CN106693030A - Chitosan nanofibers as well as large-scale electrospinning preparation method and application thereof - Google Patents
Chitosan nanofibers as well as large-scale electrospinning preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses chitosan nanofibers as well as a large-scale electrospinning preparation method and application thereof. The preparation method comprises the following steps: (1) preparing spinning precursor liquid: dissolving chitosan and a water-soluble biopolymer into water, wherein the mass ratio of the water-soluble biopolymer to the chitosan is equal to (1 to 1) to (1 to 50); (2) preparing the nanofibers by means of airflow-assisted electrospinning. In the chitosan nanofibers prepared by the method, the content of the chitosan is more than 50%, and fiber diameters are 300-900nm. The fiber preparation method is simple, and has a wide application value in the fields such as biological tissue engineering materials, wound repair materials, beauty and cosmetics and filter protection.
Description
Technical field
The present invention relates to a kind of chitosan nano fiber and its scale electro spinning method for preparing and application, belong to
Micro-nano material field.
Background technology
Chitin is a kind of natural macromolecule amylose, is distributed widely in the crust of nature crustacean, true
In the cell membrane of bacterium and plant.Shitosan (chitosan), also known as chitosan, is that chitin passes through
A kind of deacetylated cation polysaccharide boiomacromolecule for obtaining, it is however generally that, acetyl group slough 55% with
Chitosan upper or that 1% can be dissolved in 1% acetic acid or 1% hydrochloric acid can be referred to as shitosan.
Used as a kind of natural polysaccharide macromolecule, shitosan has good biocompatibility, biodegradability
With the characteristic such as antibacterial anti hemorrhagic, be widely used in recent years medical dressing, beauty and make-up, organizational project,
The numerous areas such as medicament slow release.In medical dressing field, chitosan dressing not only have natural bacteriostatic,
Hemostasis, the advantage of promotion wound healing, and possess good moisture absorbability and moisture retentivity and suppress scar proliferation etc.
Biological function.The shitosan of Chinese patent " chitosan dressing " (CN201220099775.5) report
Dressing, the not only effect with wound healing, hemostasis, while the growth of bacterium can be suppressed, with
Surface of a wound applicating property is good；In beauty and make-up field, Chinese patent " a kind of shitosan anti-wrinkle facial mask "
(CN201310544267.2) shitosan anti-wrinkle facial mask is safe and efficient disclosed in, has no toxic side effect, while
The effects such as with cutin-softening skin, whitening, anti-inflammation.
Electrostatic spinning technique is to prepare one of most simple efficient method of 1-dimention nano fiber, with Conventional nano
Material preparation technology is compared, with processing unit (plant) it is simple, raw material sources are extensive, cost of spinning is cheap, can
The advantages such as prepare with scale.In recent years, electrostatic spinning nano fiber has huge specific surface area, larger
Length/diameter ratio and high porosity, in bioengineered tissue, medical dressing, filter protection, medicament slow release
Great application potential is shown Deng field.However, because shitosan solubility is small, solution viscosity is high simultaneously
In the characteristic of polycation electrolyte so that the more difficult electrospinning of chitosan solution.In order to solve this problem, mesh
The blending side of a small amount of shitosan is added more than preceding electrospinning chitin fiber using the macromolecular material for being easy to electrospinning
Formula, such as chitosan/polyvinyl alcohol, chitosan/polyoxyethylene, shitosan/fibroin albumen, this mode
Its chitosan content of the chitosan composite fiber for obtaining is extremely low, it is impossible to gives full play to its effect, limits it
In the application in the fields such as biological medicine.Meanwhile, the existing electrospinning process for preparing chitin fiber is more
Complicated processing technology and subsequent treatment is needed, fiber production is low, it is difficult to realize large-scale production, while
Existing electrostatic spinning preparation method, more using solvent poisonous or excitatory for example trifluoroacetic acid, formic acid,
Dichloromethane, spirit acid etc. configure spinning precursor liquid, and these solvents volatilize in preparation process can cause ring
Border is polluted, and residual solvent in the fibre is very difficult to remove, the chitin fiber membrane safety reliability of gained
It is relatively low, greatly limit its application in bio-medical field.
