CN109881365A - Graphene alginate composite nano fiber and its preparation method and application - Google Patents
Graphene alginate composite nano fiber and its preparation method and application Download PDFInfo
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Abstract
The invention belongs to fibre manufacturing technology field, it is related to a kind of graphene alginate composite nano fiber and its preparation method and application, preparation method are as follows: sodium alginate and water soluble polymer are dissolved in ethanol solution, calcium chloride solution is added dropwise；Graphene dispersing solution and crosslinking agent is added, the mixed solution that sodium alginate content is 2%-6% is made；Above-mentioned mixed solution is divided into two parts, is separately added into citric acid and sodium carbonate, is dispersed with stirring uniformly, two different polymer solutions is made；Above two polymer solution is separately added into reservoir, while spinning obtains salt composite nano fiber presoma in the same collector；Above-mentioned presoma is placed under 60-100 DEG C of isoperibol and places 8-24h to get the nanofiber.Graphene alginate composite nano fiber of the invention not only has a good hygroscopicity, also has the anticoagulant performance of humidity responsiveness, and overcomes that its intensity is low, the shortcomings that being easily broken off.
Description
Technical field
The invention belongs to fibre manufacturing technology field, it is related to a kind of graphene alginate composite nano fiber and its preparation
Methods and applications.
Background technique
Graphene is carbon simple substance made of neatly being arranged as carbon atom by hexagonal lattice, and structure is highly stable.It is perfect
Lattice structure, be often mistakenly thought of as very stiff but true really not so.Connection between each carbon atom of graphene is very flexible,
When applying external mechanical force, carbon atom face is with regard to bending deformation.In this way, carbon atom there is no need to be rearranged to adapt to external force,
This also ensures that the stabilization of graphene-structured, so that graphene is also harder than diamond, the intensity steel more best than in the world
Taller upper 100 times, while can be stretched as drawing rubber.Graphene be proved to be in the world have been found that it is most thin
Substance, thickness only have 0.335 nanometer, and 200,000 films are superimposed together, and also only a hairline is so thick.Based on it
Chemical structure, graphene have many unique physicochemical properties, such as high-specific surface area, high conductivity, fabulous light transmission
Property, high mechanical strength, be easy to modify and be mass produced etc..Chinese scientific research personnel has found that the cell of bacterium can not on graphene
Growth, and human cell can be used to do bandage, food packaging even Wound dressing using this point graphene without being damaged
Deng.
Sodium alginate is the polysaccharide material refined from seaweed plants, derives from marine algae, is by β-D-MANNOSE aldehyde
The block linear polymer of acid (M) and 2 kinds of monomer compositions of α-L- guluronic acid (G) are different from chitosan, it can be in water
Dissolution rapidly.Sodium alginate has many excellent performances, such as: nontoxicity, hydrophily, biocompatibility, biodegradable
Property and cheap property etc., are therefore widely used in biomedicine field.It can be applied to by the dressing that alginate fibre is made into
In the processing of wound.When alginic acid fibre acts on wound-contacting layer, it interacts between wound and generates sea
Mosanom, calcium alginate gel.But alginate fibre intensity is lower, is not able to satisfy production requirement, limits its scope of application.
Summary of the invention
The present invention to solve the above-mentioned problems, provides a kind of graphene alginate composite nano fiber and its preparation side
Method and application, graphene alginate composite nano fiber prepared by the present invention not only have good hygroscopicity, also have anti-
Solidifying performance, and overcome that alginate fibre intensity is low, the shortcomings that being easily broken off.
To achieve the goals above, The technical solution adopted by the invention is as follows:
A kind of preparation method of graphene alginate composite nano fiber, comprising the following steps:
(1) sodium alginate and water soluble polymer are dissolved in ethanol solution, calcium chloride solution is then added dropwise；Stone is added
Black alkene dispersion liquid and crosslinking agent are dispersed with stirring the mixed solution for being uniformly made that sodium alginate content is 2%-6%；
(2) above-mentioned mixed solution is divided into two parts, citric acid is added in a solution, carbonic acid is added in another solution
Sodium is dispersed with stirring uniformly respectively, two different polymer solutions is prepared；
(3) above two polymer solution is separately added into the reservoir of electrostatic spinning apparatus, while spinning is same
A collector obtains graphene alginate composite nano fiber presoma；
(4) above-mentioned graphene sodium alginate composite nano fiber presoma is placed under 60-100 DEG C of isoperibol and places 8-
For 24 hours to get the graphene alginate composite nano fiber.
