CN114164566A - Preparation method of antibacterial nanofiber membrane - Google Patents
Preparation method of antibacterial nanofiber membrane Download PDFInfo
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- CN114164566A CN114164566A CN202111529831.4A CN202111529831A CN114164566A CN 114164566 A CN114164566 A CN 114164566A CN 202111529831 A CN202111529831 A CN 202111529831A CN 114164566 A CN114164566 A CN 114164566A
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- silver
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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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- 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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/94—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of other polycondensation products
-
- 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
- D04H1/4326—Condensation or reaction polymers
- D04H1/4358—Polyurethanes
Abstract
The invention provides a preparation method of an antibacterial nanofiber membrane, which comprises the steps of firstly preparing a silver ammonia solution and a TPU solution, then mixing the silver ammonia solution into a waterborne polyurethane system, and then dropwise adding the silver ammonia solution into the TPU solution; preparing a nanofiber membrane by an electrostatic spinning technology, and finally placing the nanofiber membrane in an electron accelerator for irradiation reduction to obtain the antibacterial nanofiber membrane. The antibacterial nanofiber membrane has the advantages of uniform silver particle distribution, excellent antibacterial performance and capability of realizing long-acting antibacterial and washable performances.
Description
Technical Field
The invention relates to the field of preparation of antibacterial materials, in particular to a preparation method of a silver-loaded antibacterial nanofiber membrane.
Background
The nano inorganic antibacterial agent as a novel antibacterial agent has the advantages of wide antibacterial spectrum, long effective antibacterial period, low toxicity, no drug resistance, high safety and the like. The nano silver is one of nano inorganic antibacterial agents and is widely applied to the fields of environmental purification, medical treatment, cosmetics, textile and the like. In the textile industry, the nano-silver can endow the fabric with the functions of antibiosis, static resistance, electromagnetic radiation resistance and the like. The antibacterial mechanism is that the nano silver is combined with the cell wall or cell membrane of the germ and directly enters the thallus, is rapidly combined with the sulfhydryl of oxygen metabolism, blocks the metabolism to make the germ lose activity until the germ dies.
The method for loading the nano silver on the textile is various, such as a spraying method, a dipping method, a padding method, a negative pressure adsorption method and the like, and the antibacterial textile prepared by the methods has poor washing and sterilizing resistance and can be used only once. Although the nano silver is doped in the spinning solution and the silver-loaded nanofiber membrane is prepared by using the electrostatic spinning technology to achieve the effects of washing resistance and long-acting antibacterial property, the nano silver is prepared by reducing the nano silver in the solution stage by using a reducing agent, so that the nano silver in the final nanofiber membrane is not uniformly distributed.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of an antibacterial nanofiber membrane.
The purpose of the invention can be realized by the following technical scheme:
the invention provides a preparation method of an antibacterial nanofiber membrane, which comprises the following steps:
(1) preparing silver nitrate solution, adding a proper amount of ammonia water, and stirring to obtain the silver ammonia solution.
(2) And (2) adding the silver-ammonia solution obtained in the step (1) into the aqueous polyurethane emulsion, and stirring to obtain the aqueous polyurethane emulsion containing silver diammine hydroxide.
(3) Preparing a TPU solution, heating to dissolve, and stirring to obtain the TPU solution.
(4) And (3) dropwise adding the aqueous polyurethane emulsion containing silver diammine hydroxide obtained in the step (2) into the TPU solution obtained in the step (3), and stirring to obtain the silver-loaded TPU solution.
(5) And (4) preparing the silver-loaded TPU solution obtained in the step (4) into a silver-loaded nanofiber membrane by utilizing an electrostatic spinning technology.
(6) And (4) carrying out irradiation reduction on the silver-loaded nanofiber membrane obtained in the step (5) by using an electron accelerator to obtain the antibacterial nanofiber membrane.
According to the invention, the concentration of the silver nitrate solution in the step (1) is 7-9 g/L.
In addition, the stirring in the step (1) is magnetic stirring for 1-2 h.
According to the invention, the solid content of the aqueous polyurethane emulsion in the step (2) is 30-35%.
In addition, the stirring in the step (2) is magnetic stirring for 2-3 h.
According to the invention, the solvent of the TPU solution in the step (3) is DMF and acetone (volume ratio is 1:1), and the mass fraction of solute is 25-30%.
In addition, the temperature rise in the step (3) is 60-80 ℃ water bath heating.
And (3) stirring in the step (3) is magnetic stirring for 3-5 hours.
