CN111455496A - Antibacterial biodegradable nanofiber and preparation method thereof - Google Patents
Antibacterial biodegradable nanofiber and preparation method thereof Download PDFInfo
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- CN111455496A CN111455496A CN201910050603.5A CN201910050603A CN111455496A CN 111455496 A CN111455496 A CN 111455496A CN 201910050603 A CN201910050603 A CN 201910050603A CN 111455496 A CN111455496 A CN 111455496A
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- spinning
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- chitosan
- nanofiber
- antibacterial effect
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- 239000002121 nanofiber Substances 0.000 title claims abstract description 39
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000009987 spinning Methods 0.000 claims abstract description 66
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229920001661 Chitosan Polymers 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 24
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims abstract description 18
- 235000019253 formic acid Nutrition 0.000 claims abstract description 18
- -1 polybutylene succinate Polymers 0.000 claims abstract description 15
- 229920000954 Polyglycolide Polymers 0.000 claims abstract description 14
- 229920000747 poly(lactic acid) Polymers 0.000 claims abstract description 14
- 239000004631 polybutylene succinate Substances 0.000 claims abstract description 14
- 229920002961 polybutylene succinate Polymers 0.000 claims abstract description 14
- 239000004633 polyglycolic acid Substances 0.000 claims abstract description 14
- 239000004626 polylactic acid Substances 0.000 claims abstract description 14
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 12
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 12
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 12
- 239000003960 organic solvent Substances 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 238000005507 spraying Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 9
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 9
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 8
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 4
- 239000000835 fiber Substances 0.000 abstract description 15
- 238000001914 filtration Methods 0.000 abstract description 11
- 239000000463 material Substances 0.000 abstract description 7
- 241000191967 Staphylococcus aureus Species 0.000 abstract description 6
- 241000588724 Escherichia coli Species 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 3
- 230000005764 inhibitory process Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 40
- 238000004519 manufacturing process Methods 0.000 description 7
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- 239000000443 aerosol Substances 0.000 description 6
- 238000010041 electrostatic spinning Methods 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 241000222122 Candida albicans Species 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 229940095731 candida albicans Drugs 0.000 description 1
- 230000005686 electrostatic field Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
Classifications
-
- 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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
-
- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D13/00—Professional, industrial or sporting protective garments, e.g. surgeons' gowns or garments protecting against blows or punches
- A41D13/05—Professional, industrial or sporting protective garments, e.g. surgeons' gowns or garments protecting against blows or punches protecting only a particular body part
- A41D13/11—Protective face masks, e.g. for surgical use, or for use in foul atmospheres
-
- 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
-
- 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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/10—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
-
- 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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/18—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from other substances
Abstract
The application relates to a biodegradable nanofiber with an antibacterial effect and a preparation method thereof, belongs to the field of filter materials, and comprises the following steps: firstly, mixing chitosan and formic acid to form formic acid solution of chitosan; dissolving polybutylene succinate, polylactic acid and polyglycolic acid in an organic solvent, slowly adding a formic acid solution of chitosan, adding a certain amount of polyvinylpyrrolidone, and stirring until the mixture is uniformly mixed to obtain a spinning solution; and spinning the spinning solution by a solution jet spinning method, injecting the spinning solution into a spinning pump body, uniformly spraying the spinning solution through a spinning nozzle, and drawing and drying under the action of constant annular high-speed airflow to obtain the nanofiber. The size of the nanofiber obtained by the solution jet spinning method is 200-700nm, the filtration efficiency of the fiber is high, and the nanofiber has a good inhibition effect on staphylococcus aureus and escherichia coli.
Description
Technical Field
The application relates to the field of filter materials, in particular to biodegradable nanofiber with an antibacterial effect and a preparation method thereof.
Background
Chitosan is a natural polymer material with broad-spectrum antibacterial effect, contains a large amount of amino and hydroxyl on a molecular chain, has good inhibitory effect on fungi (such as staphylococcus aureus, colibacillus, candida albicans and the like), and has wide application prospect in the field of antibacterial materials.
