CN108517582A - A kind of degradable antibacterial nano fiber and preparation method thereof - Google Patents
A kind of degradable antibacterial nano fiber and preparation method thereof Download PDFInfo
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- CN108517582A CN108517582A CN201810328795.7A CN201810328795A CN108517582A CN 108517582 A CN108517582 A CN 108517582A CN 201810328795 A CN201810328795 A CN 201810328795A CN 108517582 A CN108517582 A CN 108517582A
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- nano fiber
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/16—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds as constituent
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/0666—Polycondensates containing five-membered rings, condensed with other rings, with nitrogen atoms as the only ring hetero atoms
- C08G73/0672—Polycondensates containing five-membered rings, condensed with other rings, with nitrogen atoms as the only ring hetero atoms with only one nitrogen atom in the ring
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/02—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from cellulose, cellulose derivatives, or proteins
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Artificial Filaments (AREA)
Abstract
The present invention discloses a kind of preparation method of degradable antibacterial nano fiber, more specifically, is to be related to a kind of using degradable polymer and indoles monomer as degradable antibacterial nano fiber of raw material and preparation method thereof, belongs to polymeric material field.This method includes following procedure：This method first vacuumizes reactor, with dry purity nitrogen gas flushing, ensures, without residual air and moisture, to add solvent and indoles monomer, continuously stirring makes indoles be completely dissolved in solvent；Then by reactor constant temperature to low temperature environment, the initiator solution for instilling certain mass carries out solution polymerization, and reaction after a certain period of time, stands 12h at room temperature；Degradable polymer is dissolved in polybenzazole nanoparticle dispersion liquid and is configured to certain density spinning solution, then electrostatic spinning is carried out under the conditions of certain technological parameter by electrospinning device, degradable antibacterial nano fiber is made after vacuum drying.Preparation method process of the present invention is simple, and prepared degradable antibacterial nano fiber has good mechanical property and excellent bactericidal property, can be used as a kind of novel degradable antibacterial nano fiber material.
Description
Technical field
The invention belongs to polymeric material fields, are related to a kind of preparation method of degradable antibacterial nano fiber, more specifically
Ground says, be related to it is a kind of using degradable polymer and indoles monomer as the degradable antibacterial nano fiber of raw material and its preparation side
Method.
Background technology
With the development of economy, this bacterium of daily life, fungi are more and more, and the influence to health is more and more tight
Weight, people increasingly increase efficient anti-biotic material demand.Nano material due to size is small, large specific surface area, surface exist it is big
Active group is measured, stronger adsorption capacity and sterilizing ability are shown to bacterium, are a kind of antibacterials having huge applications foreground
Material.Electrostatic spinning is a kind of most effectual way preparing nanofiber, it is by high-voltage electrostatic field by electrically charged polymer
Solution or melt jet stream are out prepared, to prepare the processing technology of nanofiber, average diameter range generally at several microns extremely
Between tens nanometers.Nanofiber diameter made from electrostatic spinning technique is small, large specific surface area, porosity are high, can apply
The fields such as tissue engineering bracket material, air filtration, bio-medical, sensor.