The content of the invention
It is an object of the invention to overcome the deficiencies in the prior art, there is provided a kind of chitosan nano fiber and its
Preparation method and application, the chitosan nano fiber is obtained by air-flow auxiliary electrostatic spinning process, is prepared
Method is simple, and spinning condition requirement is low, and yield is high, suitable for mass production, the letter of spinning forerunner formula of liquid
Single, without adding excitant or poisonous solvent, the content of shitosan is high in gained nanofiber, in life
The application aspect of thing tissue engineering material, wound repair materials or beauty and make-up field has significant advantage.
To achieve these goals, the technical scheme that the present invention is provided is as follows：
A kind of chitosan nano fiber, the chitosan nano fiber is obtained by air-flow auxiliary electrostatic spin processes,
The content of shitosan is more than 50% in the chitosan nano fiber, and fibre diameter is 300~900nm.
Further, the content of shitosan is more than 95% in the chitosan nano fiber, prepares the shell and gathers
The spinning precursor liquid of sugared nanofiber is made up of water, shitosan and water-soluble biological high molecular polymer, institute
The fibre diameter for stating chitosan nano fiber is 450~800nm.
Further, the water is distilled water or deionized water, the water-soluble biological high molecular polymer
For polyethylene glycol oxide, polyvinyl alcohol, polyvinylpyrrolidone, sodium alginate, hyaluronic acid, gelatin,
One or more in collagen, polyethylene glycol.
The invention also discloses the scale electro spinning method for preparing of described chitosan nano fiber, including with
Lower step：
(1) spinning precursor liquid is prepared：Shitosan and water-soluble biological high molecular polymer are dissolved in water,
Then it is placed on magnetic stirring apparatus and stirs to forming homogeneous spinning precursor liquid, wherein, shitosan contains
Measure between 0.5%~12% (wt%), the mass ratio of water-soluble biological high molecular polymer and shitosan
It is 1:1~1:50；
(2) air-flow auxiliary electrospinning prepares nanofiber：The spinning precursor liquid prepared in step (1) is added
Enter in the feeding cylinder of electrostatic spinning apparatus, the electrostatic spinning apparatus include high voltage power supply and high voltage power supply
The connected spinning nozzle of positive pole and the feeding cylinder of spinning nozzle connection, it is grounded collector and is arranged at spinning
Aerogenesis mechanism around shower nozzle, the aerogenesis mechanism produces and spinning injection direction identical air-flow, adjustment
Spinning nozzle collects the spinning spacing of interpolar with ground connection, sets spinning voltage and aerogenesis mechanism produces air-flow
Flow velocity, opens aerogenesis mechanism and high voltage power supply, and spinning precursor liquid forms jet in the presence of electric field force,
Solvent volatilization, forms chitosan nano fiber on collector under air-flow booster action.
Further, the content of shitosan is 5%~12% in the spinning precursor liquid that the step (1) configures
(wt%) between, water-soluble biological high molecular polymer is 1 with the mass ratio of sodium alginate:20~1:43.
Further, the electrostatic spinning apparatus of the step (2) also include the syringe pump being connected with feeding cylinder,
The syringe pump pushes spinning solution to spinning nozzle, and the aerogenesis mechanism is air pump, the outlet of the air pump
Mouth is located at directly over spinning nozzle jet, airflow direction and spinning injection side that air pump gas outlet is ejected
To identical, syringe pump is provided with the injection pump controller that control spinning precursor liquid advances speed, and air pump is set
In the air pump controller for controlling to adjust air-flow velocity.
Further, the feeding cylinder connects multiple spinning nozzles, the outlet of the air pump by woven hose
Mouthful connection fan housing, spinning nozzle is uniformly distributed below fan housing, the airflow direction ejected by fan housing with spin
Silk injection direction is identical.
