CN115074864A - Novel bactericidal fiber material and preparation method thereof - Google Patents
Novel bactericidal fiber material and preparation method thereof Download PDFInfo
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- CN115074864A CN115074864A CN202210813576.4A CN202210813576A CN115074864A CN 115074864 A CN115074864 A CN 115074864A CN 202210813576 A CN202210813576 A CN 202210813576A CN 115074864 A CN115074864 A CN 115074864A
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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
- 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
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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
Abstract
The invention discloses a novel bactericidal fiber material and a preparation method thereof. The preparation method of the novel bactericidal fiber material comprises the following steps: mixing and stirring a silicon source, lactic acid and a zinc source, and dissolving the mixture in ethanol and water to prepare a silicon-zinc mixed solution; stirring and dissolving a high molecular polymer in a solvent to prepare a high molecular polymer solution; mixing the silicon-zinc mixed solution with the high molecular polymer solution, and stirring to prepare a spinning solution; preparing a silicon-zinc mixed fiber precursor by using a spinning solution through an electrostatic spinning method, taking out the silicon-zinc mixed fiber precursor, drying, heating the fiber in an inert gas atmosphere, preserving heat, and naturally cooling to obtain ZnO/SiO 2 A composite fiber material. The novel bactericidal fiber material is prepared by the preparation method of the novel bactericidal fiber material. ZnO/SiO prepared by the invention 2 The composite bactericidal fiber material has low cost, simple preparation process and high strength, and is suitable for industrial production and application.
Description
Technical Field
The invention relates to the technical field of purification materials, in particular to a novel bactericidal fiber material and a preparation method thereof.
Background
With the progress of society, the living standard of people is higher and higher, the requirement for environmental pollution control is also gradually improved, and the fiber material is used as a common raw material and is widely applied, in particular to masks, purifiers, air conditioners and the like, at present, the fiber material comprises three types of natural fibers (including plant fibers and animal fibers), inorganic fibers (such as asbestos and glass fibers) and synthetic fibers (such as polyester fibers and polyaramide fibers) and the traditional fiber has wide application range and single function, for example, the fiber is only used for filtration and adsorption and has little bactericidal property.
The nano zinc oxide is used as a novel functional material with excellent performance, and particularly has wide application prospect in the fields of antibiosis and biomedicine under the drive of new process equipment. Zinc oxide can continuously release zinc ions in an aqueous medium, the zinc ions can enter cell membranes, the cell membranes are damaged, and when the zinc ions react with certain groups of proteins in cells, the space structures of bacteria and the proteins in the cells are damaged, so that protease in the cells is inactivated, and the bacteria are killed. After destruction, zinc ions are liberated from the bacteria and the sterilization process is repeated. The nano zinc oxide can interact with the cell wall on the surface of the bacteria to destroy the cell wall of the bacteria, so that the contents are released to kill the bacteria. Therefore, the zinc oxide sterilization fiber material which is low in design and preparation cost and environment-friendly has great research significance.
Disclosure of Invention
Based on the above, the invention aims to provide a novel bactericidal fiber material and a preparation method thereof.
In a first aspect, the preparation method of the novel bactericidal fiber material comprises the following steps:
mixing and stirring a silicon source, lactic acid and a zinc source, and dissolving the mixture in ethanol and water to prepare a silicon-zinc mixed solution;
stirring and dissolving a high molecular polymer in a solvent to prepare a high molecular polymer solution;
mixing the silicon-zinc mixed solution with the high molecular polymer solution, and stirring to prepare a spinning solution;
preparing a silicon-zinc mixed fiber precursor by using a spinning solution through an electrostatic spinning method, taking out the silicon-zinc mixed fiber precursor, drying, heating the fiber in an inert gas atmosphere, preserving heat, and naturally cooling to obtain ZnO/SiO 2 A composite fiber material.
