CN113802200A - Functionalized graphene oxide/bacterial cellulose composite fiber and preparation method and application thereof - Google Patents
Functionalized graphene oxide/bacterial cellulose composite fiber and preparation method and application thereof Download PDFInfo
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L17/00—Materials for surgical sutures or for ligaturing blood vessels ; Materials for prostheses or catheters
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L17/00—Materials for surgical sutures or for ligaturing blood vessels ; Materials for prostheses or catheters
- A61L17/005—Materials for surgical sutures or for ligaturing blood vessels ; Materials for prostheses or catheters containing a biologically active substance, e.g. a medicament or a biocide
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L17/00—Materials for surgical sutures or for ligaturing blood vessels ; Materials for prostheses or catheters
- A61L17/14—Post-treatment to improve physical properties
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/20—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing organic materials
- A61L2300/23—Carbohydrates
- A61L2300/232—Monosaccharides, disaccharides, polysaccharides, lipopolysaccharides
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
- A61L2300/404—Biocides, antimicrobial agents, antiseptic agents
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Abstract
The invention discloses a functionalized graphene oxide/bacterial cellulose composite fiber and a preparation method and application thereof. The graphene oxide/bacterial cellulose composite material comprises PDDA modified graphene oxide and bacterial cellulose. A preparation method of the functionalized graphene oxide/bacterial cellulose composite fiber comprises the steps of forming a spinning solution from PDDA modified graphene oxide and activated bacterial cellulose, and then carrying out wet spinning on the spinning solution. A functionalized graphene oxide/bacterial cellulose composite fiber as described above can be used as a surgical suture. The preparation method is simple, low in cost and environment-friendly, and the obtained modified graphene oxide/bacterial cellulose composite fiber has good water absorption, high strength, good antibacterial performance, good biocompatibility and degradability.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to a functionalized graphene oxide/bacterial cellulose composite fiber and a preparation method and application thereof.
Background
The bacterial cellulose is prepared by microbial fermentation and has the same molecular structure as plant cellulose. Cellulose is the most abundant renewable resource on the earth, and has the advantages of low price, degradability, no pollution to the ecological environment and the like. The cellulose is dissolved and then converted into energy, industrial raw materials, food, medicines and feed, and the method is a better way for recycling the cellulose and protecting the environment. Bacterial cellulose is yet another important source of cellulose, an important supplement to natural cellulosic materials. Compared with the traditional plant cellulose, the bacterial cellulose has a plurality of excellent performances of high purity, high polymerization degree, high crystallinity, high hydrophilicity, high Young modulus, high strength, nanometer fineness of the fiber, higher biocompatibility, direct degradation in nature and the like. Bacterial cellulose is widely concerned by the scientific community as a novel microbial synthetic material, is widely applied to the aspects of food industry, biomedicine, papermaking, acoustic equipment, oil exploitation and the like, but reports of preparing the cellulose fiber by taking the bacterial cellulose as a textile raw material are few, so that the preparation of the cellulose fiber by taking the bacterial cellulose as the raw material has very important academic value and great social and economic significance for realizing the update of textiles and enriching the varieties of the textile and the fiber.
Disclosure of Invention
The invention aims to provide a functionalized graphene oxide/bacterial cellulose composite fiber with good water absorption, high strength, good antibacterial performance, good biocompatibility and good degradability, and a preparation method and application thereof, aiming at the defects in the prior art.
The invention discloses a functionalized graphene oxide/bacterial cellulose composite fiber, which comprises PDDA modified graphene oxide and bacterial cellulose.
According to the preparation method of the functionalized graphene oxide/bacterial cellulose composite fiber, the PDDA modified graphene oxide and the activated bacterial cellulose form a spinning solution, and then the spinning solution is subjected to wet spinning.
Further, the spinning solution is prepared by the following steps: adding PDDA modified graphene oxide powder into a 8 wt% LiCl/DMAC solvent system, performing ultrasonic treatment to form a mixed solution, adding 1.5 wt% -3 wt% of ethylenediamine activated bacterial cellulose into the mixed solution, rapidly stirring for 5-7 hours at 80-100 ℃, and then stirring for 18-22 hours at normal temperature to form a spinning stock solution, wherein the added PDDA modified graphene oxide accounts for 0.1% -0.7% of the mass of the spinning stock solution.
