CN112760811A - Chitosan-alginate composite nanofiber membrane and preparation method and application thereof - Google Patents
Chitosan-alginate composite nanofiber membrane and preparation method and application thereof Download PDFInfo
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- CN112760811A CN112760811A CN202011603561.2A CN202011603561A CN112760811A CN 112760811 A CN112760811 A CN 112760811A CN 202011603561 A CN202011603561 A CN 202011603561A CN 112760811 A CN112760811 A CN 112760811A
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
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Abstract
The invention provides a chitosan-alginate composite nanofiber membrane as well as a preparation method and application thereof, wherein the method comprises the following steps: dissolving alginate in a first solvent to obtain a first mixed solution with the mass concentration of 6-12%; dissolving chitosan and gelatin in a second solvent to obtain a second mixed solution with the mass concentration of 1-8%; and mixing the first mixed solution and the second mixed solution to obtain a spinning stock solution, introducing the spinning stock solution into an injector for electrostatic spinning, and drying to obtain the chitosan-alginate composite nanofiber membrane. The preparation method of the chitosan-alginate composite nanofiber membrane is simple to operate, consumes less time and has high efficiency. The nanofiber membrane prepared by the method has good mechanical property, water resistance and biocompatibility.
Description
Technical Field
The invention relates to a chitosan-alginate composite nanofiber membrane and a preparation method and application thereof.
Background
The electrostatic spinning method is an important method for preparing superfine fiber, and mainly carries high-voltage static electricity of thousands to tens of thousands of volts on polymer solution or melt, and charged polymer liquid drops are stretched under the action of electric field force. When the force of the electric field is large enough, the polymer droplets can overcome the surface tension to form a jet stream. The solvent evaporates during the spraying process and the fibers solidify and eventually fall onto a receiving device to form a fiber mat resembling a nonwoven. The fibers produced by electrospinning are much finer than those produced by conventional methods, typically having diameters between tens of nanometers and hundreds of nanometers.
Chitosan is used as an important heavy metal-based adsorbent because it contains functional groups such as amino groups, hydroxyl groups, etc., but it is difficult to move freely during electrospinning due to its high viscosity in acidic solution, positive charge, and strong chemical bonding effect between molecules, resulting in discontinuous fibers, beading, and even spinning breakage. For this reason, polymers such as ethylene oxide, polyvinyl alcohol, polyethylene terephthalate, cellulose, polycaprolactone, etc. have been blended with chitosan to enhance tenacity and strength of the spun yarn, but there still remains a technical problem that the process is complicated due to interaction between high molecular polymers, problems of impurities, and numerous parameters, and thus it is difficult to predict the result.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of a chitosan-alginate composite nanofiber membrane, which is simple to operate, less in time consumption and high in efficiency.
In a first aspect, the invention provides a preparation method of a chitosan-alginate composite nanofiber membrane, which comprises the following steps:
s101: dissolving alginate in a first solvent to obtain a first mixed solution with the mass concentration of 6-12%; e.g., a range of 6%, 8%, 10%, 12%, and any combination thereof;
s102: dissolving chitosan and gelatin in a second solvent to obtain a second mixed solution with the mass concentration of 1-8%; e.g., ranges of 1%, 3%, 5%, 8%, and any combination thereof;
s103: and mixing the first mixed solution and the second mixed solution to obtain a spinning stock solution, introducing the spinning stock solution into an injector for electrostatic spinning, and drying to obtain the chitosan-alginate composite nanofiber membrane.
Preferably, the weight ratio of the alginate to the gelatin is in the range of 1:2-7, such as 1:2,1:5,1:7 and any combination thereof.
The preparation method of the chitosan-alginate composite nanofiber membrane is simple to operate, consumes less time and has high efficiency, and the nanofiber membrane prepared by the method has good mechanical property, water resistance and biocompatibility.
Different solvent and material concentrations may have different degrees of influence on the effect of electrospinning.
As a specific embodiment of the present invention, the first solvent is at least one selected from the group consisting of glycerin, propylene glycol, ethylene glycol, and ethanol at a concentration of not more than 5%.
Preferably, the first solvent is a solvent obtained by mixing glycerol and ethanol with the concentration of not more than 5% according to the volume ratio of 1: 1-3.
As a specific embodiment of the invention, the second solvent is at least one selected from isopropanol, glacial acetic acid with the mass concentration of 1-3%, acetic acid and dilute hydrochloric acid with the mass concentration of 1-5%.