Further, the spinning spacing in the step (2) is 10~50cm, and spinning voltage is 15~80
KV, the propulsion speed of syringe pump is 10 μ L/min~1mL/min, the air-flow velocity 90 of air pump injection~
250L/min。
Further, the water in step (1) is distilled water or deionized water, water-soluble biological polyphosphazene polymer
Compound is polyethylene glycol oxide, polyvinyl alcohol, polyvinylpyrrolidone, sodium alginate, hyaluronic acid, bright
One or more in glue, collagen, polyethylene glycol.
Chitosan nano fiber of the invention is in bioengineered tissue material, wound repair materials, beauty
The fields such as adornment, filter protection have a wide range of applications, such as wound dressing or face-mask material etc..
The material is applied on wound as wound dressing, and its nanofibrous structures has the larger specific surface area can
Wound surface is fully fitted in, it is quick to absorb wound surface sepage, maintain the moistening beneficial to wound healing
Environment, with good gas permeability, and can effectively completely cut off extraneous foreign matter and bacterium, and the material is shitosan
It is compound with water-soluble biological high molecular polymer, and rich in shitosan, during with Wound contact, shitosan can
It is fully dissolved out, gives full play to its effect, promote cell growth, suppress scar proliferation, promotes wound healing.
Beauty mask prepared by chitosan nano fiber not only has functions that anti-bacteria wet keeping, and can adsorb weight
Metal, whitening anti-aging.
Beneficial effects of the present invention are：The invention provides a kind of chitosan nano fiber and preparation method thereof
And application, the chitosan nano fiber is obtained by air-flow auxiliary electrostatic spinning process, and preparation method is simple,
Spinning condition requirement is low, and yield is high, suitable for mass production, and spinning forerunner formula of liquid is simple, without adding
Plus excitant or poisonous solvent, the content of shitosan is high in gained nanofiber, in bioengineered tissue
The application aspect of material, wound repair materials or beauty and make-up field has significant advantage.Specifically：
(1) chitosan nano fiber of the invention is in preparation process, and the spinning forerunner formula of liquid of use is simple
Single safety, only with water as solvent, and other toxic or irritating solvents that undope so that should
Chitosan nano fiber material obtained in method has security higher, is more suitably applied to biomedicine
Etc. aspect.In order to solve the not volatile problem of aqueous solvent, the present invention is employed in fiber manufacturing process
The method of air-flow auxiliary, adds and it during spinning precursor liquid forms jet under electric field force effect
Injection direction direction identical air-flow, to accelerate the evaporation of solvent, promotes the formation of spinning, meanwhile, gas
Stream is in contact to spinning precursor liquid jet, and the effect of power is produced to it, can the effect of auxiliary electric field power, promotion
The stretching of jet, accelerates the speed of jet, so that accelerate spinning speed, while obtaining the smaller shell of diameter
Glycan nanofiber, biomedical, field of tissue engineering technology is met to fibre diameter to meet large-scale production
Requirement chitosan nano fiber demand, make the material that there is more preferable application prospect.
(2) solute of spinning precursor liquid is only shitosan and minimal amount of water-soluble biological high molecular polymerization
Thing, without adding other crosslinking agents, chitosan content is high in gained nanofiber, and material has very
Good biocompatibility, can preferably adapt in bioengineered tissue material, wound repair materials or U.S.
Hold the application demand in the fields such as cosmetic, filter protection.
(3) preparation method of chitosan nano fiber of the invention, spinning forerunner's formula of liquid safety of use
Simply, configure convenient, spinning process is simple to operate, spinning condition is gentle, processed without the complicated later stage
The chitosan nano fiber of high-purity can be directly obtained, cost of spinning is cheap, quickly can continuously prepare and receive
Rice fiber, and the method for coordinating air-flow auxiliary using many spinning nozzles in a preferred approach, can be further
Accelerate spinning speed, improve yield, preferably adapt to the demand of large-scale production chitosan nano fiber.
Brief description of the drawings
Fig. 1 is the structural representation of many shower nozzle air-flow auxiliary electrostatic device for spinning that the present invention is used.
Fig. 2 is the stereoscan photograph of chitosan nano fiber prepared by embodiment 1.