Bacteria cellulose is found for the first time by Brown 1886, can under certain condition be produced by certain bacteriums
Cellulose.Wherein most representative bacterium is acetobacter xylinum, it is a kind of rodlike gram negative strain, is particularly suitable for using
Carry out fermented-producing bacteria cellulose and yield is larger.Compared with plant cellulose, bacteria cellulose has some unique excellent
Gesture：Purity height, has biological degradability and biology at mechanical performance, good water retention property and the hydrophily that crystallinity is big, excellent
Compatibility.Its application field is very extensive, mainly has：Bio-medical, food industry, paper industry etc..Polybenzazole is that one kind contains
The heterocycle polymer of nitrogen-atoms, structure with：Polyaniline, polypyrrole are closely similar, it is with thermal stability height, oxygen in nature
The features such as change-reduction potential is high.Polybenzazole can synthesize polybenzazole by Oxoindole monomer, can also electrochemically close
At Polyindole derivatives.As conducting polymer, polybenzazole can greatly improve its electrical conductance by doping, generate sun from
Son, to have kill ability to bacterium.Polybenzazole is prepared into nanofiber, its specific surface area and surface sun can be greatly improved
Ion concentration, to greatly improve its antibacterial ability.Polybenzazole solubility is poor, it is generally mixed to progress with polymeric matrix
Electrospun nanofibers.But the dispersed phase of polybenzazole particle in a polymer matrix is poor, is easy to be formed and reunite,
And the mixed volume of polybenzazole is less, generally in 10wt% hereinafter, causing the bactericidal property of antibacterial nano fiber poor.The present invention
Using polymerisation in solution combination electrostatic spinning technique, first passes through polymerisation in solution and prepare polybenzazole nano-particle, then by degradable poly
Conjunction object, which is dissolved in polybenzazole nanoparticle dispersion liquid, forms spinning solution, then passes through electrospun nanofibers.This hair
Bright method preparation process is simple, and the ratio of nanofiber can be greatly improved up to 50wt% or more in the content of polybenzazole nano-particle
Surface area and sterilizing ability, this degradable antibacterial nano fiber can be applied in fields such as bio-medicals.
Invention content
The purpose of the present invention is using degradable polymer and indoles monomer as raw material, using polymerisation in solution combination electrostatic spinning
Technology first passes through polymerisation in solution and prepares polybenzazole nano-particle, degradable polymer is then dissolved in polybenzazole nano-particle
Spinning solution is formed in dispersion liquid, then passes through electrospun nanofibers.By adjusting solution polymerization process and Static Spinning
Silk parameter, regulates and controls the diameter of the grain size and nanofiber of polybenzazole nano-particle, makes it have good mechanical property and excellent
Bactericidal property, become a kind of novel degradable antibacterial nano fiber material.
The present invention is realized using following technical proposals.A kind of degradable antibacterial nano fiber and preparation method thereof, this method
Reactor is vacuumized first, with dry purity nitrogen gas flushing, ensures, without residual air and moisture, to add solvent and indoles list
Body, continuously stirring makes indoles be completely dissolved in solvent；Then by reactor constant temperature to low temperature environment, the initiation of certain mass is instilled
Agent solution carries out solution polymerization, and reaction after a certain period of time, stands 12h at room temperature；Degradable polymer is dissolved in poly- Yin
Certain density spinning solution is configured in diindyl nanoparticle dispersion liquid, then by electrospinning device in certain technological parameter item
Electrostatic spinning is carried out under part, and degradable antibacterial nano fiber is made after vacuum drying.
It is characterized by comprising following procedure for this method：
(1) reactor is vacuumized, is rinsed repeatedly 3 times with dry pure nitrogen gas, ensured without residual air and moisture；Indoles
Monomer uses vacuum filter, and then nitrogen seals spare after deaerating, and initiator is dissolved in solvent and is configured to initiator solution；
(2) under the conditions of stirring, nitrogen protection, solvent and indoles monomer are added in reactor, stand 30min, solvent
Dosage with indoles monomer is 1: 1~3: 1 (molar ratio)；
(3) reactor constant temperature is instilled into a certain amount of initiator solution, the use of initiator and indoles monomer to -20~0 DEG C
Amount is 0.8: 1~1.2: 1 (molar ratio), stands 8~16h of reaction；
(4) after reaction, reactor is stood into 12h at room temperature, a certain amount of degradable polymer, magnetic is then added
Power stirs 6h, is configured to the spinning solution that quality volume fraction is 2~10%；
(5) spinning solution that step (4) obtains is added in syringe, and be fixed on micro-injection pump, adopted
It is received with roller, high-pressure electrostatic 15~30kV of adjustable range, injection 0.05~0.25mL/h of flow rate pump, reception distance 15~
30cm；
(6) the degradable antibacterial nano fiber of a diameter of 200~400nm is made after being dried in vacuo.