At present, there are many kinds of filter fibers, mainly, ultrafine glass fiber mats, melt-blown polypropylene nonwoven fabrics, and the like. However, these filter materials have low filtration efficiency and poor filtration performance, and due to the limitation of the use environment, bacteria are easy to breed, and the biodegradability is poor, most of the filter fibers are prepared by an electrostatic spinning method, the traditional electrostatic spinning is completed under the action of an electrostatic field, and can be realized only by auxiliary high-voltage equipment, so that the production cost is high, and the production efficiency is low.
Based on the method, the biodegradable nanofiber with the antibacterial effect is prepared by adopting the latest solution jet spinning technology, the production efficiency is greatly improved, and the production cost is reduced.
Disclosure of Invention
In order to solve the above technical problems, the present application proposes the following technical solutions:
a method for preparing biodegradable nanofibers having an antibacterial effect, comprising the steps of:
(1) firstly, mixing chitosan and formic acid to form formic acid solution of chitosan;
(2) dissolving polybutylene succinate, polylactic acid and polyglycolic acid in an organic solvent, slowly adding the formic acid solution of the chitosan obtained in the step (1), adding a certain amount of polyvinylpyrrolidone, and stirring until the mixture is uniformly mixed to obtain a spinning solution;
(3) and (3) spinning the spinning solution obtained in the step (2) by a solution jet spinning method, injecting the spinning solution into a spinning pump body, uniformly spraying the spinning solution through a spinning nozzle, and drafting and drying the spinning solution under the action of constant annular high-speed airflow to obtain the nanofiber.
Preferably, the mass ratio of the chitosan, the polybutylene succinate, the polylactic acid, the polyglycolic acid and the polyvinylpyrrolidone is as follows: 10-25: 20-30: 40-50: 20-35: 5-10.
Preferably, the organic solvent is one or more of acetone, triethylamine, tetrahydrofuran or N, N-dimethylformamide.
Preferably, the concentration of the spinning dope is 5 to 15%.
Preferably, the wind pressure of the high-speed airflow is 0.1MPa to 0.25 MPa.
The nanofiber can be applied to the field of filter masks.
The nano-fiber prepared by the preparation method is measured to have the size of 200-700 nm. The fiber has good filtering efficiency, excellent antibacterial property and biodegradability.
Advantageous effects
(1) The chitosan has a broad-spectrum bactericidal effect, the polybutylene succinate, the polylactic acid and the polyglycolic acid have good biodegradability, the polybutylene succinate, the polylactic acid and the polyglycolic acid are used as spinning polymers to form corresponding spinning fibers with good biodegradability, the chitosan is better dispersed in polymer solutions of the polybutylene succinate, the polylactic acid and the polyglycolic acid by adding the polyvinylpyrrolidone, uniform and stable spinning solutions are obtained, and the fibers obtained by spinning have good antibacterial property and environment-friendly performance.
(2) Compared with the conventional electrostatic spinning method for preparing the nano-fibers, the method has the advantages that the solution jet spinning method is adopted, the production efficiency is higher, the production efficiency can be improved by 3-5 times, the production process is safe, and potential unsafe factors caused by high voltage are avoided; the size of the nanofiber obtained by the solution jet spinning method is 200-700nm, the nanofiber has a large specific surface area, the filtration efficiency of the nanofiber is high, and the nanofiber has a good inhibition effect on staphylococcus aureus and escherichia coli.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
The first embodiment is as follows:
a method for preparing biodegradable nanofibers having an antibacterial effect, comprising the steps of:
(1) firstly, mixing chitosan and formic acid to form formic acid solution of chitosan;
(2) dissolving polybutylene succinate, polylactic acid and polyglycolic acid in an organic solvent, slowly adding the formic acid solution of the chitosan obtained in the step (1), adding a certain amount of polyvinylpyrrolidone, and stirring until the mixture is uniformly mixed to obtain a spinning solution;
(3) and (3) spinning the spinning solution obtained in the step (2) by a solution jet spinning method, injecting the spinning solution into a spinning pump body, uniformly spraying the spinning solution through a spinning nozzle, and drafting and drying the spinning solution under the action of constant annular high-speed airflow to obtain the nanofiber.
The weight ratio of the chitosan to the polybutylene succinate to the polylactic acid to the polyglycolic acid to the polyvinylpyrrolidone is as follows: 10: 20: 40: 20: 5.
the organic solvent is a mixed solution of acetone and N, N-dimethylformamide.
The concentration of the spinning solution was 15%.