In one embodiment of the above technical solution, a silicon source, lactic acid, and a zinc source are mixed and stirred, and dissolved in ethanol and water, wherein the molar mass ratio of the total amount of the silicon source, lactic acid, and zinc source to the total amount of ethanol and water is 1: 1-2;
mixing and stirring a silicon source, lactic acid and a zinc source according to a molar mass ratio of 2:1: 2;
the molar mass ratio of the ethanol to the water is 2-3: 1.
In one embodiment of the above technical solution, the silicon source is one or a combination of tetraethoxysilane and methyl orthosilicate;
the zinc source is one or more of zinc acetate, zinc sulfate and stannic chloride.
In one embodiment of the above technical solution, the solvent is ethanol and water, and the molar mass ratio of ethanol to water is 1: 0.5-2.
In one embodiment, the molar mass ratio of the silicon-zinc mixed solution to the high molecular polymer solution is 1: 1-2.
In one embodiment, the molecular polymer is PVA, and the mass content of the PVA in the high molecular polymer solution is 5 to 15%.
In one embodiment, the preparation of the silicon-zinc mixed fiber precursor by using the spinning solution through an electrostatic spinning method includes: pouring the spinning solution into a liquid tank of a needleless electrostatic spinning machine for electrostatic spinning, wherein the relevant parameters are as follows: the positive voltage is 12kv, the negative voltage is 5kv, the rotating speed of the needle is 120r/min, the distance from the receiving device to the needle is 15cm, and the rotating speed of the receiving device is 50 r/min.
In one embodiment of the technical scheme, the fiber is taken out and dried in a vacuum drying oven, then is put into a muffle furnace to be heated to 500-800 ℃ in the inert gas atmosphere for heat preservation for 0.5-2h, and then is naturally cooled to room temperature to prepare ZnO/SiO 2 A composite fiber material.
In one embodiment of the technical scheme, the prepared ZnO/SiO 2 The fiber diameter of the composite fiber material is 0.5-1 um.
In a second aspect, a novel bactericidal fiber material is prepared by the preparation method of any one of the above novel bactericidal fiber materials.
Compared with the prior art, the novel composite bactericidal fiber material and the preparation method thereof have the beneficial effects that:
ZnO/SiO prepared by the invention 2 The composite bactericidal fiber material is prepared by taking silicon dioxide silicon nanofiber as a substrate material and modifying the silicon dioxide silicon nanofiber by using zinc oxide 2 The antibacterial effect is achieved by compounding the antibacterial fiber material. ZnO/SiO prepared by the invention 2 The composite bactericidal fiber material not only has the function of sterilizing at room temperature, but also has excellent durability. In addition, SiO 2 As a supporting framework structure, the steel plate has the characteristics of high strength, corrosion resistance, high temperature resistance and the like. ZnO/SiO prepared by the invention 2 The composite bactericidal fiber material has low cost, simple preparation process and high strength, and is suitable for industrial production and application.
For a better understanding and practice, the invention is described in detail below with reference to the accompanying drawings.
Drawings
FIG. 1 is ZnO/SiO 2 SEM image of composite fibrous material.
FIG. 2 is SiO 2 SEM image of composite fibrous material.
FIG. 3 is a graph comparing the results before and after the examples.
FIG. 4 is a graph showing a comparison of the results before and after the comparative example.
Detailed Description
The terms of orientation of up, down, left, right, front, back, top, bottom, and the like, referred to or may be referred to in this specification, are defined relative to their configuration, and are relative concepts. Therefore, it may be changed according to different positions and different use states. Therefore, these and other directional terms should not be construed as limiting terms.
The implementations described in the exemplary embodiments below are not intended to represent all implementations consistent with the present disclosure. Rather, they are merely examples of implementations consistent with certain aspects of the present disclosure.
The terminology used in the present disclosure is for the purpose of describing particular embodiments only and is not intended to be limiting of the disclosure. As used in this disclosure, the singular forms "a", "an", and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It should also be understood that the term "and/or" as used herein refers to and encompasses any and all possible combinations of one or more of the associated listed items.