Further, the wet spinning comprises the following specific steps: and after the spinning stock solution is subjected to centrifugal bubble removal, the spinning stock solution enters a coagulating bath after passing through a section of air under the action of a digital injection pump, is formed in the coagulating bath, and is subjected to hot water bath stretching, water washing and drying post-treatment to obtain the composite fiber.
Further, sucking a certain amount of spinning solution after centrifugation by using an injector at room temperature, extruding the spinning solution into a coagulating bath at room temperature at a speed of 0.1-1 ml/min through a 0.21-0.5 mm needle tube under the action of an injection pump, wherein a certain gap is formed between the spinning needle tube and the coagulating bath in the process, and the gap is 1-5 cm; and (3) stretching the solidified and formed fiber in hot water at the temperature of 40-70 ℃, wherein the stretching multiple is 1.3-1.8 times, and finally cleaning and drying the stretched fiber in deionized water.
Further, the spinning solution centrifugation bubble removal comprises the following specific steps: the obtained spinning solution was poured into a 50ml centrifuge tube, and the centrifuge tube was placed in a centrifuge and centrifuged at 6000rpm for 10 min.
Further, the specific steps of graphene oxide modification include preparing 1mg/ml uniform GO aqueous solution, dripping PDDA aqueous solution into GO aqueous solution under the action of magnetic stirring until GO becomes hydrophobic, immediately stopping stirring, performing suction filtration, washing and freeze drying.
Application of the functionalized graphene oxide/bacterial cellulose fiber to preparation of a surgical suture.
Compared with the prior art, the invention has the following advantages:
1. according to the invention, the bacterial cellulose is activated by using the ethylenediamine at normal temperature, the crystallinity of the bacterial cellulose is reduced under the condition that the bacterial cellulose structure is not changed, the dissolving capacity of the bacterial cellulose in a LiCl/DMAC solvent system is greatly improved, and the bacterial cellulose can be completely dissolved under the conditions of proper temperature, heating time and stirring speed.
2. According to the invention, the PDDA is used for modifying the graphene oxide, and the GO prepared by the improved Hummers method has high oxidation degree and very good dispersibility in water. Meanwhile, GO has a large width-thickness ratio and can form nematic liquid crystal in an aqueous solution. Li ions in an LiCl/DMAC solvent system can destroy the electrostatic interaction between GO to enable GO to be agglomerated, graphene oxide modified by PDDA can be well dissolved in the LiCl/DMAC solvent system, the modified graphene oxide and bacterial cellulose have strong interface interaction, and then stress transfer between the modified graphene oxide and the bacterial cellulose is enhanced, and the strength of the bacterial cellulose is greatly improved.
3. The preparation method is simple, low in cost and environment-friendly, and the obtained modified graphene oxide/bacterial cellulose composite fiber has good water absorption, high strength, good antibacterial performance, good biocompatibility and degradability.
Drawings
FIG. 1 is a scanned image of the surface of FG0/BC composite fiber obtained in example 4;
FIG. 2 is a scanned image of the BC fiber obtained in comparative example 2;
FIG. 3 is a stress strain plot of the fibers obtained in example 3, example 4, example 5, and comparative example 2;
FIG. 4 shows the degradation rates of the fibers obtained in comparative example 2 and example 4 in beta-glucanase over different periods of time.
Detailed Description
The following are specific embodiments of the present invention and are further described with reference to the drawings, but the present invention is not limited to these embodiments.
Example 1:
(1) 0.3 wt% FGO was added to DMAC solvent and sonicated for one and a half hours to form a homogeneous solution. 8 wt% LiCl was added to the mixed solution of FGO-DMAC at 80 ℃ and stirred to dissolve it uniformly. Then heating to 100 ℃, and adding the ethylenediamine modified bacterial cellulose, wherein the mass fraction of the bacterial cellulose is 2.5 wt%. Heating at 100 deg.C for 7 hr, stopping heating after 7 hr, and stirring at room temperature for 22 hr to obtain uniform spinning solution.