Preferably, the second solvent is a solvent obtained by mixing 1-3% of glacial acetic acid and 1-5% of diluted hydrochloric acid according to a volume ratio of 1: 2-6.
As a specific embodiment of the present invention, the alginate is at least one selected from sodium alginate and calcium alginate.
The raw materials in the present invention may be prepared by themselves or may be obtained commercially, and the present invention is not particularly limited thereto.
In a specific embodiment of the present invention, in the step S103, in the mixing operation, the mixture is stirred at a rotation speed of 100r/min-500r/min for 5min-40min and then is allowed to stand for 2h-5h, for example, the rotation speed may be in a range of 100r/min, 300r/min, 500r/min and any combination thereof, the stirring time may be in a range of 5min, 15min, 25min, 35min and any combination thereof, and the standing time may be in a range of 2h, 4h, 5h and any combination thereof.
As a specific embodiment of the present invention, in the step S103, the receiving distance is 10cm to 15cm, for example, 10cm, 13cm, 15cm and any combination thereof.
As a specific embodiment of the present invention, in the step S103, the voltage of the electrostatic spinning may be in a range of 5kV to 10kV, such as 5kV, 7kV, 10kV and any combination thereof; the flow rate can range from 0.5mL/h to 0.8mL/h, such as 0.5mL/h, 0.6mL/h, 0.7mL/h, 0.8mL/h, and any combination thereof.
As a specific embodiment of the present invention, in the step S103, the needle diameter may be in a range of 0.3mm to 0.8mm, such as 0.3mm, 0.5mm, 0.8mm, and any combination thereof; the spinning time may range from 2h to 6h, such as 2h, 4h, 6h, and any combination thereof.
As a specific embodiment of the present invention, the chitosan has a weight average molecular weight of about 200000-300000, such as a range of 200000, 250000, 300000 and any combination thereof.
As a specific embodiment of the present invention, the weight average molecular weight of the alginate is in the range of 150000-250000, such as 150000, 200000, 250000 and any combination thereof.
In a second aspect, the present invention provides a composite nanofiber membrane prepared using the method.
As a specific embodiment of the present invention, the composite nanofiber membrane has a fiber diameter ranging from 30nm to 150nm, such as 30nm, 70nm, 100nm, 130nm, 150nm, and any combination thereof.
In a third aspect, the invention provides an application of the composite nanofiber membrane in the field of biomedicine.
The preparation method of the chitosan-alginate composite nanofiber membrane is simple to operate, consumes less time and has high efficiency, and the nanofiber membrane prepared by the method has uniform fiber diameter distribution, and has good mechanical property, water resistance and biocompatibility.
Detailed Description
The present invention is further illustrated by the following examples, which are not to be construed as limiting the invention in any way.
The sources of the materials in the following examples and comparative examples are as follows:
sodium alginate is obtained from Aladdin, and has weight average molecular weight of 200000;
chitosan was purchased from Shanxi Panier Biotech, Inc. and had a weight average molecular weight of 250000.
Example 1
Embodiment 1 provides a chitosan-alginate composite nanofiber membrane with a fiber diameter of 70nm-100nm, and the preparation method comprises the following steps:
(1) alginate is dissolved in a first solvent to obtain a first mixed solution with the mass concentration of 6%. The first solvent is obtained by mixing glycerol and ethanol with the mass concentration of 4% according to the volume ratio of 1: 3.
(2) And dissolving chitosan and gelatin in a second solvent to obtain a second mixed solution with the mass concentration of 1%. Wherein the weight ratio of the alginate to the gelatin is 1:7, and the second solvent is obtained by mixing 1% by mass of glacial acetic acid and 5% by mass of dilute hydrochloric acid according to the volume ratio of 1: 2.
(3) And mixing the first mixed solution and the second mixed solution to obtain a spinning stock solution, introducing the spinning stock solution into an injector for electrostatic spinning, wherein the receiving distance is 15cm, the voltage of electrostatic spinning is 5kV, the flow rate is 0.8mL/h, the diameter of a needle is 0.3mm, and the spinning time is 6 h. Drying to obtain the chitosan-alginate composite nanofiber membrane. During mixing, stirring the mixture for 40min at the rotating speed of 100r/min, and then standing the mixture for 2 h.