The wind pressure of the high-speed airflow is 0.25 MPa.
The nanofiber can be applied to the field of filter masks.
According to determination, the size of the nanofiber prepared by the preparation method is 200nm, the filtration efficiency of the fiber to NaCl aerosol with the number median diameter of 75nm and the mass median diameter of 260nm under the condition that the aerosol flow is 50L/min is 98.37% measured by a CertiTest8130 type automatic filter material tester, the antibacterial performance of the fiber is tested according to the national standard GB/T20944.3-2008 with the filtration resistance of 175.4 Pa., the antibacterial rate of the fiber to staphylococcus aureus is 97.6%, and the antibacterial rate to escherichia coli reaches 98.3%.
Example two:
a method for preparing biodegradable nanofibers having an antibacterial effect, comprising the steps of:
(1) firstly, mixing chitosan and formic acid to form formic acid solution of chitosan;
(2) dissolving polybutylene succinate, polylactic acid and polyglycolic acid in an organic solvent, slowly adding the formic acid solution of the chitosan obtained in the step (1), adding a certain amount of polyvinylpyrrolidone, and stirring until the mixture is uniformly mixed to obtain a spinning solution;
(3) and (3) spinning the spinning solution obtained in the step (2) by a solution jet spinning method, injecting the spinning solution into a spinning pump body, uniformly spraying the spinning solution through a spinning nozzle, and drafting and drying the spinning solution under the action of constant annular high-speed airflow to obtain the nanofiber.
The weight ratio of the chitosan to the polybutylene succinate to the polylactic acid to the polyglycolic acid to the polyvinylpyrrolidone is as follows: 25: 30: 50: 35: 10.
the organic solvent is a mixed solution of triethylamine and tetrahydrofuran.
The concentration of the spinning solution was 15%.
The wind pressure of the high-speed airflow is 0.1 MPa.
The nanofiber can be applied to the field of filter masks.
According to determination, the size of the nanofiber prepared by the preparation method is 700nm, the filtration efficiency of the fiber to NaCl aerosol with the number median diameter of 75nm and the mass median diameter of 260nm under the condition that the aerosol flow is 50L/min is measured by a CertiTest8130 type automatic filter material tester to be 96.34%, the filtration resistance is 160.5 Pa., and the antibacterial performance of the fiber is tested according to the national standard GB/T20944.3-2008, so that the antibacterial rate of the fiber to staphylococcus aureus is 99.9%, and the antibacterial rate to escherichia coli is 99.9%.
EXAMPLE III
A method for preparing biodegradable nanofibers having an antibacterial effect, comprising the steps of:
(1) firstly, mixing chitosan and formic acid to form formic acid solution of chitosan;
(2) dissolving polybutylene succinate, polylactic acid and polyglycolic acid in an organic solvent, slowly adding the formic acid solution of the chitosan obtained in the step (1), adding a certain amount of polyvinylpyrrolidone, and stirring until the mixture is uniformly mixed to obtain a spinning solution;
(3) and (3) spinning the spinning solution obtained in the step (2) by a solution jet spinning method, injecting the spinning solution into a spinning pump body, uniformly spraying the spinning solution through a spinning nozzle, and drafting and drying the spinning solution under the action of constant annular high-speed airflow to obtain the nanofiber.
The weight ratio of the chitosan to the polybutylene succinate to the polylactic acid to the polyglycolic acid to the polyvinylpyrrolidone is as follows: 15: 205: 45: 27: 7.
the organic solvent is a mixed solution of acetone and tetrahydrofuran.
The concentration of the spinning dope was 7%.
The wind pressure of the high-speed airflow is 0.19 MPa.
The nanofiber can be applied to the field of filter masks.
