontrolled requirement of humidity; (2) adopt one-component solvent to carry out spinning, cost is low, simple to operate; (3) the method a step can obtain Static Spinning polylactic acid nano hole tunica fibrosa, and it is tens pore space structures arriving hundreds of nanometer that obtained tunica fibrosa can present aperture on single fiber.
Detailed description of the invention
Technical solution of the present invention is not limited to following cited specific embodiments, and the scope of its optional parameters is comparatively wide, can be enumerate in instantiation, also can choose other parameters and carry out spinning.Below some concrete embodiments:
Embodiment 1:
First prepare PLA solution, for dichloromethane solvent, measure 68.4ml carrene, then add 9g PLA, and magnetic agitation 2h.
After preparation of spinning solution completes, added by spinning solution in syringe, be placed on below syringe simultaneously by water-bath receiving slit, then unlatching high voltage source and syringe pump start electrostatic spinning.The each technological parameter of electrostatic spinning: temperature 25 DEG C, humidity 20%, concentration of dope 9%, voltage 20kV, receiving range 10cm, syringe pump fltting speed 2ml/h.Static Spinning polylactic acid nano hole tunica fibrosa is obtained through drying after spinning terminates.
Embodiment 2:
First prepare PLA solution, for dichloromethane solvent, measure 69.1ml carrene, then add 8g PLA, and magnetic agitation 1h.
After preparation of spinning solution completes, added by spinning solution in syringe, be placed on below syringe simultaneously by water-bath receiving slit, then unlatching high voltage source and syringe pump start electrostatic spinning.The each technological parameter of electrostatic spinning: temperature 20 DEG C, humidity 25%, concentration of dope 8%, voltage 25kV, receiving range 5cm, syringe pump fltting speed 3ml/h.Static Spinning polylactic acid nano hole tunica fibrosa is obtained through drying after spinning terminates.
Embodiment 3:
First prepare PLA solution, for chloroform solvent, measure 60.4ml carrene, then add 10g PLA, and magnetic agitation 3h.
After preparation of spinning solution completes, added by spinning solution in syringe, be placed on below syringe simultaneously by water-bath receiving slit, then unlatching high voltage source and syringe pump start electrostatic spinning.The each technological parameter of electrostatic spinning: temperature 23 DEG C, humidity 30%, concentration of dope 10%, voltage 10kV, receiving range 15cm, syringe pump fltting speed 1ml/h.Static Spinning polylactic acid nano hole tunica fibrosa is obtained through drying after spinning terminates.

Claims (5)

1. a preparation method for Static Spinning polylactic acid nano hole tunica fibrosa, the preparation facilities adopted comprises syringe, syringe pump, water-bath receiving slit and high voltage source.It is characterized in that comprising the following steps:
1) particles of polylactic acid being used for electrostatic spinning is dissolved in the solvent of one-component;
2) open high voltage source, apply appropriate voltage, open the syringe pump be connected with syringe simultaneously, with the PLA spinning solution in suitable speed pushing syringe, on the surface of water-bath receiving slit, finally form the polylactic acid fiber membrane with nano-pore structure.
2. preparation method according to claim 1, is characterized in that: the solvent in described PLA spinning solution is selected from the one in chloroform, carrene.
3. preparation method according to claim 1, is characterized in that: the mass concentration of described PLA spinning solution is 8 ~ 10%.
4. preparation method according to claim 1, is characterized in that: described from syringe needle to the distance of water-bath receiving slit be 10 ~ 15cm.
5. preparation method according to claim 1, is characterized in that: the voltage that described high voltage source applies is 10 ~ 30kV, and the fltting speed of syringe pump is 1 ~ 5ml/h.
CN201410468060.6A 2014-09-12 2014-09-12 Preparation method of electrostatic spinning polylactic acid nano-pore fiber membrane Pending CN104213331A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105506862A (en) * 2016-01-29 2016-04-20 哈尔滨理工大学 Preparation method for sandwich type medical stone/polymer composite film

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101401955A (en) * 2008-11-14 2009-04-08 南京大学医学院附属鼓楼医院 Method for producing nano-fibre bracket material with levorotation polylactic acid as base material
CN101748560A (en) * 2009-12-11 2010-06-23 江南大学 Spinning method of electrostatically spun composite material of multiple nano level holes
CN102517673A (en) * 2011-11-23 2012-06-27 浙江大学 Method for preparing polymer porous nanofiber through mixed phase separation
CN102926135A (en) * 2011-08-09 2013-02-13 东丽纤维研究所(中国)有限公司 Biodegradable composite superfine fiber non-woven fabric and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101401955A (en) * 2008-11-14 2009-04-08 南京大学医学院附属鼓楼医院 Method for producing nano-fibre bracket material with levorotation polylactic acid as base material
CN101748560A (en) * 2009-12-11 2010-06-23 江南大学 Spinning method of electrostatically spun composite material of multiple nano level holes
CN102926135A (en) * 2011-08-09 2013-02-13 东丽纤维研究所(中国)有限公司 Biodegradable composite superfine fiber non-woven fabric and preparation method thereof
CN102517673A (en) * 2011-11-23 2012-06-27 浙江大学 Method for preparing polymer porous nanofiber through mixed phase separation

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105506862A (en) * 2016-01-29 2016-04-20 哈尔滨理工大学 Preparation method for sandwich type medical stone/polymer composite film
CN105506862B (en) * 2016-01-29 2019-03-15 哈尔滨理工大学 Sandwich type medical stone/polymer composite film preparation method

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Application publication date: 20141217