CN115613349B - ZnO-loaded fluorinated SiO 2 Fiber and preparation method and application thereof - Google Patents
ZnO-loaded fluorinated SiO 2 Fiber and preparation method and application thereof Download PDFInfo
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- CN115613349B CN115613349B CN202211173238.5A CN202211173238A CN115613349B CN 115613349 B CN115613349 B CN 115613349B CN 202211173238 A CN202211173238 A CN 202211173238A CN 115613349 B CN115613349 B CN 115613349B
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- 239000000835 fiber Substances 0.000 title claims abstract description 64
- 229910004298 SiO 2 Inorganic materials 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000243 solution Substances 0.000 claims abstract description 42
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000002243 precursor Substances 0.000 claims abstract description 23
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 14
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 14
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000011701 zinc Substances 0.000 claims description 25
- 238000003756 stirring Methods 0.000 claims description 15
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 10
- DXODQEHVNYHGGW-UHFFFAOYSA-N 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-heptadecafluorooctyl-tris(trifluoromethoxy)silane Chemical group FC(F)(F)O[Si](OC(F)(F)F)(OC(F)(F)F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F DXODQEHVNYHGGW-UHFFFAOYSA-N 0.000 claims description 7
- 229940057499 anhydrous zinc acetate Drugs 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 7
- DJWUNCQRNNEAKC-UHFFFAOYSA-L zinc acetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O DJWUNCQRNNEAKC-UHFFFAOYSA-L 0.000 claims description 7
- 230000000845 anti-microbial effect Effects 0.000 claims description 6
- 229940089951 perfluorooctyl triethoxysilane Drugs 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 239000004599 antimicrobial Substances 0.000 claims description 3
- 238000001523 electrospinning Methods 0.000 claims description 3
- 239000004744 fabric Substances 0.000 claims description 3
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 19
- 230000003115 biocidal effect Effects 0.000 abstract description 2
- 229910052731 fluorine Inorganic materials 0.000 abstract description 2
- 239000011737 fluorine Substances 0.000 abstract description 2
- 239000012784 inorganic fiber Substances 0.000 abstract description 2
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 abstract 1
- 239000002121 nanofiber Substances 0.000 description 14
- 239000000463 material Substances 0.000 description 5
- 241000191967 Staphylococcus aureus Species 0.000 description 3
- 239000006916 nutrient agar Substances 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- 241000588724 Escherichia coli Species 0.000 description 2
- 239000003242 anti bacterial agent Substances 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 208000035143 Bacterial infection Diseases 0.000 description 1
- 241000192125 Firmicutes Species 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 206010035148 Plague Diseases 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 241000607479 Yersinia pestis Species 0.000 description 1
- 208000022362 bacterial infectious disease Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 description 1
- 230000014599 transmission of virus Effects 0.000 description 1
Classifications
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/44—Oxides or hydroxides of elements of Groups 2 or 12 of the Periodic System; Zincates; Cadmates
-
- 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
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
Abstract
The invention belongs to the technical field of inorganic fiber antibiosis, and provides a ZnO-loaded fluorinated SiO 2 A fiber and a preparation method and application thereof. The preparation method comprises the following steps: s1, mixing tetraethoxysilane, hydrochloric acid solution, ethanol and water, and reacting to obtain SiO 2 Sol; s2, siO 2 Mixing sol and fluoride, reacting, and obtaining fluorinated SiO by using electrostatic spinning technology after the reaction is finished 2 A fiber; s3, fluoridize SiO 2 Adding the fiber into Zn precursor solution to perform hydrothermal reaction to obtain ZnO-loaded fluorinated SiO 2 And (3) fibers. ZnO-loaded fluorinated SiO prepared by the method 2 The fiber contains double active components ZnO and fluorine, so that the ZnO-loaded fluorinated SiO 2 The antibacterial property of the fiber is longer and more durable.
Description
Technical Field
The invention relates to the technical field of inorganic fiber antibiosis, in particular to a ZnO-loaded fluorinated SiO 2 A fiber and a preparation method and application thereof.
