CN109881365B - Graphene alginate composite nanofiber and preparation method and application thereof - Google Patents
Graphene alginate composite nanofiber and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of fiber manufacturing, and relates to a graphene alginate composite nanofiber as well as a preparation method and an application thereof, wherein the preparation method comprises the following steps: dissolving sodium alginate and water-soluble polymer in ethanol solution, and dropwise adding calcium chloride solution; adding graphene dispersion liquid and a cross-linking agent to prepare a mixed solution with the sodium alginate content of 2-6%; dividing the mixed solution into two parts, respectively adding citric acid and sodium carbonate, and uniformly stirring and dispersing to obtain two different polymer solutions; respectively adding the two polymer solutions into a liquid storage tank, and spinning at the same collector to obtain a salt composite nanofiber precursor; and placing the precursor in a constant temperature environment of 60-100 ℃ for 8-24h to obtain the nanofiber. The graphene alginate composite nanofiber disclosed by the invention not only has good hygroscopicity, but also has humidity-responsive anticoagulation performance, and overcomes the defects of low strength and easiness in breakage.
Description
Technical Field
The invention belongs to the technical field of fiber manufacturing, and relates to a graphene alginate composite nanofiber as well as a preparation method and application thereof.
Background
The graphene is a simple carbon substance formed by regularly arranging carbon atoms according to hexagonal lattices, and has a very stable structure. The perfect lattice structure is often mistaken for being very stiff, but this is not the case. The connection between the individual carbon atoms of graphene is very flexible, and the planes of carbon atoms are bent and deformed when an external mechanical force is applied. Thus, the carbon atoms do not need to be rearranged to adapt to external force, the stability of the graphene structure is ensured, the graphene is harder than diamond, the strength of the graphene is 100 times higher than that of the best steel in the world, and the graphene can be stretched like rubber. Graphene has proven to be the thinnest substance found in the world, with a thickness of only 0.335 nm, with 20 thousand films stacked together, and only as thick as one hair line. Based on its chemical structure, graphene has many unique physicochemical properties, such as high specific surface area, high conductivity, excellent light transmittance, high mechanical strength, easy modification, mass production, and the like. Chinese researchers find that bacterial cells cannot grow on graphene, but human cells cannot be damaged, and the graphene can be used as a bandage, food package, even wound dressing and the like.
The alginate is extracted from seaweed, is block linear polymer comprising β -D-mannuronic acid (M) and α -L-guluronic acid (G)2 monomers, is different from chitosan, and can be dissolved in water quickly.
Disclosure of Invention
The invention aims to solve the problems and provides the graphene alginate composite nanofiber as well as the preparation method and the application thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of graphene alginate composite nanofibers comprises the following steps:
(1) dissolving sodium alginate and water-soluble polymer in ethanol solution, and then dropwise adding calcium chloride solution; adding the graphene dispersion liquid and the cross-linking agent, and uniformly stirring and dispersing to obtain a mixed solution with the sodium alginate content of 2-6%;
(2) dividing the mixed solution into two parts, adding citric acid into one part of the solution, adding sodium carbonate into the other part of the solution, and respectively stirring and dispersing uniformly to prepare two different polymer solutions;
(3) respectively adding the two polymer solutions into liquid storage tanks of an electrostatic spinning device, and simultaneously spinning at the same collector to obtain a graphene alginate composite nanofiber precursor;
(4) and placing the precursor of the graphene alginate composite nanofiber in a constant temperature environment of 60-100 ℃ for 8-24h to obtain the graphene alginate composite nanofiber.
In the steps of the method, the water-soluble polymer is one or more of xanthan gum, polyoxyethylene, chitosan, polyethylene glycol, polyvinyl alcohol and carboxymethyl cellulose, and the concentration of the water-soluble polymer in the mixed solution is 3% -7%.
In the steps of the method, the dosage of the calcium chloride is 1-5% of the mass of the sodium alginate.
In the steps of the method, the solvent of the graphene dispersion liquid is N, N-dimethylformamide, and the dosage of the graphene is 0.5-5% of the raw material components. According to the invention, graphene is uniformly dispersed in N, N-dimethylformamide in advance to form graphene dispersion liquid, and then the graphene dispersion liquid is added into the pre-crosslinked sodium alginate solution to be stirred and dispersed, so that the graphene can be prevented from being aggregated, and a stable and uniform graphene sodium alginate solution is formed.