In figure, 1- high voltage power supplies, 2- air pumps, 3- syringe pumps, 4- feed cylinders, 5- woven hoses, 6- spinning nozzles,
7- wires, 8- fan housings, 9- ground connection collectors.
Specific embodiment
According to following embodiments, the present invention may be better understood.However, those skilled in the art holds
Readily understood, specific material proportion, process conditions and its result described by embodiment are merely to illustrate this
Invention is without should also without limitation on the present invention described in detail in claims.
Embodiment 1
A kind of scale electro spinning method for preparing of chitosan nano fiber, comprises the following steps：
(1) spinning precursor liquid is prepared：By water soluble chitosan and polyethylene glycol oxide PEO (average molecular matter
5000000) dissolving in deionized water, is then placed on stirring on magnetic stirring apparatus homogeneous to being formed to amount
Spinning precursor liquid, wherein, the content of shitosan is the mass ratio of 0.5wt%, polyethylene glycol oxide and shitosan
It is 1:50；
(2) air-flow auxiliary electrospinning prepares nanofiber：The spinning precursor liquid prepared in step (1) is added
Enter in the feeding cylinder of electrostatic spinning apparatus, the electrostatic spinning apparatus include high voltage power supply and high voltage power supply
The connected spinning nozzle of positive pole and feeding cylinder, the air pump of spinning nozzle connection, the gas outlet of air pump is located at
Directly over spinning nozzle jet, the airflow direction that air pump gas outlet is ejected is identical with spinning injection direction,
The spinning spacing that spinning nozzle collects interpolar with ground connection is 50cm, and spinning voltage is 80kV, and air pump is produced
The flow velocity 250L/min of air-flow, opens air pump and high voltage power supply, and spinning precursor liquid is in the presence of electric field force
Jet is formed, solvent evaporation forms chitosan nano fiber on collector under air-flow booster action, institute
Chitosan nano fiber average diameter is obtained in 820 ± 36nm.
Embodiment 2
A kind of scale electro spinning method for preparing of chitosan nano fiber, comprises the following steps：
(1) spinning precursor liquid is prepared：By water soluble chitosan and polyethylene glycol oxide PEO (average molecular matter
5000000) dissolving in deionized water, is then placed on stirring on magnetic stirring apparatus homogeneous to being formed to amount
Spinning precursor liquid, wherein, the content of shitosan is 5wt%, and polyethylene glycol oxide is with the mass ratio of shitosan
1:20；
(2) air-flow auxiliary electrospinning prepares nanofiber：The spinning precursor liquid prepared in step (1) is added
Enter in the feeding cylinder of electrostatic spinning apparatus, the electrostatic spinning apparatus include high voltage power supply and high voltage power supply
The connected spinning nozzle of positive pole and feeding cylinder, the air pump of spinning nozzle connection, the gas outlet of air pump is located at
Directly over spinning nozzle jet, the airflow direction that air pump gas outlet is ejected is identical with spinning injection direction,
The spinning spacing that spinning nozzle collects interpolar with ground connection is 25cm, and spinning voltage is 25kV, and air pump is produced
The flow velocity 90L/min of air-flow, opens air pump and high voltage power supply, and spinning precursor liquid is in the presence of electric field force
Jet is formed, solvent evaporation forms chitosan nano fiber on collector under air-flow booster action, institute
Chitosan nano fiber average diameter is obtained in 520 ± 40nm, the shape characteristic of gained chitosan nano fiber is such as
Shown in Fig. 2.