In above method step, the water soluble polymer is xanthan gum, polyethylene glycol oxide, chitosan, polyethylene glycol, gathers
One of vinyl alcohol, carboxymethyl cellulose are a variety of, and in the mixed solution, the concentration of the water soluble polymer is
3%-7%.
In above method step, the dosage of the calcium chloride is the 1%-5% of sodium alginate quality.
In above method step, the solvent of the graphene dispersing solution is n,N-Dimethylformamide, the dosage of graphene
For the 0.5%-5% of raw material components.Graphene is uniformly dispersed by the present invention in n,N-Dimethylformamide in advance, is formed
Then graphene dispersing solution is added in the sodium alginate soln of precrosslink and is dispersed with stirring, can prevent stone by graphene dispersing solution
Black alkene aggregation, forms the graphene sodium alginate soln of stable uniform.
In above method step, the graphene is impregnated prior to ultrasound in antimicrobial fluid in advance before preparing graphene dispersing solution
6-12h is handled, the antimicrobial fluid is the mixture of Flos Lonicerae extractive solution, Folium Artemisiae Argyi extractive liquid or both.
In above method step, the crosslinking agent is ethylene glycol diglycidylether, ethylene glycol dimethacrylate, first
One or more, the dosage of the crosslinking agent of base hydroxy-ethyl acrylate, N hydroxymethyl acrylamide, hydroxy propyl methacrylate
For the 0.1%-3% of raw material components.
In above method step, in two kinds of polymer solution, the content of the citric acid and sodium carbonate is respectively 3%-
6%, the mass ratio of the citric acid and sodium carbonate is 1.1:1-1.5:1.
In above method step, the electrospinning conditions are as follows: electrostatic spinning voltage is 15-45kV, and spinning distance is
10-30cm, it is 5-15 μ L/min that spinning solution, which promotes rate,.
In above method step, in advance by above-mentioned graphene sodium alginate composite nano fiber presoma low-temperature vacuum drying
Afterwards, then be placed under 60-100 DEG C of isoperibol place 8-24h to get the graphene alginate composite nano fiber.
Mixed solution is divided into two parts by the present invention, is separately added into citric acid in two parts of solution and sodium carbonate stirs evenly
Afterwards, spinning is then carried out respectively, but common receive makes to same collector containing there are two types of the nanofibers phases of heterogeneity
Mutually interaction winding, two kinds of nanofibers interactions are intertwined, and form the graphene alginate composite nano fiber.When this
Graphene alginate composite nano fiber is in use, at high humidity, enabling to citric acid and sodium carbonate to react to each other and releasing
Sodium citrate is put, the performance with humidity responsiveness release anti-coagulants can be applied to wound dressing, prevent auxiliary material from absorbing blood
After solidify, the substance influenced between dressing and wound interacts.
It is a further object of the present invention to provide a kind of preparation sides with above-mentioned graphene alginate composite nano fiber
The graphene alginate composite nano fiber of method preparation.The diameter of the nanofiber is 200-900nm.
The invention also discloses a kind of above-mentioned graphene alginate composite nano fiber medical field application.
The invention has the benefit that
Present invention nanofiber as made from the method that precrosslink, electrostatic spinning and thermal crosslinking techniques combine has straight
The characteristics of diameter is small, large specific surface area, nano fibrous membrane obtained are wound by two kinds of nanofibers interactions containing different materials,
It wherein will form several holes being mutually communicated, the nano fibrous membrane obtained porosity with higher and specific surface area, have
Good water imbibition and retentiveness.
Graphene is uniformly dispersed by the present invention in n,N-Dimethylformamide in advance, forms graphene dispersing solution,
Then graphene dispersing solution is added in the sodium alginate soln of precrosslink and is dispersed with stirring, can prevent graphene from assembling, formed
The mixed solution of stable uniform graphene sodium alginate.The present invention is by being dispersed in spinning precursor liquid for graphene uniform
In, it is distributed by the graphene uniform in nanofiber made from spinning, nanofiber intensity with higher and extension at break
Rate.Graphene of the invention is impregnated in antimicrobial fluid in advance by ultrasound, antimicrobial component has been loaded, so that nanofiber obtained has
Certain anti-microbial property.