In a first aspect, the preparation method of the novel bactericidal fiber material comprises the following steps:
step 101, mixing and stirring a silicon source, lactic acid and a zinc source, and dissolving the mixture in ethanol and water to prepare a silicon-zinc mixed solution. Wherein the molar mass ratio of the total amount of the silicon source, the lactic acid and the zinc source to the total amount of the ethanol and the water is 1: 1-2.
Mixing and stirring a silicon source, lactic acid and a zinc source according to a molar mass ratio of 2:1: 2.
The molar mass ratio of the ethanol to the water is 2-3: 1.
Optionally, the silicon source is one or a combination of ethyl orthosilicate and methyl orthosilicate.
Optionally, the zinc source is one or more of zinc acetate, zinc sulfate, and tin chloride.
102, stirring and dissolving the high molecular polymer in a solvent to prepare a high molecular polymer solution.
In one embodiment, the solvent is ethanol and water, and the molar mass ratio of ethanol to water is 1: 0.5-2.
Preferably, the molar mass ratio of the silicon-zinc mixed solution to the high molecular polymer solution is 1: 1-2.
In one embodiment, the molecular polymer species is PVA and has a mass content of 5 to 15% in the high molecular polymer solution.
And 103, mixing and stirring the silicon-zinc mixed solution and the high molecular polymer solution to prepare the spinning solution.
104, preparing a silicon-zinc mixed fiber precursor by using the spinning solution through an electrostatic spinning method, taking out the silicon-zinc mixed fiber precursor, drying, heating the fiber in an inert gas atmosphere, preserving heat, and naturally cooling to obtain ZnO/SiO 2 A composite fiber material.
In one embodiment, the preparation of the silicon-zinc mixed fiber precursor by an electrospinning method using the spinning solution comprises: pouring the spinning solution into a liquid tank of a needleless electrostatic spinning machine for electrostatic spinning, wherein the relevant parameters are as follows: the positive voltage is 12kv, the negative voltage is 5kv, the rotating speed of the needle is 120r/min, the distance from the receiving device to the needle is 15cm, and the rotating speed of the receiving device is 50 r/min.
In one embodiment, the fiber is taken out and dried in a vacuum drying oven, then placed in a muffle furnace in an inert gas atmosphere, heated to 500-800 ℃, and kept for 0.5-2h, and then naturally cooled to room temperature to prepare ZnO/SiO 2 A composite fiber material.
In one embodiment, the resulting ZnO/SiO is prepared 2 The fiber diameter of the composite fiber material is 0.5-1 um.
In a second aspect, the novel bactericidal fiber material is prepared by the preparation method of the novel bactericidal fiber material.
Examples
Weighing 7g of tetraethoxysilane, 3.5g of lactic acid and 7g of zinc acetate, adding the mixture into 100ml of ethanol and water mixed solution, placing the mixture into a conical flask, sealing, stirring and mixing, carrying out water bath at 45 ℃, and stirring for 2 hours to prepare silicon-zinc mixed solution.
5g of PVA was weighed and dissolved in a solvent under stirring to prepare a high molecular polymer solution.
And mixing and stirring the silicon-zinc mixed solution and the high molecular polymer solution to prepare the spinning solution.
And preparing a silicon-zinc mixed fiber precursor by using the spinning solution through an electrostatic spinning method. The spinning solution is poured into a liquid tank of a needleless electrostatic spinning machine for electrostatic spinning, and relevant parameters are as follows: the positive voltage is 12kv, the negative voltage is 5kv, the rotating speed of the needle is 120r/min, the distance from the receiving device to the needle is 15cm, and the rotating speed of the receiving device is 50 r/min.
Taking out the silicon-zinc mixed fiber precursor, drying in a vacuum drying oven, putting into a muffle furnace, heating to 700 ℃ in an inert gas atmosphere, preserving heat for 2h, naturally cooling to room temperature, and preparing to obtain ZnO/SiO 2 A composite fiber material.
Referring to FIG. 1, the prepared ZnO/SiO 2 The fiber diameter of the composite fiber material is 0.5-1 um.