(2) The spinning dope was poured into a 50ml centrifuge tube and centrifuged at 6000rpm for 10min to remove air bubbles. Sucking a certain amount of spinning stock solution by using an injector, and extruding the spinning stock solution in the injector into a coagulating bath through a 0.41mm needle tube at a speed of 0.25ml/min under the action of a digital injection pump, wherein the gap between the needle tube and the coagulating bath is 1 cm. The coagulation bath was deionized water. And stretching the obtained bacterial cellulose fiber by 1.5 times in a hot water bath at 60 ℃, washing with deionized water, and drying to obtain a finished product FGO/BC composite fiber.
Example 2:
(1) 0.4 wt% FGO was added to DMAC solvent and sonicated for one and a half hours to form a homogeneous solution. 8 wt% LiCl was added to the mixed solution of FGO-DMAC at 80 ℃ and stirred to dissolve it uniformly. Then heating to 100 ℃, and adding the ethylenediamine modified bacterial cellulose, wherein the mass fraction of the bacterial cellulose is 2.5 wt%. Heating at 100 deg.C for 7 hr, stopping heating after 7 hr, and stirring at room temperature for 22 hr to obtain uniform spinning solution.
(2) The spinning dope was poured into a 50ml centrifuge tube and centrifuged at 6000rpm for 10min to remove air bubbles. Sucking a certain amount of spinning stock solution by using an injector, and extruding the spinning stock solution in the injector into a coagulating bath through a 0.41mm needle tube at a speed of 0.25ml/min under the action of a digital injection pump, wherein the gap between the needle tube and the coagulating bath is 1 cm. The coagulation bath was a mixed solution of deionized water and DMAc, which accounted for 30% of the total coagulation bath. And stretching the obtained bacterial cellulose fiber by 1.4 times in a hot water bath at 60 ℃, washing with deionized water, and drying to obtain a finished product FGO/BC composite fiber.
Example 3:
(1) 0.1 wt% FGO was added to DMAC solvent and sonicated for one and a half hours to form a homogeneous solution. 8 wt% LiCl was added to the mixed solution of FGO-DMAC at 80 ℃ and stirred to dissolve it uniformly. Then heating to 100 ℃, and adding the ethylenediamine modified bacterial cellulose, wherein the mass fraction of the bacterial cellulose is 2.5 wt%. Heating at 100 deg.C for 7 hr, stopping heating after 7 hr, and stirring at room temperature for 20 hr to obtain uniform spinning solution.
(2) The spinning dope was poured into a 50ml centrifuge tube and centrifuged at 6000rpm for 10min to remove air bubbles. Sucking a certain amount of spinning stock solution by using an injector, and extruding the spinning stock solution in the injector into a coagulating bath through a 0.5mm needle tube at a speed of 0.1ml/min under the action of a digital injection pump, wherein the gap between the needle tube and the coagulating bath is 5 cm. The coagulating bath is a mixed solution of ethanol and DMAc, and the ratio of the ethanol to the DMAc is 2: 1. and stretching the obtained bacterial cellulose fiber by 1.4 times in a hot water bath at 60 ℃, washing with deionized water, and drying to obtain a finished product FGO/BC composite fiber. The stress-strain curve of the obtained FGO/BC composite fiber is shown in FIG. 3.
Example 4:
(1) 0.4 wt% FGO was added to DMAC solvent and sonicated for one and a half hours to form a homogeneous solution. 8 wt% LiCl was added to the mixed solution of FGO-DMAC at 80 ℃ and stirred to dissolve it uniformly. Then heating to 100 ℃, and adding the ethylenediamine modified bacterial cellulose, wherein the mass fraction of the bacterial cellulose is 2.5 wt%. Heating at 100 deg.C for 7 hr, stopping heating after 7 hr, and stirring at room temperature for 22 hr to obtain uniform spinning solution.