Mixed solution is divided into two parts by the present invention, is separately added into citric acid in two parts of solution and sodium carbonate stirs evenly
Afterwards, spinning is then carried out respectively, but common receive makes to same collector containing there are two types of the nanofibers phases of heterogeneity
Mutually interaction winding, two kinds of nanofibers interactions are intertwined, and form the graphene alginate with intercommunication porous structure
Composite nano fiber.
Nano fibrous membrane of the invention has intercommunication porous structure, can be improved the contact area of humidity response, is conducive to
Liquid passes through fiber surface wetting fibre, and liquid touches citric acid and sodium carbonate, enables to citric acid and sodium carbonate mutual
Reaction release anti-coagulants, the performance with humidity responsiveness release anti-coagulants can be applied to wound dressing, prevent auxiliary material from absorbing
It is solidified after blood, the substance influenced between dressing and wound interacts.
Specific embodiment
According to following embodiments, the present invention may be better understood.However, as it will be easily appreciated by one skilled in the art that real
It applies specific structure, process conditions and its result described in example and is merely to illustrate the present invention without right should will not be limited
The present invention described in detail in claim.
Embodiment 1
A kind of preparation method of graphene alginate composite nano fiber:
Graphene is placed in ultrasound in the mixed extract of honeysuckle and folium artemisiae argyi and impregnates 12h, drying, after then weighing drying
Graphene and n,N-Dimethylformamide, prepare graphene concentration be 11mg/g graphene dispersing solution；Calcium chloride is weighed, is matched
Calcium chloride solution processed；
Sodium alginate and polyethylene glycol oxide are dissolved in ethanol solution, calcium chloride solution is then added dropwise, until mixing molten
The content of calcium chloride in liquid is the 5% of sodium alginate quality, and 30min is stirred after being added dropwise to complete, graphene dispersion is then added
Liquid and ethylene glycol diglycidylether, be dispersed with stirring uniformly, be made sodium alginate content be 3%, polyoxyethylene content 7%
Mixed solution, wherein the dosage of graphene is the 4% of raw material components, and the dosage of ethylene glycol diglycidylether is raw material group
1% divided；
Above-mentioned mixed solution is divided into two parts, 6% citric acid is added in a solution, is added in another solution
4% sodium carbonate is dispersed with stirring uniformly respectively, two different polymer solutions is prepared；By both polymer solutions
It is separately added into the reservoir of electrostatic spinning apparatus, is 30kV in electrostatic spinning voltage, spinning distance is 10cm, and spinning solution promotes
Under the conditions of rate is 5 μ L/min, while spinning obtains graphene alginate composite nano fiber forerunner in the same collector
Body；
After above-mentioned graphene sodium alginate composite nano fiber presoma low-temperature vacuum drying, it is placed in 80 DEG C of isoperibols
Lower placement is for 24 hours to get the graphene alginate composite nano fiber.
A kind of graphene alginate prepared by the preparation method with above-mentioned graphene alginate composite nano fiber is multiple
Close nanofiber.The average diameter of the nanofiber is 300nm.
A kind of application of above-mentioned graphene alginate composite nano fiber in medical field.
Embodiment 2
A kind of preparation method of graphene alginate composite nano fiber:
Graphene is placed in ultrasound in Flos Lonicerae extractive solution and impregnates 12h, drying weighs graphene after then weighing drying
And n,N-Dimethylformamide, prepare the graphene dispersing solution that graphene concentration is 11mg/g；Calcium chloride is weighed, calcium chloride is prepared
Solution；
Sodium alginate and carboxymethyl cellulose are dissolved in ethanol solution, calcium chloride solution is then added dropwise, until mixing
The content of calcium chloride in solution is the 1% of sodium alginate quality, and 30min is stirred after being added dropwise to complete, and graphene point is then added
Dispersion liquid, hydroxyethyl methacrylate and ethylene glycol dimethacrylate are dispersed with stirring uniformly, and sodium alginate content is made and is
6%, the mixed solution that carboxymethyl cellulose level is 5%, wherein the dosage of graphene is the 1% of raw material components, metering system
The dosage of sour hydroxyl ethyl ester is the 2% of raw material components, and the dosage of ethylene glycol dimethacrylate is the 1% of raw material components；
Above-mentioned mixed solution is divided into two parts, 3.5% citric acid is added in a solution, is added in another solution
3% sodium carbonate is dispersed with stirring uniformly respectively, two different polymer solutions is prepared；By both polymer solutions
It is separately added into the reservoir of electrostatic spinning apparatus, is 30kV in electrostatic spinning voltage, spinning distance is 15cm, and spinning solution promotes
Under the conditions of rate is 10 μ L/min, while spinning is in the same collector, before obtaining graphene alginate composite nano fiber
Drive body；
After above-mentioned graphene sodium alginate composite nano fiber presoma low-temperature vacuum drying, it is placed in 100 DEG C of constant temperature rings
8h is placed under border to get the graphene alginate composite nano fiber.