Example 2
Embodiment 2 provides a chitosan-alginate composite nanofiber membrane with a fiber diameter of 90nm to 120nm, and the preparation method comprises the following steps:
(1) alginate is dissolved in a first solvent to obtain a first mixed solution with the mass concentration of 12%. The first solvent is obtained by mixing glycerol and ethanol with the mass concentration of 2% according to the volume ratio of 1: 1.
(2) And dissolving chitosan and gelatin in a second solvent to obtain a second mixed solution with the mass concentration of 8%. Wherein the weight ratio of the alginate to the gelatin is 1:2, and the second solvent is obtained by mixing glacial acetic acid with the mass concentration of 3% and dilute hydrochloric acid with the mass concentration of 1% according to the volume ratio of 1: 6.
(3) And mixing the first mixed solution and the second mixed solution to obtain a spinning stock solution, introducing the spinning stock solution into an injector for electrostatic spinning, wherein the receiving distance is 10cm, the electrostatic spinning voltage is 10kV, the flow rate is 0.5mL/h, the needle diameter is 0.8mm, and the spinning time is 2 h. Drying to obtain the chitosan-alginate composite nanofiber membrane. And during mixing, stirring for 5min at the rotation speed of 500r/min, and standing for 5 h.
Example 3
Embodiment 3 provides a chitosan-alginate composite nanofiber membrane with a fiber diameter of 100nm-120nm, and the preparation method comprises the following steps:
(1) alginate is dissolved in a first solvent to obtain a first mixed solution with the mass concentration of 9%. The first solvent is obtained by mixing glycerol and 3% ethanol according to a volume ratio of 1: 2.
(2) And dissolving chitosan and gelatin in a second solvent to obtain a second mixed solution with the mass concentration of 4%. Wherein the weight ratio of the alginate to the gelatin is 1:5, and the second solvent is obtained by mixing 2% glacial acetic acid and 3% diluted hydrochloric acid according to the volume ratio of 1: 4.
(3) And mixing the first mixed solution and the second mixed solution to obtain a spinning stock solution, introducing the spinning stock solution into an injector for electrostatic spinning, wherein the receiving distance is 12cm, the voltage of the electrostatic spinning is 7kV, the flow rate is 0.7mL/h, the diameter of a needle is 0.5mm, and the spinning time is 4 h. Drying to obtain the chitosan-alginate composite nanofiber membrane. During mixing, stirring the mixture for 25min at the rotating speed of 200r/min, and standing the mixture for 3 h.
Example 4
Example 4 differs from example 1 only in that the first solvent in example 4 is glycerol and the second solvent is glacial acetic acid at a mass concentration of 1%, and the remaining parameters and steps are the same.
Example 5
Example 5 differs from example 1 only in that the first solvent in example 5 is ethanol at a concentration of 3% and the second solvent is acetic acid, with the remaining parameters and steps being the same.
Example 6
Example 6 differs from example 1 only in that the first solvent in example 6 is ethylene glycol and the second solvent is glacial acetic acid at a mass concentration of 3%, and the remaining parameters and steps are the same.
Comparative example 1
Comparative example 1 differs from example 1 only in that no gelatin is added to comparative example 1 and the other preparation methods and procedures are the same.
Comparative example 2
Comparative example 2 differs from example 2 only in that no gelatin is added to comparative example 2 and the other preparation methods and procedures are the same.
Comparative example 3
Comparative example 3 differs from example 3 only in that no gelatin is added in comparative example 3 and the other preparation methods and procedures are the same.
The chitosan-alginate composite nanofiber membranes prepared in the examples and the comparative examples are subjected to mechanical property tests, and the results are shown in table 1.
TABLE 1 mechanical Properties of Chitosan-alginate composite nanofiber membranes of examples and comparative examples
| Elongation at break/% | Tensile strength/MPa | |
| Example 1 | 90 | 6.37 |
| Example 2 | 87.5 | 6.71 |
| Example 3 | 91.2 | 6.45 |
| Example 4 | 88.2 | 6.12 |
| Example 5 | 85.3 | 6.06 |
| Example 6 | 86.1 | 6.01 |
| Comparative example 1 | 35.8 | 4.62 |
| Comparative example 2 | 35.8 | 4.16 |
| Comparative example 3 | 41.6 | 3.84 |
As can be seen from table 1, the chitosan-alginate composite nanofiber membranes of examples of the present invention have better elongation at break and tensile strength than those of comparative examples 1-3, and particularly, the chitosan-alginate composite nanofiber membranes of examples 1-3 have better mechanical properties due to the use of a specific combination of solvents and electrospinning parameters.