According to the invention, the volume ratio of the aqueous polyurethane emulsion containing silver diammine hydroxide and the TPU solution added in the step (4) is 1:100-1:300,
in addition, the stirring in the step (4) is mechanical stirring for 3-5 h.
According to the invention, the electrostatic spinning process parameters in the step (5) are as follows: the flow rate of the spinning solution is 3-5 mL/h; the injection amount is 3-5 ml; the voltage of the positive electrode is 15-18 kv; the receiving distance is 10-15 cm; receiving the rotation speed of the roller of 100-200 r/min.
According to the invention, the irradiation reduction in the step (6) has the energy of 0.3-0.5MeV and the irradiation time of 10-30 min.
As a preferable technical scheme, the preparation method of the antibacterial nanofiber membrane comprises the following steps:
(1) preparing a silver nitrate solution with the concentration of 7-9g/L, adding a proper amount of ammonia water, and magnetically stirring for 1-2h to obtain the silver ammonia solution.
(2) And (2) adding the silver-ammonia solution obtained in the step (1) into the aqueous polyurethane emulsion with the solid content of 30-35%, and magnetically stirring for 2-3h to obtain the aqueous polyurethane emulsion containing silver diammine hydroxide.
(3) Preparing a TPU solution with solute mass percent of 25-30%, wherein DMF and acetone (volume ratio is 1:1) are used as solvents, heating and dissolving the mixture in a water bath at 60-80 ℃, and magnetically stirring the mixture for 3-5 hours to obtain the TPU solution.
(4) Dropwise adding the aqueous polyurethane emulsion containing the silver diammine hydroxide obtained in the step (2) into the TPU solution obtained in the step (3), wherein the volume ratio of the aqueous polyurethane emulsion containing the silver diammine hydroxide to the TPU solution is 1:100-1:300, and mechanically stirring for 3-5h to obtain the silver-loaded TPU solution.
(5) Preparing the silver-loaded TPU solution obtained in the step (4) into a silver-loaded nanofiber membrane by using an electrostatic spinning technology, wherein the technological parameters are as follows: the flow rate of the spinning solution is 3-5 mL/h; the injection amount is 3-5 ml; the voltage of the positive electrode is 15-18 kv; the receiving distance is 10-15 cm; receiving the rotation speed of the roller of 100-200 r/min.
(6) And (4) carrying out irradiation reduction on the silver-loaded nanofiber membrane obtained in the step (5) for 10-30min by using an electron accelerator with the energy of 0.3-0.5MeV to obtain the antibacterial nanofiber membrane.
Compared with the preparation of nano silver by reducing agent in solution stage, the antibacterial nano fiber membrane prepared by the preferable technical scheme utilizes an electron accelerator to irradiate the nano fiber membrane to reduce silver diammine hydroxide in situ in TPU fiber to generate a nano silver simple substance, so that nano silver particles are distributed more uniformly in TPU fiber.
Compared with the prior art, the invention at least has the following beneficial effects:
the nano silver particles are coated by the waterborne polyurethane and the TPU matrix in a double-layer manner, so that the TPU fiber has excellent washing and sterilizing resistance and long-acting antibacterial performance, and the nano silver particles are uniformly distributed in the TPU fiber, so that the whole nanofiber membrane does not have a weak protection area.
Drawings
Fig. 1 is a SEM image of silver-loaded nanofibers.
Detailed Description
To better illustrate the invention and to facilitate the understanding of the technical solutions thereof, typical but non-limiting examples of the invention are as follows:
example 1
The embodiment provides a preparation method of an antibacterial nanofiber membrane, which comprises the following steps:
(1) preparing a silver nitrate solution with the concentration of 7g/L, adding a proper amount of ammonia water, and magnetically stirring for 1h to obtain the silver ammonia solution.
(2) And (2) adding the silver-ammonia solution obtained in the step (1) into the aqueous polyurethane emulsion with the solid content of 30%, and magnetically stirring for 2h to obtain the aqueous polyurethane emulsion containing silver diammine hydroxide.
(3) Preparing a TPU solution with solute mass percent of 25%, wherein DMF and acetone (volume ratio is 1:1) are used as solvents, heating and dissolving in a water bath at 60 ℃, and stirring for 5 hours by magnetic force to obtain the TPU solution.
(4) Dropwise adding the aqueous polyurethane emulsion containing the silver diammine hydroxide obtained in the step (2) into the TPU solution obtained in the step (3), wherein the volume ratio of the aqueous polyurethane emulsion containing the silver diammine hydroxide to the TPU solution is 1:100, and mechanically stirring for 5 hours to obtain the silver-loaded TPU solution.