A kind of graphene alginate prepared by the preparation method with above-mentioned graphene alginate composite nano fiber is multiple
Close nanofiber.The average diameter of the nanofiber is 600nm.
A kind of application of above-mentioned graphene alginate composite nano fiber in medical field.
Embodiment 3
A kind of preparation method of graphene alginate composite nano fiber:
Graphene is placed in ultrasound in the mixed extract of honeysuckle and folium artemisiae argyi and impregnates 12h, drying, after then weighing drying
, graphene and n,N-Dimethylformamide are weighed, the graphene dispersing solution that graphene concentration is 11mg/g is prepared；Weigh chlorination
Calcium prepares calcium chloride solution；
Sodium alginate, polyvinyl alcohol and carboxymethyl cellulose are dissolved in ethanol solution, calcium chloride solution is then added dropwise,
Until the content of the calcium chloride in mixed solution is the 3% of sodium alginate quality, 30min is stirred after being added dropwise to complete, is then added
Graphene dispersing solution, hydroxyethyl methacrylate are dispersed with stirring uniformly, and it is 2%, polyvinyl alcohol content that sodium alginate content, which is made,
The mixed solution for being 2% for 4%, carboxymethyl cellulose level, wherein the dosage of graphene is the 5% of raw material components, methyl-prop
The dosage of olefin(e) acid hydroxyl ethyl ester is the 2% of raw material components；
Above-mentioned mixed solution is divided into two parts, 5% citric acid is added in a solution, is added in another solution
4% sodium carbonate is dispersed with stirring uniformly respectively, two different polymer solutions is prepared；By both polymer solutions
It is separately added into the reservoir of electrostatic spinning apparatus, is 30kV in electrostatic spinning voltage, spinning distance is 15cm, and spinning solution promotes
Under the conditions of rate is 15 μ L/min, while spinning is in the same collector, before obtaining graphene alginate composite nano fiber
Drive body；
After above-mentioned graphene sodium alginate composite nano fiber presoma low-temperature vacuum drying, it is placed in 60 DEG C of isoperibols
Lower placement 16h is to get the graphene alginate composite nano fiber.
A kind of graphene alginate prepared by the preparation method with above-mentioned graphene alginate composite nano fiber is multiple
Close nanofiber.The average diameter of the nanofiber is 700nm.
A kind of application of above-mentioned graphene alginate composite nano fiber in medical field.
The hygroscopic measuring method of fiber is as follows: if nano fibrous membrane obtained by 1-3 of the embodiment of the present invention is cut into
Dry plate measures the dry weight W1 (g) of every sample as sample.Sample is placed in the straight culture dish through being 90mm, is added
50mL deionized water, after needing to place 30 seconds at room temperature according to test, one jiao for holding sample under the arm with tweezers is hung 60 seconds in the sky,
The weight in wet base W2 (g) of providing sample.The imbibition rate of Unit Weight sample=(W2-W1)/W1.
The results are shown in Table 1.
The moisture pick-up properties of 1 fiber of table
| Imbibition rate (g/g) | |
| Embodiment 1 | 28.9 |
| Embodiment 2 | 27.8 |
| Embodiment 3 | 26.3 |
It is found that graphene alginate composite nano fiber produced by the present invention has good water imbibition.
Mechanics Performance Testing: after tested, graphene alginate composite nano fiber obtained by the present invention has good
Breaking strength and elongation at break, breaking strength 12.8-23.1cN/dtex, elongation at break 32.1-43.2%.
Anti-microbial property test: after Escherichia coli and staphylococcus aureus activation, strain is connected on inclined-plane, 37 DEG C of trainings
12h is supported, with the bacterium solution on sterile water washing inclined-plane, surveys OD value, it is suitable with the strain amount for ensuring to be inoculated with every time, take strain amount suitable
Bacterium solution be coated on culture medium flat plate, the filter paper of diameter 0.6cm is placed in plate with tweezers, by 1- of the embodiment of the present invention
Graphene alginate composite nano fiber obtained by embodiment 3 is cut into the disk that diameter is 0.6cm, experiment 1- experiment respectively
Graphene alginate composite nano fiber obtained by 1- of embodiment of the present invention embodiment 3 is placed on 3 groups of filter paper respectively
Disk, each experimental group are arranged 3 in parallel, 12h are cultivated in 37 DEG C of constant incubators, places and disappears on the filter paper of blank control group
The diameter for crossing poison is the common gauze of 0.6cm, the diameter of measurement experiment group and control group inhibition zone.Experimental result is shown in Table 2.