(2) The spinning dope was poured into a 50ml centrifuge tube and centrifuged at 6000rpm for 10min to remove air bubbles. Sucking a certain amount of spinning stock solution by using an injector, and extruding the spinning stock solution in the injector into a coagulating bath through a 0.5mm needle tube at a speed of 0.1ml/min under the action of a digital injection pump, wherein the gap between the needle tube and the coagulating bath is 5 cm. The coagulating bath is a mixed solution of ethanol and DMAc, and the ratio of the ethanol to the DMAc is 2: 1. and stretching the obtained bacterial cellulose fiber by 1.6 times in a hot water bath at 60 ℃, washing with deionized water, and drying to obtain a finished product FGO/BC composite fiber. The scanning electron microscope image of the obtained FGO/BC composite fiber is shown in FIG. 1, the stress-strain curve of the obtained FGO/BC composite fiber is shown in FIG. 3, and the degradability of the obtained FGO/BC composite fiber is shown in FIG. 4.
Example 5:
(1) 0.7 wt% FGO was added to DMAC solvent and sonicated for one and a half hours to form a homogeneous solution. 8 wt% LiCl was added to the mixed solution of FGO-DMAC at 80 ℃ and stirred to dissolve it uniformly. Then heating to 100 ℃, and adding the ethylenediamine modified bacterial cellulose, wherein the mass fraction of the bacterial cellulose is 2.5 wt%. Heating at 100 deg.C for 7 hr, stopping heating after 7 hr, and stirring at room temperature for 22 hr to obtain uniform spinning solution.
(2) The spinning dope was poured into a 50ml centrifuge tube and centrifuged at 6000rpm for 10min to remove air bubbles. Sucking a certain amount of spinning stock solution by using an injector, and extruding the spinning stock solution in the injector into a coagulating bath through a 0.5mm needle tube at a speed of 0.1ml/min under the action of a digital injection pump, wherein the gap between the needle tube and the coagulating bath is 5 cm. The coagulating bath is a mixed solution of ethanol and DMAc, and the ratio of ethanol to DMAc is 1: 2. and stretching the obtained bacterial cellulose fiber by 1.7 times in a hot water bath at 50 ℃, washing with deionized water, and drying to obtain the finished bacterial cellulose fiber. The stress-strain curve of the obtained FGO/BC composite fiber is shown in FIG. 3.
Comparative example 1:
comparative example 1 differs from example 2 in that no FGO is added and the other steps are the same as example 2.
Comparative example 2:
comparative example 2 differs from example 4 in that no FGO is added and the other steps are the same as example 4. The scanning electron microscope image of the obtained BC fiber is shown in fig. 2, the stress-strain curve of the obtained BC fiber is shown in fig. 3, and the degradability of the obtained BC fiber is shown in fig. 4.
Testing the performance of the bacterial cellulose fiber and the FGO/bacterial cellulose composite fiber:
the fibers of examples 1 to 5 and comparative examples 1 to 2 were subjected to mechanical property test and bacteriostatic effect test, the bacteriostatic effect was measured by using a plate technique, and the test results are shown in the following table.
Test result table of mechanical property test and antibacterial effect test
The above table shows that the mechanical property and the antibacterial rate of the composite fiber in the embodiment 1-2 are superior to those of the comparative example 1; the mechanical property and the bacteriostatic rate of the composite fibers in the embodiments 3-4 are superior to those of the comparative example 2, the bacteriostatic rate of the composite fibers in the embodiment 5 is superior to that of the comparative example 2, and the mechanical property is reduced compared with that of the comparative example 2. This shows that the proper FGO can improve the strength of the bacterial cellulose, because the FGO and the bacterial cellulose have stronger interfacial bonding force, which is beneficial to the transmission of stress when stressed, and when the FGO is added in an excessive amount, the FGO can agglomerate to cause the reduction of mechanical property. FGO has better antibacterial activity, and the antibacterial rate of the composite fiber is gradually increased along with the increase of the content of FGO. The mechanical properties of example 1 are better than those of example 2, and the properties of example 4 are better than those of examples 3 and 5 mainly because the mechanical properties are improved by slowing down the fiber coagulation rate and forming a dense structure inside the fiber by adding proper DMAc to the coagulation bath because of the difference between the FGO content and the coagulation bath. The main factor for the mechanical properties of example 2 over example 4 is the distance of the needle from the coagulation bath surface. When the needle tube is at a certain distance from the liquid level of the coagulating bath, the macromolecular chains in the spinning solution have a self-orientation process under the action of gravity, which is beneficial to improving the mechanical property.