Embodiment 3
A kind of scale electro spinning method for preparing of chitosan nano fiber, comprises the following steps：
(1) spinning precursor liquid is prepared：By water soluble chitosan and PVAC polyvinylalcohol (relative molecular mass
200000) dissolving in deionized water, is then placed on heating stirring on magnetic stirring apparatus equal to being formed
Phase spinning precursor liquid, wherein, the content of shitosan is the mass ratio of 10wt%, polyvinyl alcohol and shitosan
It is 1:30；
(2) air-flow auxiliary electrospinning prepares nanofiber：The spinning precursor liquid prepared in step (1) is added
Enter in the feeding cylinder of electrostatic spinning apparatus, the electrostatic spinning apparatus include high voltage power supply and high voltage power supply
Syringe pump that the feeding cylinder that the connected spinning nozzle of positive pole is connected with spinning nozzle is connected with feeding cylinder,
Air pump, the gas outlet of air pump is located at directly over spinning nozzle jet, the air-flow that air pump gas outlet is ejected
Direction is identical with spinning injection direction, and the spinning spacing that spinning nozzle collects interpolar with ground connection is 30cm, is spun
Filament voltage is 35kV, and air pump produces the flow velocity 120L/min of air-flow, syringe pump to be pushed to spinning nozzle and spun
Silk liquid, the propulsion speed of syringe pump is 10 μ L/min, opens air pump, high voltage power supply and syringe pump, spinning
Precursor liquid forms jet in the presence of electric field force, and solvent evaporation is on collector under air-flow booster action
Sodium alginate nano fiber is formed, gained chitosan nano fiber average diameter is in 650 ± 60nm.
Embodiment 4
A kind of scale electro spinning method for preparing of chitosan nano fiber, comprises the following steps：
(1) spinning precursor liquid is prepared：By (relative point of water soluble chitosan and polyvinylpyrrolidone PVP
Protonatomic mass 1300000) dissolve in deionized water, then it is placed on stirring on magnetic stirring apparatus and is extremely formed
Homogeneous spinning precursor liquid, wherein, the content of shitosan is 12wt%, polyvinylpyrrolidone and shitosan
Mass ratio be 1:43；
(2) air-flow auxiliary electrospinning prepares nanofiber：The spinning precursor liquid prepared in step (1) is added
Enter in the feeding cylinder of electrostatic spinning apparatus, the electrostatic spinning apparatus are many shower nozzle air-flow auxiliary electrostatic spinning
Device, apparatus structure schematic diagram as shown in figure 1, the device include high voltage power supply 1, with high voltage power supply 1 just
7 spinning nozzles 6 that pole is connected by wire 7, the feeding cylinder that spinning nozzle 6 is connected by woven hose 5
4, the connection syringe pump 3 of feeding cylinder 4, the device is additionally provided with air pump 2, the gas outlet connection of the air pump 2
8,7 spinning nozzles 6 of fan housing are uniformly distributed below fan housing 8, the airflow direction ejected by fan housing 8
Identical with spinning injection direction, the spinning spacing between spinning nozzle 6 and ground connection collector 9 is 45cm, is spun
Filament voltage is 40kV, and air pump produces the flow velocity 250L/min of air-flow, syringe pump to be pushed to spinning nozzle and spun
Silk liquid, the propulsion speed of syringe pump is 1mL/min, opens air pump, high voltage power supply and syringe pump, spinning
Precursor liquid forms jet in the presence of electric field force, and solvent evaporation is on collector under air-flow booster action
Chitosan nano fiber is formed, gained chitosan nano fiber average diameter is in 750 ± 40nm.
The above, explanation embodiment only of the invention is not any to the present invention in form and substantive
On limitation, it is noted that for those skilled in the art, do not departing from present invention side
On the premise of method, some improvement and supplement made also should be regarded as protection scope of the present invention.It is all to be familiar with sheet
Technical professional, without departing from the spirit and scope of the present invention, using disclosed above
The equivalent variations of a little variation, modification and evolution made of technology contents, be equivalent reality of the invention
Apply example；Meanwhile, all any equivalent variations done to above-described embodiment according to substantial technological of the invention
Variation, modification and evolution, still fall within the scope of technical scheme.
Claims (10)
1. a kind of chitosan nano fiber, it is characterised in that the chitosan nano fiber is aided in quiet by air-flow
Electrical spinning method is obtained, and the content of shitosan is more than 50% in the chitosan nano fiber, and fibre diameter is
300~900 nanometers.
2. a kind of chitosan nano fiber as claimed in claim 1, it is characterised in that the chitosan nano
The content of shitosan is more than 95% in rice fiber, prepare the spinning precursor liquid of the chitosan nano fiber by water,
Shitosan and water-soluble biological high molecular polymer are constituted, and the fibre diameter of the chitosan nano fiber is
450~800 nanometers.