Preparation method process of the present invention is simple, prepared degradable antibacterial nano fiber have good mechanical property and
Excellent bactericidal property can be used as a kind of novel degradable antibacterial nano fiber material.
Specific implementation mode
Embodiment 1：
Reactor is vacuumized, is rinsed repeatedly 3 times with dry pure nitrogen gas, is ensured without residual air and moisture；Indoles list
Body uses vacuum filter, and then nitrogen seals spare after deaerating, and dibenzoyl peroxide is dissolved in chloroform and is configured to draw
Send out agent solution；Under the conditions of stirring, nitrogen protection, chloroform and indoles monomer are added in reactor, stand 30min, three
The dosage of chloromethanes and indoles monomer is 1: 1 (molar ratio)；By reactor constant temperature to 0 DEG C, a certain amount of initiator solution is instilled,
The dosage of initiator and indoles monomer is 0.8: 1 (molar ratio), stands reaction 8h；After reaction, at room temperature by reactor
12h is stood, a certain amount of polyhydroxybutyrate fat is then added, magnetic agitation 6h is configured to the spinning that quality volume fraction is 2%
Solution；The spinning solution of acquisition is added in syringe, and is fixed on micro-injection pump, is connect using roller
It receives, high-pressure electrostatic adjustable range 15kV, injects flow rate pump 0.25mL/h, receive distance 15cm；It is made after vacuum drying a diameter of
The degradable antibacterial nano fiber of 400nm.
Embodiment 2：
Reactor is vacuumized, is rinsed repeatedly 3 times with dry pure nitrogen gas, is ensured without residual air and moisture；Indoles list
Body uses vacuum filter, and then nitrogen seals spare after deaerating, and fine be dissolved in tetrafluoro isopropanol of two isobutyl of azo is configured to draw
Send out agent solution；Under the conditions of stirring, nitrogen protection, tetrafluoro isopropanol and indoles monomer are added in reactor, stand 30min,
The dosage of tetrafluoro isopropanol and indoles monomer is 2: 1 (molar ratios)；By reactor constant temperature to -5 DEG C, a certain amount of initiator is instilled
The dosage of solution, initiator and indoles monomer is 1: 1 (molar ratio), stands reaction 12h；After reaction, by reactor in room
Temperature is lower to stand 12h, and a certain amount of polylactic acid is then added, and it is molten to be configured to the spinning that quality volume fraction is 4% by magnetic agitation 6h
Liquid；The spinning solution of acquisition is added in syringe, and is fixed on micro-injection pump, is received using roller,
High-pressure electrostatic adjustable range 20kV injects flow rate pump 0.15mL/h, receives distance 20cm；It is made after vacuum drying a diameter of
The degradable antibacterial nano fiber of 340nm.
Embodiment 3：
Reactor is vacuumized, is rinsed repeatedly 3 times with dry pure nitrogen gas, is ensured without residual air and moisture；Indoles list
Body uses vacuum filter, then seals spare after nitrogen degassing, dissolves ammonium persulfate into deionized water that be configured to initiator molten
Liquid；Under the conditions of stirring, nitrogen protection, tetrahydrofuran and indoles monomer are added in reactor, stand 30min, tetrahydrofuran
Dosage with indoles monomer is 3: 1 (molar ratios)；By reactor constant temperature to -20 DEG C, a certain amount of initiator solution is instilled, is caused
The dosage of agent and indoles monomer is 1.2: 1 (molar ratios), stands reaction 16h；After reaction, reactor is stood at room temperature
12h, is then added a certain amount of polycaprolactone, and magnetic agitation 6h is configured to the spinning solution that quality volume fraction is 6%；It will
The spinning solution of acquisition is added in syringe, and is fixed on micro-injection pump, is received using roller, and high pressure is quiet
Electric adjustable range 30kV injects flow rate pump 0.05mL/h, receives distance 30cm；Obtained a diameter of 200nm's can after vacuum drying
Degradation antimicrobial nanofiber.