According to determination, the size of the nanofiber prepared by the preparation method is 460nm, the filtration efficiency of the fiber to NaCl aerosol with the number median diameter of 75nm and the mass median diameter of 260nm under the condition that the aerosol flow is 50L/min is measured by using a CertiTest8130 type automatic filter material tester to be 97.20%, the filtration resistance is 165.2 Pa., the antibacterial performance of the fiber is tested according to the national standard GB/T20944.3-2008, the antibacterial rate of the fiber to staphylococcus aureus is 98.5%, and the antibacterial rate to escherichia coli is 97.9%.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (8)
1. A method for preparing biodegradable nanofibers having an antibacterial effect, comprising the steps of:
(1) firstly, mixing chitosan and formic acid to form formic acid solution of chitosan;
(2) dissolving polybutylene succinate, polylactic acid and polyglycolic acid in an organic solvent, slowly adding the formic acid solution of the chitosan obtained in the step (1), adding a certain amount of polyvinylpyrrolidone, and stirring until the mixture is uniformly mixed to obtain a spinning solution;
(3) and (3) spinning the spinning solution obtained in the step (2) by a solution jet spinning method, injecting the spinning solution into a spinning pump body, uniformly spraying the spinning solution through a spinning nozzle, and drafting and drying the spinning solution under the action of constant annular high-speed airflow to obtain the nanofiber.
2. The method of preparing biodegradable nanofibers having antibacterial effect according to claim 1, wherein the mass ratio of the chitosan, polybutylene succinate, polylactic acid, polyglycolic acid, polyvinylpyrrolidone is: 10-25: 20-30: 40-50: 20-35: 5-10.
3. The method for preparing biodegradable nanofibers having an antibacterial effect according to claim 1 or 2, wherein the organic solvent is one or more of acetone, triethylamine, tetrahydrofuran or N, N-dimethylformamide.
4. The method for preparing biodegradable nanofibers having antibacterial effect according to any one of claims 1 to 3, wherein the concentration of the spinning dope is 5 to 15%.
5. The method for preparing biodegradable nanofibers having antibacterial effect according to any one of claims 1 to 4, wherein the wind pressure of the high speed air stream is 0.1MPa to 0.25 MPa.
6. The method for preparing biodegradable nanofibers having antibacterial effect according to any one of claims 1 to 5, wherein the size of the nanofibers is 200-700 nm.
7. Biodegradable nanofibers having antibacterial effect prepared by the preparation method of any one of claims 1 to 6.
8. Use of the nanofibers according to claim 7 in the field of filter masks.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910050603.5A CN111455496A (en) | 2019-01-20 | 2019-01-20 | Antibacterial biodegradable nanofiber and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910050603.5A CN111455496A (en) | 2019-01-20 | 2019-01-20 | Antibacterial biodegradable nanofiber and preparation method thereof |
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| Publication Number | Publication Date |
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| CN111455496A true CN111455496A (en) | 2020-07-28 |
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| CN201910050603.5A Pending CN111455496A (en) | 2019-01-20 | 2019-01-20 | Antibacterial biodegradable nanofiber and preparation method thereof |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101903568A (en) * | 2007-10-15 | 2010-12-01 | 埃尔马科有限公司 | Method for production of nanofibres |
| CN102965849A (en) * | 2012-11-22 | 2013-03-13 | 天津大学 | Method for preparing medical barrier membrane by electrostatic spinning |
| CN108660530A (en) * | 2018-05-28 | 2018-10-16 | 泽塔纳米科技（苏州）有限公司 | A kind of composite fibre filtering material and preparation method thereof |
| CN108774758A (en) * | 2018-05-28 | 2018-11-09 | 泽塔纳米科技（苏州）有限公司 | A kind of preparation method of nanofiber |
| CN109137131A (en) * | 2018-09-04 | 2019-01-04 | 江苏科来材料科技有限公司 | The modified antibacterial degradable nanofiber of solution gunite and its application in air filtration |
-
2019
- 2019-01-20 CN CN201910050603.5A patent/CN111455496A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101903568A (en) * | 2007-10-15 | 2010-12-01 | 埃尔马科有限公司 | Method for production of nanofibres |
| CN102965849A (en) * | 2012-11-22 | 2013-03-13 | 天津大学 | Method for preparing medical barrier membrane by electrostatic spinning |
| CN108660530A (en) * | 2018-05-28 | 2018-10-16 | 泽塔纳米科技（苏州）有限公司 | A kind of composite fibre filtering material and preparation method thereof |
| CN108774758A (en) * | 2018-05-28 | 2018-11-09 | 泽塔纳米科技（苏州）有限公司 | A kind of preparation method of nanofiber |
| CN109137131A (en) * | 2018-09-04 | 2019-01-04 | 江苏科来材料科技有限公司 | The modified antibacterial degradable nanofiber of solution gunite and its application in air filtration |
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