(5) Preparing the silver-loaded TPU solution obtained in the step (4) into a silver-loaded nanofiber membrane by using an electrostatic spinning technology, wherein the technological parameters are as follows: the flow rate of the spinning solution is 3 mL/h; the injection amount is 3 ml; the voltage of the positive electrode is 15 kv; receiving distance is 10 cm; the rotation speed of the receiving roller is 100 r/min.
(6) And (4) carrying out irradiation reduction on the silver-loaded nanofiber membrane obtained in the step (5) for 10min by using an electron accelerator with the energy of 0.3MeV to obtain the antibacterial nanofiber membrane.
Example 2
The embodiment provides a preparation method of an antibacterial nanofiber membrane, which comprises the following steps:
(1) preparing a silver nitrate solution with the concentration of 8g/L, adding a proper amount of ammonia water, and magnetically stirring for 1.5h to obtain the silver ammonia solution.
(2) And (2) adding the silver-ammonia solution obtained in the step (1) into the aqueous polyurethane emulsion with the solid content of 32%, and magnetically stirring for 2.5h to obtain the aqueous polyurethane emulsion containing silver diammine hydroxide.
(3) Preparing a TPU solution with solute mass percent of 27%, wherein DMF and acetone (volume ratio is 1:1) are used as solvents, heating and dissolving the mixture in a water bath at 70 ℃, and stirring the mixture for 4 hours by magnetic force to obtain the TPU solution.
(4) Dropwise adding the aqueous polyurethane emulsion containing the silver diammine hydroxide obtained in the step (2) into the TPU solution obtained in the step (3), wherein the volume ratio of the aqueous polyurethane emulsion containing the silver diammine hydroxide to the TPU solution is 1:200, and mechanically stirring for 4 hours to obtain the silver-loaded TPU solution.
(5) Preparing the silver-loaded TPU solution obtained in the step (4) into a silver-loaded nanofiber membrane by using an electrostatic spinning technology, wherein the technological parameters are as follows: the flow rate of the spinning solution is 4 mL/h; the injection amount is 4 ml; the voltage of the positive electrode is 16 kv; receiving distance is 12 cm; the rotation speed of the receiving roller is 150 r/min.
(6) And (4) carrying out irradiation reduction on the silver-loaded nanofiber membrane obtained in the step (5) for 20min by using an electron accelerator with the energy of 0.4MeV to obtain the antibacterial nanofiber membrane.
Example 3
The embodiment provides a preparation method of an antibacterial nanofiber membrane, which comprises the following steps:
(1) preparing a silver nitrate solution with the concentration of 9g/L, adding a proper amount of ammonia water, and magnetically stirring for 2 hours to obtain the silver ammonia solution.
(2) And (2) adding the silver-ammonia solution obtained in the step (1) into the aqueous polyurethane emulsion with the solid content of 35%, and magnetically stirring for 3 hours to obtain the aqueous polyurethane emulsion containing silver diammine hydroxide.
(3) Preparing a TPU solution with solute mass percent of 30%, wherein DMF and acetone (volume ratio is 1:1) are used as solvents, heating and dissolving the mixture in a water bath at 80 ℃, and magnetically stirring the mixture for 3 hours to obtain the TPU solution.
(4) Dropwise adding the aqueous polyurethane emulsion containing the silver diammine hydroxide obtained in the step (2) into the TPU solution obtained in the step (3), wherein the volume ratio of the aqueous polyurethane emulsion containing the silver diammine hydroxide to the TPU solution is 1:300, and mechanically stirring for 3 hours to obtain the silver-loaded TPU solution.
(5) Preparing the silver-loaded TPU solution obtained in the step (4) into a silver-loaded nanofiber membrane by using an electrostatic spinning technology, wherein the technological parameters are as follows: the flow rate of the spinning solution is 5 mL/h; the injection amount is 5 ml; the voltage of the positive electrode is 18 kv; receiving distance is 15 cm; the rotation speed of the receiving roller is 200 r/min.
(6) And (4) carrying out irradiation reduction on the silver-loaded nanofiber membrane obtained in the step (5) for 30min by using an electron accelerator with the energy of 0.5MeV to obtain the antibacterial nanofiber membrane.
Claims (8)
1. A method for preparing an antibacterial nanofiber membrane, which is characterized by comprising the following steps:
(1) preparing silver nitrate solution, adding a proper amount of ammonia water, and stirring to obtain the silver ammonia solution.