The anti-microbial property of 2 different disposal group of table
| Processing group | Escherichia coli/cm | Staphylococcus aureus/cm |
| Embodiment 1 | 1.1 | 0.9 |
| Embodiment 2 | 1.0 | 0.9 |
| Embodiment 3 | 1.1 | 0.8 |
| Blank control group | 0 | 0 |
The technical concepts and features of embodiment of above only to illustrate the invention, its object is to allow be familiar with technique
People understands the content of present invention and is implemented, and it is not intended to limit the scope of the present invention, and all spirit according to the present invention is real
The equivalent change or modification that matter is done should all be contained in lid protection scope of the present invention.
Claims (10)
1. a kind of preparation method of graphene alginate composite nano fiber, which comprises the following steps:
(1) sodium alginate and water soluble polymer are dissolved in ethanol solution, calcium chloride solution is then added dropwise；Graphene is added
Dispersion liquid and crosslinking agent are dispersed with stirring the mixed solution for being uniformly made that sodium alginate content is 2%-6%；
(2) above-mentioned mixed solution is divided into two parts, citric acid is added in a solution, sodium carbonate is added in another solution, point
It is not dispersed with stirring uniformly, two different polymer solutions is prepared；
(3) above two polymer solution is separately added into the reservoir of electrostatic spinning apparatus, while spinning is in the same receipts
Collector obtains graphene alginate composite nano fiber presoma；
(4) above-mentioned graphene sodium alginate composite nano fiber presoma is placed under 60-100 DEG C of isoperibol and places 8-24h,
Up to the graphene alginate composite nano fiber.
2. a kind of preparation method of graphene alginate composite nano fiber according to claim 1, which is characterized in that
The water soluble polymer is xanthan gum, in polyethylene glycol oxide, chitosan, polyethylene glycol, polyvinyl alcohol, carboxymethyl cellulose
One or more, in the mixed solution, the concentration of the water soluble polymer is 3%-7%.
3. a kind of preparation method of graphene alginate composite nano fiber according to claim 1, which is characterized in that
The dosage of the calcium chloride is the 1%-5% of sodium alginate quality.
4. a kind of preparation method of graphene alginate composite nano fiber according to claim 1, which is characterized in that
The solvent of the graphene dispersing solution is n,N-Dimethylformamide, and the dosage of graphene is the 0.5-5% of raw material components.
5. a kind of preparation method of graphene alginate composite nano fiber as claimed in claim 4, which is characterized in that institute
Graphene is stated before preparing graphene dispersing solution in advance prior to immersion treatment 6-12h ultrasonic in antimicrobial fluid, the antimicrobial fluid is gold
The mixture of honeysuckle flower extracting solution, Folium Artemisiae Argyi extractive liquid or both.
6. a kind of preparation method of graphene alginate composite nano fiber according to claim 1, which is characterized in that
The crosslinking agent is ethylene glycol diglycidylether, ethylene glycol dimethacrylate, hydroxyethyl methacrylate, N- methylol
Acrylamide, hydroxy propyl methacrylate it is one or more, the dosage of the crosslinking agent is the 0.1%-3% of raw material components.
7. a kind of preparation method of graphene alginate composite nano fiber according to claim 1, which is characterized in that
In two kinds of polymer solution, the content of the citric acid and sodium carbonate is respectively 3%-6%, the citric acid and sodium carbonate
Mass ratio is 1.1:1-1.5:1.
8. a kind of preparation method of graphene alginate composite nano fiber according to claim 1, which is characterized in that
The electrospinning conditions are as follows: electrostatic spinning voltage is 15-45kV, and spinning distance is 10-30cm, and spinning solution propulsion rate is
5-15μL/min。
9. a kind of described in any item stones of the preparation method preparation of graphene alginate composite nano fiber of claim 1-7
Black alkene alginate composite nano fiber.
10. a kind of graphene alginate composite nano fiber as claimed in claim 9 is in the application of medical field.
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