In the steps of the method, the graphene is subjected to ultrasonic immersion treatment in an antibacterial solution in advance for 6-12 hours before the graphene dispersion liquid is prepared, and the antibacterial solution is a honeysuckle extract, a folium artemisiae argyi extract or a mixture of the honeysuckle extract and the folium artemisiae argyi extract.
In the steps of the method, the cross-linking agent is one or more of ethylene glycol diglycidyl ether, ethylene glycol dimethacrylate, hydroxyethyl methacrylate, N-methylolacrylamide and hydroxypropyl methacrylate, and the dosage of the cross-linking agent is 0.1-3% of the raw material components.
In the steps of the method, the contents of citric acid and sodium carbonate in the two polymer solutions are respectively 3% -6%, and the mass ratio of citric acid to sodium carbonate is 1.1:1-1.5: 1.
In the steps of the method, the electrostatic spinning conditions in the step (3) are as follows: the electrostatic spinning voltage is 15-45kV, the spinning distance is 10-30cm, and the spinning solution advancing speed is 5-15 mu L/min.
In the steps of the method, the graphene sodium alginate composite nanofiber precursor is dried in vacuum at a low temperature in advance, and then placed in a constant temperature environment of 60-100 ℃ for 8-24 hours, so that the graphene sodium alginate composite nanofiber is obtained.
The method comprises the steps of uniformly dividing a mixed solution into two parts, respectively adding citric acid and sodium carbonate into the two parts of the mixed solution, uniformly stirring, respectively spinning, and jointly receiving the two parts of the mixed solution to the same collector, so that nanofiber filaments containing two different components are mutually and alternately wound, and the two nanofiber filaments are mutually and alternately wound together to form the graphene alginate composite nanofiber. When this compound nanofiber of graphite alkene alginate used, under high humidity, can make citric acid and sodium carbonate interact release sodium citrate, have the performance of humidity responsiveness release anticoagulant, can be applied to wound dressing, prevent that the auxiliary material from absorbing the solidification behind the blood, influence the material interaction between dressing and wound.
The invention also aims to provide the graphene alginate composite nanofiber prepared by the preparation method of the graphene alginate composite nanofiber. The diameter of the nanofiber is 200-900 nm.
The invention also discloses an application of the graphene alginate composite nanofiber in the medical field.
The invention has the beneficial effects that:
the nanofiber prepared by the method combining the pre-crosslinking technology, the electrostatic spinning technology and the thermal crosslinking technology has the characteristics of small diameter and large specific surface area, the prepared nanofiber membrane is formed by alternately winding two types of nanofibers containing different materials, a plurality of mutually communicated holes can be formed in the nanofiber membrane, and the prepared nanofiber membrane has high porosity and specific surface area and has good water absorption and water retention.
According to the invention, graphene is uniformly dispersed in N, N-dimethylformamide in advance to form graphene dispersion liquid, and then the graphene dispersion liquid is added into the pre-crosslinked sodium alginate solution to be stirred and dispersed, so that graphene aggregation can be prevented, and a stable and uniform mixed solution of graphene sodium alginate is formed. According to the invention, the graphene is uniformly dispersed in the spinning precursor solution, and the graphene in the nanofiber prepared by spinning is uniformly distributed, so that the nanofiber has higher strength and elongation at break. The graphene is soaked in an antibacterial solution in advance in an ultrasonic mode, and an antibacterial component is loaded, so that the prepared nanofiber has a certain antibacterial property.
The method comprises the steps of uniformly dividing a mixed solution into two parts, respectively adding citric acid and sodium carbonate into the two parts of the mixed solution, uniformly stirring, respectively spinning, and jointly receiving the two parts of the mixed solution to the same collector, so that the nanofiber filaments containing two different components are mutually and alternately wound, and the two nanofiber filaments are mutually and alternately wound together to form the graphene alginate composite nanofiber with the communicated porous structure.
The nanofiber membrane disclosed by the invention has an intercommunicated porous structure, can improve the contact area of humidity response, is beneficial to the infiltration of liquid into fibers through the surfaces of the fibers, and the liquid contacts citric acid and sodium carbonate, so that the citric acid and the sodium carbonate can react with each other to release an anticoagulant, has the performance of humidity response on the release of the anticoagulant, can be applied to wound dressings, and can prevent auxiliary materials from coagulating after absorbing blood and influencing the material interaction between the dressings and wounds.