Background
Currently, diseases caused by bacterial infection or viral transmission present humans with an increasing threat of safety and health, which again plague us in different forms, resulting in tremendous loss of human lives and properties. The wide use of antimicrobial materials has led to an increasing awareness and safety awareness of people for healthy life.
In the research of inorganic antibacterial nano-fibers, siO 2 The nanofiber has a plurality of unique properties such as large specific surface area, low heat conductivity coefficient, chemical inertness, good biocompatibility, safety and no toxicity, and SiO 2 The microporous environment in the nanofibers can provide support for slow release of the antimicrobial component. SiO (SiO) 2 The excellent performance of the nanofiber can lead the nanofiber to be widely applied to sensingA catalyst, a conductive fiber, biomedicine and the like. Furthermore, siO 2 The nanofiber does not show any inherent Raman characteristic peak in the surface enhanced Raman scattering detection, which makes the nanofiber an ideal matrix material, namely SiO 2 The biocompatibility of nanofibers makes them particularly attractive in the biomedical field, especially in wound dressing, medical hygiene, tissue engineering and even food packaging. However, pure SiO 2 Nanofibers have significant hydrophilicity, which is difficult to achieve anti-adhesion properties of bacteria on the surface. Therefore, hydrophobic materials must be selected to chemically modify the surface to provide a hydrophobic interface.
Among various inorganic antibacterial agents, nano ZnO has been verified to have good antibacterial activity against gram-positive bacteria and gram-negative bacteria. In addition, znO is widely used in the fields of foods, cosmetics and medicines due to its safety and biocompatibility. However, no mature theoretical research and practical application have yet been carried out so far that ZnO and SiO 2 The nanofiber is simultaneously applied to the antibacterial material.
Thus, how to do with pure SiO 2 Modifying the nanofiber and modifying the modified SiO 2 The simultaneous application of nanofibers and ZnO in antimicrobial materials is a problem that needs to be addressed by those skilled in the art.
Disclosure of Invention
In view of this, the present invention provides a ZnO-supported fluorinated SiO 2 The fiber and the preparation method and application thereof aim to solve the technical problems of poor antibacterial effect and short antibacterial time of the existing inorganic antibacterial agent.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the invention provides a ZnO-loaded fluorinated SiO 2 A method of making a fiber comprising the steps of:
s1, mixing tetraethoxysilane, hydrochloric acid solution, ethanol and water, and reacting to obtain SiO 2 Sol;
S2、SiO 2 mixing sol and fluoride, reacting, and using electrostatic spinning technologyObtaining fluorinated SiO by operation 2 A fiber;
s3, fluoridize SiO 2 Adding the fiber into Zn precursor solution to perform hydrothermal reaction to obtain ZnO-loaded fluorinated SiO 2 And (3) fibers.
Further, in the step S1, the volume ratio of the tetraethoxysilane, the hydrochloric acid solution, the ethanol and the water is 60 to 80: 6-8: 20 to 27: 12-20.
Further, in the step S1, the mass concentration of the hydrochloric acid solution is 1-5%; the reaction temperature is 60-90 ℃, and the reaction time is 2-4 hours; the reaction is carried out under stirring conditions, and the stirring speed is 300-800 rpm.
Further, in the step S2, the fluoride is perfluorooctyl trimethoxysilane and/or 1h,2 h-perfluorooctyl triethoxysilane; the reaction time is 0.1-0.5 h;
the SiO is 2 The mass ratio of the sol to the fluoride is 1-5: 1.
further, in the step S2, the conditions of the electrospinning technique are as follows: the voltage of the positive electrode is 10-30 kV, the working distance is 10-20 cm, and the flow rate of the solution is 1-5 mL/h.
In step S3, the temperature of the hydrothermal reaction is 120-180 ℃, and the time of the hydrothermal reaction is 10-20 hours.