While certain specific embodiments of the present invention have been described in detail by way of illustration, it will be understood by those skilled in the art that the foregoing is illustrative only and is not limiting of the scope of the invention, as various modifications or additions may be made to the specific embodiments described and substituted in a similar manner by those skilled in the art without departing from the scope of the invention as defined in the appending claims. It should be understood by those skilled in the art that any modifications, equivalents, improvements and the like made to the above embodiments in accordance with the technical spirit of the present invention are included in the scope of the present invention.
Claims (8)
1. A functionalized graphene oxide/bacterial cellulose composite fiber is characterized in that: the graphene oxide/bacterial cellulose composite material comprises PDDA modified graphene oxide and bacterial cellulose.
2. A method for preparing the functionalized graphene oxide/bacterial cellulose composite fiber according to claim 1, wherein the method comprises the following steps: and forming a spinning stock solution by using the PDDA modified graphene oxide and the activated bacterial cellulose, and then carrying out wet spinning on the spinning stock solution.
3. The preparation method of the functionalized graphene oxide/bacterial cellulose composite fiber according to claim 2, wherein the preparation method comprises the following steps: the spinning solution is prepared by the following steps: adding PDDA modified graphene oxide powder into a 8 wt% LiCl/DMAC solvent system, performing ultrasonic treatment to form a mixed solution, adding 1.5 wt% -3 wt% of ethylenediamine activated bacterial cellulose into the mixed solution, rapidly stirring for 5-7 hours at 80-100 ℃, and then stirring for 18-22 hours at normal temperature to form a spinning stock solution, wherein the added PDDA modified graphene oxide accounts for 0.1% -0.7% of the mass of the spinning stock solution.
4. The preparation method of the functionalized graphene oxide/bacterial cellulose composite fiber according to claim 3, wherein the preparation method comprises the following steps: the wet spinning method comprises the following specific steps: and after the spinning stock solution is subjected to centrifugal bubble removal, the spinning stock solution enters a coagulating bath after passing through a section of air under the action of a digital injection pump, is formed in the coagulating bath, and is subjected to hot water bath stretching, water washing and drying post-treatment to obtain the composite fiber.
5. The method of claim 4, wherein the functionalized graphene oxide/bacterial cellulose fiber is prepared by the following steps: sucking a certain amount of centrifuged spinning solution by using an injector at room temperature, extruding the spinning solution into a coagulating bath at room temperature at 0.1-1 ml/min through a 0.21-0.5 mm needle tube under the action of an injection pump, wherein a certain gap is formed between the spinning needle tube and the coagulating bath in the process, and the gap is 1-5 cm; and (3) stretching the solidified and formed fiber in hot water at the temperature of 40-70 ℃, wherein the stretching multiple is 1.3-1.8 times, and finally cleaning and drying the stretched fiber in deionized water.
6. The method of claim 5, wherein the functionalized graphene oxide/bacterial cellulose fiber is prepared by the following steps: the spinning solution centrifugation bubble removal method comprises the following specific steps: the obtained spinning solution was poured into a 50ml centrifuge tube, and the centrifuge tube was placed in a centrifuge and centrifuged at 6000rpm for 10 min.
7. The method of claim 2, wherein the functionalized graphene oxide/bacterial cellulose fiber is prepared by the following steps: the specific steps of graphene oxide modification include preparing 1mg/ml uniform GO aqueous solution, dripping PDDA aqueous solution into GO aqueous solution under the action of magnetic stirring until GO becomes hydrophobic, immediately stopping stirring, performing suction filtration, washing and freeze drying.
8. Use of functionalized graphene oxide/bacterial cellulose fibers according to claim 1, characterized in that: used for preparing surgical suture.
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