Detailed Description
The invention will be better understood from the following examples. However, one skilled in the art will readily appreciate that the specific structures, process conditions, and results thereof described in the examples are meant to be illustrative only and should not, nor should they be taken as limiting the invention as detailed in the claims.
Example 1
A preparation method of graphene alginate composite nanofibers comprises the following steps:
placing graphene in a mixed extracting solution of honeysuckle and folium artemisiae argyi, ultrasonically soaking for 12h, drying, then weighing the dried graphene and N, N-dimethylformamide, and preparing a graphene dispersion liquid with the graphene concentration of 11 mg/g; weighing calcium chloride, and preparing a calcium chloride solution;
dissolving sodium alginate and polyoxyethylene in an ethanol solution, then dropwise adding a calcium chloride solution until the content of calcium chloride in the mixed solution is 5% of the mass of the sodium alginate, stirring for 30min after dropwise adding is completed, then adding a graphene dispersion liquid and ethylene glycol diglycidyl ether, and uniformly stirring and dispersing to prepare a mixed solution with the content of the sodium alginate being 3% and the content of the polyoxyethylene being 7%, wherein the amount of the graphene is 4% of the amount of the raw material components, and the amount of the ethylene glycol diglycidyl ether is 1% of the amount of the raw material components;
dividing the mixed solution into two parts, adding 6% citric acid into one part of the solution, adding 4% sodium carbonate into the other part of the solution, and respectively stirring and dispersing uniformly to prepare two different polymer solutions; respectively adding the two polymer solutions into a liquid storage tank of an electrostatic spinning device, and simultaneously spinning at the same collector under the conditions that the electrostatic spinning voltage is 30kV, the spinning distance is 10cm, and the spinning solution advancing speed is 5 mu L/min to obtain a graphene alginate composite nanofiber precursor;
and (3) drying the graphene sodium alginate composite nanofiber precursor in vacuum at a low temperature, and placing the dried precursor in a constant temperature environment of 80 ℃ for 24 hours to obtain the graphene sodium alginate composite nanofiber.
A graphene alginate composite nanofiber prepared by the preparation method of the graphene alginate composite nanofiber. The average diameter of the nanofibers was 300 nm.
An application of the graphene alginate composite nanofiber in the medical field.
Example 2
A preparation method of graphene alginate composite nanofibers comprises the following steps:
placing graphene in honeysuckle extract, ultrasonically soaking for 12h, drying, then weighing the dried weighed graphene and N, N-dimethylformamide, and preparing graphene dispersion liquid with the graphene concentration of 11 mg/g; weighing calcium chloride, and preparing a calcium chloride solution;
dissolving sodium alginate and carboxymethyl cellulose in an ethanol solution, then dropwise adding a calcium chloride solution until the content of calcium chloride in the mixed solution is 1% of the mass of the sodium alginate, stirring for 30min after dropwise adding is completed, then adding a graphene dispersion liquid, hydroxyethyl methacrylate and ethylene glycol dimethacrylate, and uniformly stirring and dispersing to obtain a mixed solution with the content of the sodium alginate of 6% and the content of the carboxymethyl cellulose of 5%, wherein the amount of graphene is 1% of the raw material component, the amount of the hydroxyethyl methacrylate is 2% of the raw material component, and the amount of the ethylene glycol dimethacrylate is 1% of the raw material component;
dividing the mixed solution into two parts, adding 3.5% citric acid into one part of the solution, adding 3% sodium carbonate into the other part of the solution, and respectively stirring and dispersing uniformly to prepare two different polymer solutions; respectively adding the two polymer solutions into a liquid storage tank of an electrostatic spinning device, and simultaneously spinning at the same collector under the conditions that the electrostatic spinning voltage is 30kV, the spinning distance is 15cm, and the spinning solution advancing speed is 10 mu L/min to obtain a graphene alginate composite nanofiber precursor;
and (3) drying the graphene sodium alginate composite nanofiber precursor in vacuum at a low temperature, and placing the dried precursor in a constant temperature environment of 100 ℃ for 8 hours to obtain the graphene sodium alginate composite nanofiber.
A graphene alginate composite nanofiber prepared by the preparation method of the graphene alginate composite nanofiber. The average diameter of the nanofibers was 600 nm.
An application of the graphene alginate composite nanofiber in the medical field.