Further, in the step S3, the Zn source in the Zn precursor solution is anhydrous zinc acetate and/or anhydrous zinc nitrate; the mass concentration of the Zn precursor solution is 0.1-0.5%.
Further, in the step S3, siO is fluorinated 2 The mass volume ratio of the fiber to the Zn precursor solution is 1g: 1-5 mL.
The invention provides the ZnO-loaded fluorinated SiO prepared by the preparation method 2 And (3) fibers.
The invention also provides the ZnO-loaded fluorinated SiO 2 Use of a fiber for the preparation of an antimicrobial fabric.
Compared with the prior art, the invention has the following beneficial effects:
1. in the present inventionIn the light, the fluoride makes the fiber have stronger hydrophobicity, so that the fiber is endowed with remarkable antibacterial adhesion activity; the dual active components ZnO and fluorine coexist, so that the ZnO-loaded fluorinated SiO prepared by the invention 2 The antibacterial performance of the fiber is longer and more durable;
2. the preparation method has the advantages that no polymer material is added in the preparation process, so that the characteristics of the pure inorganic nano fiber are ensured, and the pure inorganic nano fiber has good biocompatibility;
3. ZnO-loaded fluorinated SiO prepared by the method 2 The fiber can achieve double antibacterial effects of rejection/contact from the antibacterial mechanism, and has more remarkable antibacterial effect than a single rejection type or contact type antibacterial material.
Drawings
FIG. 1 is a ZnO-supported fluorinated SiO prepared in example 1 of the present invention 2 SEM image of the fiber.
Detailed Description
The invention provides a ZnO-loaded fluorinated SiO 2 A method of making a fiber comprising the steps of:
s1, mixing tetraethoxysilane, hydrochloric acid solution, ethanol and water, and reacting to obtain SiO 2 Sol;
S2、SiO 2 mixing sol and fluoride, reacting, and obtaining fluorinated SiO by using electrostatic spinning technology after the reaction is finished 2 A fiber;
s3, fluoridize SiO 2 Adding the fiber into Zn precursor solution to perform hydrothermal reaction to obtain ZnO-loaded fluorinated SiO 2 And (3) fibers.
In the present invention, in the step S1, the volume ratio of the tetraethoxysilane, the hydrochloric acid solution, the ethanol and the water is 60 to 80: 6-8: 20 to 27:12 to 20, preferably 62 to 77:6.5 to 7.5: 22-26: 13 to 17, more preferably 66 to 72:7:23 to 25:14 to 16.
In the present invention, in the step S1, the mass concentration of the hydrochloric acid solution is 1 to 5%, preferably 2 to 4%, and more preferably 3%; the reaction temperature is 60-90 ℃, preferably 65-85 ℃, and more preferably 70-80 ℃; the reaction time is 2 to 4 hours, preferably 2.5 to 3.5 hours, and more preferably 3 hours; the reaction is carried out under stirring at a rotation speed of 300 to 800rpm, preferably 400 to 700rpm, more preferably 500 to 600rpm.
In the present invention, in the step S2, the fluoride is perfluorooctyl trimethoxysilane and/or 1h,2 h-perfluorooctyl triethoxysilane, preferably perfluorooctyl trimethoxysilane; the reaction time is 0.1 to 0.5h, preferably 0.2 to 0.4h, and more preferably 0.3h; the reaction is carried out under the room temperature condition; the SiO is 2 The mass ratio of the sol to the fluoride is 1-5: 1.
in the present invention, in the step S2, the conditions of the electrospinning technique are as follows: the positive electrode voltage is 10 to 30kV, preferably 15 to 25kV, and more preferably 20kV; the working distance is 10-20 cm, preferably 12-18 cm, and more preferably 14-16 cm; the flow rate of the solution is 1 to 5mL/h, preferably 2 to 4mL/h, and more preferably 3mL/h.
In the present invention, in the step S3, the temperature of the hydrothermal reaction is 120 to 180 ℃, preferably 130 to 160 ℃, and more preferably 140 to 150 ℃; the hydrothermal reaction time is 10 to 20 hours, preferably 12 to 18 hours, and more preferably 14 to 16 hours.