Referring to FIG. 3, ZnO/SiO obtained by the above comparative example 2 The effective antibacterial effect of the composite fiber material on escherichia coli is 90%. The novel composite sterilization fiber material has a perfect removal effect on sterilization.
ZnO/SiO 2 The sterilization principle of the composite fiber material is as follows:
ZnO/SiO 2 the composite fiber material slowly releases zinc ions in the use process, when the zinc ions reach cell membranes, the zinc ions are firmly adsorbed on the cell membranes by virtue of coulomb force because the cell membranes have negative charges, and the zinc ions can further penetrate through cell walls to enter pathogenic bacteria and react with sulfhydryl (-SH) and amino (-NH) groups existing in proteins and nucleic acids in organisms 2 ) And the functional groups containing sulfur and ammonia react to coagulate bacterial protein, destroy the activity of bacterial cell synthetase and make the cell lose division and proliferation capacity and finally die. In addition, when the bacteria lose activity, zinc ions are dissociated from the bacteria, and the sterilization activity is continuously repeated, so that the lasting antibacterial effect is maintained.
Comparative example
Weighing 7g of ethyl orthosilicate and 3.5g of lactic acid, adding the ethyl orthosilicate and the lactic acid into 100ml of ethanol-water mixed solution, placing the mixture into a conical flask, sealing, stirring and mixing the mixture, carrying out water bath at 45 ℃, and stirring for 2 hours to obtain a silicon solution.
5g of PVA was weighed and dissolved in a solvent under stirring to prepare a high molecular polymer solution.
And mixing and stirring the silicon solution and the high molecular polymer solution to prepare the spinning solution.
And preparing a silicon fiber precursor by using the spinning solution through an electrostatic spinning method. The spinning solution is poured into a liquid tank of a needleless electrostatic spinning machine for electrostatic spinning, and relevant parameters are as follows: the positive voltage is 12kv, the negative voltage is 5kv, the rotating speed of the needle is 120r/min, the distance from the receiving device to the needle is 15cm, and the rotating speed of the receiving device is 50 r/min.
Mixing SiO 2 Taking out the composite fiber material precursor, drying in a vacuum drying oven, putting into a muffle furnace, preserving heat at 700 ℃ for 2h, naturally cooling to room temperature, and preparing to obtain SiO 2 Composite fibrous material (see fig. 2).
Referring to FIG. 4, SiO produced 2 The effective antibacterial effect of the composite fiber material on escherichia coli is 0%. Indicating that the common silicon dioxide fiber has almost no antibacterial effect.
Compared with the prior art, the novel composite bactericidal fiber material and the preparation method thereof have the beneficial effects that:
ZnO/SiO prepared by the invention 2 The composite bactericidal fiber material is prepared by taking silicon dioxide silicon nanofiber as a substrate material and modifying the silicon dioxide silicon nanofiber by using zinc oxide 2 The antibacterial effect is achieved by compounding the antibacterial fiber material. ZnO/SiO prepared by the invention 2 The composite bactericidal fiber material not only has the function of sterilizing at room temperature, but also has excellent durability. In addition, SiO 2 As a supporting framework structure, the steel plate has the characteristics of high strength, corrosion resistance, high temperature resistance and the like. ZnO/SiO prepared by the invention 2 The composite bactericidal fiber material has low cost, simple preparation process and high strength, and is suitable for industrial production and application.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is specific and detailed, but not to be understood as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
Claims (10)
1. A preparation method of a novel bactericidal fiber material is characterized by comprising the following steps:
mixing and stirring a silicon source, lactic acid and a zinc source, and dissolving the mixture in ethanol and water to prepare a silicon-zinc mixed solution;
stirring and dissolving a high molecular polymer in a solvent to prepare a high molecular polymer solution;
mixing the silicon-zinc mixed solution with the high molecular polymer solution, and stirring to prepare a spinning solution;
preparing a silicon-zinc mixed fiber precursor by using a spinning solution through an electrostatic spinning method, taking out the silicon-zinc mixed fiber precursor, drying, heating the fiber in an inert gas atmosphere, preserving heat, and naturally cooling to obtain ZnO/SiO 2 A composite fiber material.