Example 3
A preparation method of graphene alginate composite nanofibers comprises the following steps:
placing graphene in a mixed extracting solution of honeysuckle and folium artemisiae argyi, ultrasonically soaking for 12h, drying, weighing the dried graphene and N, N-dimethylformamide, and preparing a graphene dispersion liquid with the graphene concentration of 11 mg/g; weighing calcium chloride, and preparing a calcium chloride solution;
dissolving sodium alginate, polyvinyl alcohol and carboxymethyl cellulose in an ethanol solution, then dropwise adding a calcium chloride solution until the content of calcium chloride in the mixed solution is 3% of the mass of the sodium alginate, stirring for 30min after dropwise adding is completed, then adding a graphene dispersion liquid and hydroxyethyl methacrylate, and uniformly stirring and dispersing to obtain a mixed solution with the content of the sodium alginate of 2%, the content of the polyvinyl alcohol of 4% and the content of the carboxymethyl cellulose of 2%, wherein the amount of the graphene is 5% of the raw material components, and the amount of the hydroxyethyl methacrylate is 2% of the raw material components;
dividing the mixed solution into two parts, adding 5% citric acid into one part of the solution, adding 4% sodium carbonate into the other part of the solution, and respectively stirring and dispersing uniformly to prepare two different polymer solutions; respectively adding the two polymer solutions into a liquid storage tank of an electrostatic spinning device, and simultaneously spinning at the same collector under the conditions that the electrostatic spinning voltage is 30kV, the spinning distance is 15cm, and the spinning solution advancing speed is 15 mu L/min to obtain a graphene alginate composite nanofiber precursor;
and (3) drying the graphene sodium alginate composite nanofiber precursor in vacuum at a low temperature, and placing the dried precursor in a constant temperature environment of 60 ℃ for 16 hours to obtain the graphene sodium alginate composite nanofiber.
A graphene alginate composite nanofiber prepared by the preparation method of the graphene alginate composite nanofiber. The average diameter of the nanofibers was 700 nm.
An application of the graphene alginate composite nanofiber in the medical field.
The moisture absorption of the fibers was measured as follows: the nanofiber membranes prepared in examples 1 to 3 of the present invention were cut into several pieces as samples, and the dry weight W1(g) of each piece of the sample was measured. The sample was placed in a 90mm petri dish, 50mL of deionized water was added, and after standing at room temperature for 30 seconds as required for the test, the sample was held by tweezers at one corner and suspended in the air for 60 seconds, and the wet weight W2(g) of the sample was measured. The liquid absorption rate per unit weight of the sample was (W2-W1)/W1.
The results are shown in Table 1.
TABLE 1 moisture absorption Properties of the fibers
| Liquid absorption rate (g/g) | |
| Example 1 | 28.9 |
| Example 2 | 27.8 |
| Example 3 | 26.3 |
Therefore, the graphene alginate composite nanofiber prepared by the method has good water absorption.
And (3) testing mechanical properties: tests prove that the graphene alginate composite nanofiber prepared by the invention has good breaking strength and elongation at break, the breaking strength is 12.8-23.1cN/dtex, and the elongation at break is 32.1-43.2%.
And (3) testing antibacterial performance: activating Escherichia coli and Staphylococcus aureus, inoculating strain to the slant, culturing at 37 deg.C for 12 hr, washing the bacterial solution on the slant with sterile water, measuring OD value, to ensure that the strains inoculated each time are equal in quantity, bacterial liquid with the equal strains is taken and coated on a culture medium plate, a filter paper sheet with the diameter of 0.6cm is placed in the plate by tweezers, the graphene alginate composite nanofiber prepared in the embodiments 1 to 3 of the invention is respectively cut into round pieces with the diameter of 0.6cm, the graphene alginate composite nanofiber round pieces prepared in the embodiments 1 to 3 of the invention are respectively placed on the filter paper pieces of the groups in the experiments 1 to 3, 3 pieces of each experiment group are arranged in parallel, the experiment groups are cultured in a constant temperature incubator at 37 ℃ for 12 hours, sterile common gauze with the diameter of 0.6cm is placed on the filter paper pieces of the blank control group, and the diameters of the inhibition zones of the experiment groups and the control group are measured. The results are shown in Table 2.