In the present invention, in the step S3, the Zn source in the Zn precursor solution is anhydrous zinc acetate and/or anhydrous zinc nitrate, preferably anhydrous zinc acetate; the mass concentration of the Zn precursor solution is 0.1 to 0.5%, preferably 0.2 to 0.4%, and more preferably 0.3%.
In the present invention, in the step S3, siO is fluorinated 2 The mass volume ratio of the fiber to the Zn precursor solution is 1g: 1-5 mL.
The invention provides the ZnO-loaded fluorinated SiO prepared by the preparation method 2 And (3) fibers.
The invention also provides the ZnO-loaded fluorinated SiO 2 Use of a fiber for the preparation of an antimicrobial fabric.
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
63 parts of ethyl orthosilicate, 6.7 parts of HCl with the mass concentration of 1 percent, 24 parts of ethanol and 14 parts of water are mixed and added into a reaction system, and stirred for 2.5 hours under the stirring condition of 450rpm at 65 ℃ to obtain SiO 2 Sol;
SiO is made of 2 Sol and perfluoro octyl trimethoxy silane according to the mass ratio of 3:1, stirring for 0.1h at room temperature, and performing electrostatic spinning to obtain fluorinated SiO 2 The fiber, wherein the conditions of the electrostatic spinning are as follows: the voltage of the positive electrode is 20kV, the working distance is 15cm, and the flow rate of the solution is 3mL/h;
preparing Zn precursor solution with mass concentration of 0.1% by using anhydrous zinc acetate, and fluorinating SiO 2 The mass volume ratio of the fiber is 1g:1mL of the ZnO-loaded fluorinated SiO is added into the Zn precursor solution, and the ZnO-loaded fluorinated SiO is obtained after hydrothermal reaction for 14h at the temperature of 125 DEG C 2 And (3) fibers.
FIG. 1 shows a ZnO-supported fluorinated SiO prepared in this example 2 SEM image of the fiber, as can be seen from fig. 1, znO nanoparticles were successfully loaded to fluorinated SiO 2 The surface of the fiber.
Example 2
66 parts of tetraethoxysilane, 7 parts of HCl with the mass concentration of 2%, 22 parts of ethanol and 15 parts of water are mixed and added into a reaction system, and stirred for 3 hours under the stirring condition of 500rpm at 70 ℃ to obtain SiO 2 Sol;
SiO is made of 2 Sol and 1H, 2H-perfluoro octyl triethoxysilane according to the mass ratio of 1:1, stirring for 0.2h at room temperature, and performing electrostatic spinning to obtain fluorinated SiO 2 The fiber, wherein the conditions of the electrostatic spinning are as follows: the positive voltage is 22kV, the working distance is 14cm, and the solution flow rate is 3mL/h;
preparing Zn precursor solution with mass concentration of 0.2% by using anhydrous zinc acetate, and fluorinating SiO 2 The mass volume ratio of the fiber is 1g:2mL was added to the Zn precursor solution,hydrothermal reaction is carried out for 12 hours at 130 ℃ to obtain ZnO-loaded fluorinated SiO 2 And (3) fibers.
Example 3
68 parts of tetraethoxysilane, 8 parts of HCl with the mass concentration of 3%, 25 parts of ethanol and 16 parts of water are mixed and added into a reaction system, and stirred for 3 hours under the stirring condition of 600rpm at 75 ℃ to obtain SiO 2 Sol;
SiO is made of 2 Sol and perfluoro octyl trimethoxy silane according to the mass ratio of 2:1, stirring for 0.3h at room temperature, and performing electrostatic spinning to obtain fluorinated SiO 2 The fiber, wherein the conditions of the electrostatic spinning are as follows: the positive electrode voltage is 25kV, the working distance is 16cm, and the solution flow rate is 3mL/h;
preparing Zn precursor solution with mass concentration of 0.3% by using anhydrous zinc acetate, and fluorinating SiO 2 The mass volume ratio of the fiber is 1g:3mL of the ZnO-loaded fluorinated SiO is added into the Zn precursor solution, and the ZnO-loaded fluorinated SiO is obtained after hydrothermal reaction for 13h at 140 DEG C 2 And (3) fibers.