2. The method for preparing a novel bactericidal fiber material according to claim 1, characterized in that: mixing and stirring a silicon source, lactic acid and a zinc source, and dissolving the mixture in ethanol and water, wherein the molar mass ratio of the total amount of the silicon source, the lactic acid and the zinc source to the total amount of the ethanol and the water is 1: 1-2;
mixing and stirring a silicon source, lactic acid and a zinc source according to a molar mass ratio of 2:1: 2;
the molar mass ratio of the ethanol to the water is 2-3: 1.
3. The method for preparing the novel bactericidal fiber material according to claim 2, characterized in that: the silicon source is one or a combination of tetraethoxysilane and methyl orthosilicate;
the zinc source is one or more of zinc acetate, zinc sulfate and stannic chloride.
4. The method for preparing the novel bactericidal fiber material according to claim 1, characterized in that: the solvent is ethanol and water, and the molar mass ratio of the ethanol to the water is 1: 0.5-2.
5. The method for preparing a novel bactericidal fiber material according to claim 1, characterized in that: the molar mass ratio of the silicon-zinc mixed solution to the high molecular polymer solution is 1: 1-2.
6. The method for preparing a novel bactericidal fiber material according to claim 1, characterized in that: the molecular polymer is PVA, and the mass content of the molecular polymer in the high molecular polymer solution is 5-15%.
7. The method for preparing a novel bactericidal fiber material according to any one of claims 1 to 6, characterized in that: the preparation method of the silicon-zinc mixed fiber precursor by using the spinning solution through an electrostatic spinning method comprises the following steps: pouring the spinning solution into a liquid tank of a needleless electrostatic spinning machine for electrostatic spinning, wherein the relevant parameters are as follows: the positive voltage is 12kv, the negative voltage is 5kv, the rotating speed of the needle is 120r/min, the distance from the receiving device to the needle is 15cm, and the rotating speed of the receiving device is 50 r/min.
8. The method for preparing a novel bactericidal fiber material according to any one of claims 1 to 6, characterized in that: taking out the fiber, drying in a vacuum drying box, putting the fiber into a muffle furnace, heating to 500-800 ℃ in an inert gas atmosphere, preserving the heat for 0.5-2h, and naturally cooling to room temperature to prepare ZnO/SiO 2 A composite fiber material.
9. The method for preparing a novel bactericidal fiber material according to claim 8, characterized in that: prepared ZnO/SiO 2 The fiber diameter of the composite fiber material is 0.5-1 um.
10. A novel bactericidal fiber material is characterized in that: prepared by the method for preparing the novel bactericidal fiber material according to any one of claims 1 to 9.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114588317A (en) * | 2022-03-09 | 2022-06-07 | 诺一迈尔(苏州)生命科技有限公司 | Flexible inorganic nanofiber composite scaffold and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102733005A (en) * | 2012-05-16 | 2012-10-17 | 青岛科技大学 | Preparation method for hollow SiO2/ZnO composite nanofibers |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102733005A (en) * | 2012-05-16 | 2012-10-17 | 青岛科技大学 | Preparation method for hollow SiO2/ZnO composite nanofibers |
Non-Patent Citations (3)
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| HONG-DI ZHANG ET AL.: "Electrospun ZnO/SiO2 hybrid nanofibers for flexible pressure sensor", no. 51, pages 085102 * |
| XIN ZHANG: "In situ Generation of Well-Dispersed ZnO Quantum Dots on Electrospun Silica Nanotubes with High Photocatalytic Activity", pages 785 - 790 * |
| 徐姝颖: "《抗菌性氧化锌薄膜材料》", 冶金工业出版社, pages: 12 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114588317A (en) * | 2022-03-09 | 2022-06-07 | 诺一迈尔(苏州)生命科技有限公司 | Flexible inorganic nanofiber composite scaffold and preparation method thereof |
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