In conclusion, the preparation method of the chitosan-alginate composite nanofiber membrane is simple to operate, consumes less time and has high efficiency, and the nanofiber membrane prepared by the method has uniform fiber diameter distribution, good mechanical property, water resistance and biocompatibility.
Any numerical value mentioned in this specification, if there is only a two unit interval between any lowest value and any highest value, includes all values from the lowest value to the highest value incremented by one unit at a time. For example, if it is stated that the amount of a component, or a value of a process variable such as temperature, pressure, time, etc., is 50 to 90, it is meant in this specification that values of 51 to 89, 52 to 88 … …, and 69 to 71, and 70 to 71, etc., are specifically enumerated. For non-integer values, units of 0.1, 0.01, 0.001, or 0.0001 may be considered as appropriate. These are only some specifically named examples. In a similar manner, all possible combinations of numerical values between the lowest value and the highest value enumerated are to be considered to be disclosed in this application.
It should be noted that the above-mentioned embodiments are only for explaining the present invention, and do not constitute any limitation to the present invention. The present invention has been described with reference to exemplary embodiments, but the words which have been used herein are words of description and illustration, rather than words of limitation. The invention can be modified, as prescribed, within the scope of the claims and without departing from the scope and spirit of the invention. Although the invention has been described herein with reference to particular means, materials and embodiments, the invention is not intended to be limited to the particulars disclosed herein, but rather extends to all other methods and applications having the same functionality.
Claims (10)
1. A preparation method of a chitosan-alginate composite nanofiber membrane is characterized by comprising the following steps:
s101: dissolving alginate in a first solvent to obtain a first mixed solution with the mass concentration of 6-12%;
s102: dissolving chitosan and gelatin in a second solvent to obtain a second mixed solution with the mass concentration of 1-8%; preferably, the weight ratio of the alginate to the gelatin is 1: 2-7;
s103: and mixing the first mixed solution and the second mixed solution to obtain a spinning stock solution, introducing the spinning stock solution into an injector for electrostatic spinning, and drying to obtain the chitosan-alginate composite nanofiber membrane.
2. The method for preparing a chitosan-alginate composite nanofiber membrane according to claim 1, wherein the first solvent is at least one selected from the group consisting of glycerin, propylene glycol, ethylene glycol, and ethanol having a concentration of not more than 5%; preferably, the first solvent is a solvent obtained by mixing glycerol and ethanol with the concentration of not more than 5% according to the volume ratio of 1: 1-3; and/or the second solvent is at least one selected from isopropanol, glacial acetic acid with the mass concentration of 1% -3%, acetic acid and dilute hydrochloric acid with the mass concentration of 1% -5%; preferably, the second solvent is a solvent obtained by mixing 1-3% of glacial acetic acid and 1-5% of diluted hydrochloric acid according to a volume ratio of 1: 2-6.
3. The method for preparing chitosan-alginate composite nanofiber membrane according to claim 1 or 2, wherein the alginate is at least one selected from sodium alginate and calcium alginate.
4. The method for preparing a chitosan-alginate composite nanofiber membrane according to any one of claims 1 to 3, wherein in the step S103, the mixing operation is performed by stirring at a rotation speed of 100r/min-500r/min for 5min-40min and then standing for 2h-5 h.
5. The method for preparing a chitosan-alginate composite nanofiber membrane according to any one of claims 1 to 4, wherein, in the step S103, the receiving distance is 10cm-15 cm; and/or the voltage of electrostatic spinning is 5kV to 10kV, and the flow rate is 0.5mL/h to 0.8 mL/h.
6. The method for preparing a chitosan-alginate composite nanofiber membrane according to any one of claims 1 to 5, wherein in the step S103, the diameter of a needle is 0.3mm to 0.8mm, and the spinning time is 2h to 6 h.
7. The method for preparing a chitosan-alginate composite nanofiber membrane as claimed in any one of claims 1 to 6, wherein the weight average molecular weight of the chitosan is 200000-300000; and/or the weight average molecular weight of the alginate is 150000-250000.
8. The chitosan-alginate composite nanofiber membrane prepared by the method of any one of claims 1-7.
9. The chitosan-alginate composite nanofiber membrane of claim 8, having a fiber diameter of 30nm-150 nm.
10. The use of the chitosan-alginate composite nanofiber membrane of claim 8 or 9 in the field of biomedicine.
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