Embodiment 4：
Reactor is vacuumized, is rinsed repeatedly 3 times with dry pure nitrogen gas, is ensured without residual air and moisture；Indoles list
Body uses vacuum filter, and then nitrogen seals spare after deaerating, and iron chloride is dissolved in deionized water and is configured to initiator solution；
Under the conditions of stirring, nitrogen protection, dimethylformamide and indoles monomer are added in reactor, stand 30min, dimethyl methyl
The dosage of amide and indoles monomer is 1.5: 1 (molar ratios)；By reactor constant temperature to -10 DEG C, it is molten to instill a certain amount of initiator
The dosage of liquid, initiator and indoles monomer is 1.1: 1 (molar ratios), stands reaction 14h；After reaction, by reactor in room
Temperature is lower to stand 12h, and a certain amount of cellulose is then added, and magnetic agitation 6h is configured to the spinning that quality volume fraction is 10%
Solution；The spinning solution of acquisition is added in syringe, and is fixed on micro-injection pump, is connect using roller
It receives, high-pressure electrostatic adjustable range 25kV, injects flow rate pump 0.01mL/h, receive distance 25cm；It is made after vacuum drying a diameter of
The degradable antibacterial nano fiber of 250nm.
Claims (6)
1. a kind of degradable antibacterial nano fiber, it is characterized in that, it is passed through using degradable polymer and indoles monomer as raw material
What polymerisation in solution and electrostatic spinning were prepared.
2. a kind of degradable antibacterial nano fiber and preparation method thereof, it is characterized in that it includes the following steps：
(1) reactor is vacuumized, is rinsed repeatedly 3 times with dry pure nitrogen gas, ensured without residual air and moisture；Indoles monomer
It using vacuum filter, then seals spare after nitrogen degassing, initiator is dissolved in solvent and is configured to initiator solution；
(2) under the conditions of stirring, nitrogen protection, solvent and indoles monomer are added in reactor, stand 30min, solvent and Yin
The dosage of diindyl monomer is 1: 1~3: 1 (molar ratio)；
(3) reactor constant temperature is instilled into a certain amount of initiator solution, the dosage of initiator and indoles monomer is to -20~0 DEG C
0.8: 1~1.2: 1 (molar ratio) stands 8~16h of reaction；
(4) after reaction, reactor is stood into 12h at room temperature, a certain amount of degradable polymer is then added, magnetic force stirs
6h is mixed, the spinning solution that quality volume fraction is 2~10% is configured to；
(5) spinning solution that step (4) obtains is added in syringe, and be fixed on micro-injection pump, using rolling
Cylinder is received, high-pressure electrostatic 15~30kV of adjustable range, injection 0.05~0.25mL/h of flow rate pump, and reception distance 15~
30cm；
(6) the degradable antibacterial nano fiber of a diameter of 200~400nm is made after being dried in vacuo.
3. a kind of degradable antibacterial nano fiber according to claim 2 and preparation method thereof, it is characterized in that：Described draws
Hair agent is one kind in fine two isobutyl of azo, ammonium persulfate, benzoyl peroxide, iron chloride.
4. a kind of degradable antibacterial nano fiber according to claim 2 and preparation method thereof, it is characterized in that：Described draws
Hair agent solvent is one kind in deionized water, chloroform, tetrafluoro isopropanol.
5. a kind of degradable antibacterial nano fiber according to claim 2 and preparation method thereof, it is characterized in that：The Yin
Diindyl solvent is one kind in chloroform, tetrafluoro isopropanol, tetrahydrofuran, dimethylformamide.
6. a kind of degradable antibacterial nano fiber according to claim 2 and preparation method thereof, it is characterized in that：Described can
Degradation polymer is one kind in polyhydroxybutyrate fat, polylactic acid, polycaprolactone, cellulose.
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Cited By (2)
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| CN114933724A (en) * | 2022-06-21 | 2022-08-23 | 陕西科技大学 | Preparation method of nonionic cellulose/polycaprolactone-based antibacterial film |
| CN115852699A (en) * | 2022-11-17 | 2023-03-28 | 天津工业大学 | Preparation method of photodynamic rechargeable antibacterial antiviral nanofiber membrane |
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