3. a kind of chitosan nano fiber as claimed in claim 2, it is characterised in that the water is distillation
Water or deionized water, the water-soluble biological high molecular polymer are polyethylene glycol oxide, polyvinyl alcohol, poly- second
One kind or many in alkene pyrrolidone, sodium alginate, hyaluronic acid, gelatin, collagen, polyethylene glycol
Kind.
4. the scale electro spinning method for preparing of the chitosan nano fiber such as claims 1 to 3 as described in any one,
It is characterised in that it includes following steps：
(1) spinning precursor liquid is prepared：Shitosan and water-soluble biological high molecular polymer are dissolved in water,
Then it is placed on magnetic stirring apparatus and stirs to forming homogeneous spinning precursor liquid, wherein, the content of shitosan
Between 0.5%~12% (wt%), water-soluble biological high molecular polymer is 1 with the mass ratio of shitosan:1~
1:50；
(2) air-flow auxiliary electrospinning prepares nanofiber：The spinning precursor liquid that will be prepared in step (1) is added
In the feeding cylinder of electrostatic spinning apparatus, the electrostatic spinning apparatus include high voltage power supply and high-voltage power cathode
Connected spinning nozzle and spinning nozzle connection feeding cylinder, be grounded collector and be arranged at spinning nozzle week
The aerogenesis mechanism for enclosing, the aerogenesis mechanism produces and spinning injection direction identical air-flow, adjustment spinning nozzle
With the spinning spacing that ground connection collects interpolar, spinning voltage is set and aerogenesis mechanism produces the flow velocity of air-flow, open
Aerogenesis mechanism and high voltage power supply, spinning precursor liquid form jet in the presence of electric field force, aid in making in air-flow
Volatilized with lower solvent, chitosan nano fiber is formed on collector.
5. the scale electro spinning method for preparing of chitosan nano fiber as claimed in claim 4, its feature exists
In, in the spinning precursor liquid of the step (1) configuration the content of shitosan between 5%~12% (wt%),
Water-soluble biological high molecular polymer is 1 with the mass ratio of sodium alginate:20~1:43.
6. the scale electro spinning method for preparing of chitosan nano fiber as claimed in claim 4, its feature exists
In the electrostatic spinning apparatus of the step (2) also include the syringe pump being connected with feeding cylinder, the syringe pump
Spinning solution is pushed to spinning nozzle, the aerogenesis mechanism is air pump, and the gas outlet of the air pump is sprayed positioned at spinning
Directly over head jet, the airflow direction that air pump gas outlet is ejected is identical with spinning injection direction, syringe pump
The injection pump controller that control spinning precursor liquid advances speed is provided with, air pump is arranged at control and regulation air-flow stream
The air pump controller of speed.
7. the scale electro spinning method for preparing of chitosan nano fiber as claimed in claim 6, its feature exists
In, the feeding cylinder connects multiple spinning nozzles by woven hose, and the gas outlet of the air pump connects fan housing,
Spinning nozzle is uniformly distributed below fan housing, and the airflow direction ejected by fan housing is identical with spinning injection direction.
8. the scale electro spinning method for preparing of chitosan nano fiber as claimed in claim 6, its feature exists
In the spinning spacing in the step (2) is 10~50 centimetres, and spinning voltage is 15~80 kilovolts, injection
The propulsion speed of pump be 10 mul/min~1 ml/min, air pump injection 90~250 liters of air-flow velocity/
Minute.
9. the scale electro spinning method for preparing of chitosan nano fiber as claimed in claim 4, its feature exists
In the water in step (1) is distilled water or deionized water, and water-soluble biological high molecular polymer is polyoxygenated
Ethene, polyvinyl alcohol, polyvinylpyrrolidone, sodium alginate, hyaluronic acid, gelatin, collagen,
One or more in polyethylene glycol.
10. the chitosan nano fiber as described in any one in claims 1 to 3 is in bioengineered tissue material
Material, wound repair materials, beauty and make-up, the application in filter protection field.
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