TABLE 2 antimicrobial Properties of the different treatment groups
| Treatment group | Escherichia coli/cm | Staphylococcus aureus/cm |
| Example 1 | 1.1 | 0.9 |
| Example 2 | 1.0 | 0.9 |
| Example 3 | 1.1 | 0.8 |
| Blank control group | 0 | 0 |
The above embodiments are merely illustrative of the technical concept and features of the present invention, and the present invention is not limited thereto, and equivalent changes and modifications made according to the spirit of the present invention should be covered thereby.
Claims (10)
1. The preparation method of the graphene alginate composite nanofiber is characterized by comprising the following steps:
(1) dissolving sodium alginate and water-soluble polymer in ethanol solution, and then dropwise adding calcium chloride solution; adding the graphene dispersion liquid and the cross-linking agent, and uniformly stirring and dispersing to obtain a mixed solution with the sodium alginate content of 2-6%;
(2) dividing the mixed solution into two parts, adding citric acid into one part of the solution, adding sodium carbonate into the other part of the solution, and respectively stirring and dispersing uniformly to prepare two different polymer solutions;
(3) respectively adding the two polymer solutions into liquid storage tanks of an electrostatic spinning device, and simultaneously spinning at the same collector to obtain a graphene alginate composite nanofiber precursor;
(4) and placing the precursor of the graphene alginate composite nanofiber in a constant temperature environment of 60-100 ℃ for 8-24h to obtain the graphene alginate composite nanofiber.
2. The method for preparing graphene alginate composite nanofibers according to claim 1, wherein the water-soluble polymer is one or more of xanthan gum, polyethylene oxide, chitosan, polyethylene glycol, polyvinyl alcohol and carboxymethyl cellulose, and the concentration of the water-soluble polymer in the mixed solution is 3% -7%.
3. The preparation method of the graphene alginate composite nanofiber according to claim 1, wherein the amount of the calcium chloride is 1% -5% of the mass of the sodium alginate.
4. The method for preparing the graphene alginate composite nanofiber according to claim 1, wherein a solvent of the graphene dispersion liquid is N, N-dimethylformamide, and the amount of graphene is 0.5-5% of the raw material components.
5. The method for preparing graphene alginate composite nanofibers according to claim 4, wherein the graphene is subjected to ultrasonic immersion treatment in an antibacterial solution in advance for 6-12 hours before the graphene dispersion liquid is prepared, and the antibacterial solution is honeysuckle flower extract, folium artemisiae argyi extract or a mixture of the honeysuckle flower extract and the folium artemisiae argyi extract.
6. The method for preparing graphene alginate composite nanofibers according to claim 1, wherein the cross-linking agent is one or more of ethylene glycol diglycidyl ether, ethylene glycol dimethacrylate, hydroxyethyl methacrylate, N-methylol acrylamide, hydroxypropyl methacrylate, and the amount of the cross-linking agent is 0.1% -3% of the raw material components.
7. The preparation method of the graphene alginate composite nanofiber according to claim 1, wherein the contents of citric acid and sodium carbonate in the two polymer solutions are respectively 3% -6%, and the mass ratio of citric acid to sodium carbonate is 1.1:1-1.5: 1.
8. The preparation method of the graphene alginate composite nanofiber as claimed in claim 1, wherein the electrospinning conditions in the step (3) are as follows: the electrostatic spinning voltage is 15-45kV, the spinning distance is 10-30cm, and the spinning solution advancing speed is 5-15 mu L/min.
9. The graphene alginate composite nanofiber prepared by the preparation method of the graphene alginate composite nanofiber as claimed in any one of claims 1 to 7.
10. The graphene alginate composite nanofiber as claimed in claim 9, wherein the graphene alginate composite nanofiber is applied to the medical field.
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| CN102304348A (en) * | 2011-08-26 | 2012-01-04 | 浙江理工大学 | Method for preparing moisture-content-adjustable material |
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| US20040106344A1 (en) * | 2002-06-28 | 2004-06-03 | Looney Dwayne Lee | Hemostatic wound dressings containing proteinaceous polymers |
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| CN101619507A (en) * | 2009-08-10 | 2010-01-06 | 浙江理工大学 | Preparation method of temperature and humidity adjustment fiber |
| CN102304348A (en) * | 2011-08-26 | 2012-01-04 | 浙江理工大学 | Method for preparing moisture-content-adjustable material |
| CN104178845A (en) * | 2014-08-14 | 2014-12-03 | 青岛大学 | Multifunctional high-performance carbon-based nanoparticle/sodium alginate composite fibers and preparation method thereof |
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