(2) And (2) adding the silver-ammonia solution obtained in the step (1) into the aqueous polyurethane emulsion, and stirring to obtain the aqueous polyurethane emulsion containing silver diammine hydroxide.
(3) Preparing a TPU solution, heating to dissolve, and stirring to obtain the TPU solution.
(4) And (3) dropwise adding the aqueous polyurethane emulsion containing silver diammine hydroxide obtained in the step (2) into the TPU solution obtained in the step (3), and stirring to obtain the silver-loaded TPU solution.
(5) And (4) preparing the silver-loaded TPU solution obtained in the step (4) into a silver-loaded nanofiber membrane by utilizing an electrostatic spinning technology.
(6) And (4) carrying out irradiation reduction on the silver-loaded nanofiber membrane obtained in the step (5) by using an electron accelerator to obtain the antibacterial nanofiber membrane.
2. The method for preparing an antibacterial nanofiber membrane as claimed in claim 1, wherein the concentration of the silver nitrate solution in the step (1) is 7-9g/L, and the stirring is magnetic stirring for 1-2 h.
3. The preparation method of the antibacterial nanofiber membrane as claimed in claim 1, wherein the solid content of the aqueous polyurethane emulsion in the step (2) is 30% -35%, and the stirring is magnetic stirring for 2-3 h.
4. The method for preparing an antibacterial nanofiber membrane as claimed in claim 1, wherein in the step (3), the solvents of the TPU solution are DMF and acetone (volume ratio 1:1), the mass fraction of the solute is 25% -30%, the temperature rise is 60-80 ℃ water bath heating, and the stirring is magnetic stirring for 3-5 h.
5. The method for preparing an antibacterial nanofiber membrane as claimed in claim 1, wherein the volume ratio of the aqueous polyurethane emulsion containing silver diammine hydroxide to the TPU solution added dropwise in step (4) is 1:100-1:300, and the stirring is mechanical stirring for 3-5 h.
6. The method for preparing an antibacterial nanofiber membrane as claimed in claim 1, wherein the electrostatic spinning process parameters in step (5) are as follows: the flow rate of the spinning solution is 3-5 mL/h; the injection amount is 3-5 ml; the voltage of the positive electrode is 15-18 kv; the receiving distance is 10-15 cm; receiving the rotation speed of the roller of 100-200 r/min.
7. The method for preparing an antibacterial nanofiber membrane as claimed in claim 1, wherein the energy of the irradiation reduction in step (6) is 0.3-0.5MeV and the irradiation time is 10-30 min.
8. The method of any one of claims 1-7, wherein the method comprises the steps of:
(1) preparing a silver nitrate solution with the concentration of 7-9g/L, adding a proper amount of ammonia water, and magnetically stirring for 1-2h to obtain the silver ammonia solution.
(2) And (2) adding the silver-ammonia solution obtained in the step (1) into the aqueous polyurethane emulsion with the solid content of 30-35%, and magnetically stirring for 2-3h to obtain the aqueous polyurethane emulsion containing silver diammine hydroxide.
(3) Preparing a TPU solution with solute mass percent of 25-30%, wherein DMF and acetone (volume ratio is 1:1) are used as solvents, heating and dissolving the mixture in a water bath at 60-80 ℃, and magnetically stirring the mixture for 3-5 hours to obtain the TPU solution.
(4) Dropwise adding the aqueous polyurethane emulsion containing the silver diammine hydroxide obtained in the step (2) into the TPU solution obtained in the step (3), wherein the volume ratio of the aqueous polyurethane emulsion containing the silver diammine hydroxide to the TPU solution is 1:100-1:300, and mechanically stirring for 3-5h to obtain the silver-loaded TPU solution.
(5) Preparing the silver-loaded TPU solution obtained in the step (4) into a silver-loaded nanofiber membrane by using an electrostatic spinning technology, wherein the technological parameters are as follows: the flow rate of the spinning solution is 3-5 mL/h; the injection amount is 3-5 ml; the voltage of the positive electrode is 15-18 kv; the receiving distance is 10-15 cm; receiving the rotation speed of the roller of 100-200 r/min.
(6) And (4) carrying out irradiation reduction on the silver-loaded nanofiber membrane obtained in the step (5) for 10-30min by using an electron accelerator with the energy of 0.3-0.5MeV to obtain the antibacterial nanofiber membrane.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN115637503A (en) * | 2022-11-04 | 2023-01-24 | 太仓协大申泰羊毛衫有限公司 | Composite wool fiber, preparation method thereof and woolen sweater prepared from composite wool fiber |
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Application publication date: 20220311 |