Example 4
75 parts of ethyl orthosilicate, 6 parts of HCl with the mass concentration of 4%, 26 parts of ethanol and 18 parts of water are mixed and added into a reaction system, and stirred for 3 hours under the stirring condition of 650rpm at 80 ℃ to obtain SiO 2 Sol;
SiO is made of 2 Sol and 1H, 2H-perfluoro octyl triethoxysilane according to the mass ratio of 4:1, stirring for 0.4h at room temperature, and performing electrostatic spinning to obtain fluorinated SiO 2 The fiber, wherein the conditions of the electrostatic spinning are as follows: the positive electrode voltage is 15kV, the working distance is 12cm, and the solution flow rate is 4mL/h;
preparing Zn precursor solution with mass concentration of 0.4% by using anhydrous zinc nitrate, and fluorinating SiO 2 The mass volume ratio of the fiber is 1g:4mL of the ZnO-loaded fluorinated SiO is added into the Zn precursor solution, and the ZnO-loaded fluorinated SiO is obtained after hydrothermal reaction for 16h at 150 DEG C 2 And (3) fibers.
Example 5
80 parts of tetraethoxysilane, 6 parts of HCl with the mass concentration of 5%, 20 parts of ethanol and 20 parts of water are mixed and added into a reaction system, and stirred for 4 hours under the stirring condition of 400rpm at 90 ℃ to obtain SiO 2 Sol;
SiO is made of 2 Sol and perfluoro octyl trimethoxy silane according to the mass ratio of 5:1, stirring for 0.5h at room temperature, and performing electrostatic spinning to obtain fluorinated SiO 2 The fiber, wherein the conditions of the electrostatic spinning are as follows: the voltage of the positive electrode is 20kV, the working distance is 15cm, and the flow rate of the solution is 5mL/h;
preparing Zn precursor solution with mass concentration of 0.5% by using anhydrous zinc nitrate, and fluorinating SiO 2 The mass volume ratio of the fiber is 1g:5mL of the ZnO-loaded fluorinated SiO is added into the Zn precursor solution, and the ZnO-loaded fluorinated SiO is obtained after hydrothermal reaction for 10 hours at 180 DEG C 2 And (3) fibers.
Performance testing
ZnO-loaded fluorinated SiO prepared by the method 2 The antibacterial property of the fiber is tested by the following specific test steps: taking 7 identical nutrient agar culture mediums, and carrying ZnO-loaded fluorinated SiO prepared in examples 1-5 2 Fiber, common SiO 2 Fibers and fluorinated SiO 2 The fibers are respectively coated on nutrient agar culture mediums, 7 nutrient agar culture mediums are put into the same environment to culture escherichia coli and staphylococcus aureus, and different SiO's are verified by a plate counting method 2 The antibacterial effect of the fibers is shown in table 1.
TABLE 1 different SiOs 2 Antibacterial effect of fiber
| Sample of | Antibacterial ratio (Escherichia coli) | Antibacterial ratio (Staphylococcus aureus) |
| Example 1 | 100％ | 100％ |
| Example 2 | 100％ | 100％ |
| Example 3 | 100％ | 100％ |
| Example 4 | 100％ | 100％ |
| Example 5 | 100％ | 100％ |
| Plain SiO 2 Fiber | 3％ | 2％ |
| Fluorinated SiO 2 Fiber | 65％ | 63％ |
As can be obtained from Table 1, znO-supported fluorinated SiO prepared by the present invention 2 The fiber has higher antibacterial rate to colibacillus and staphylococcus aureus, which indicates that the ZnO-loaded fluorinated SiO 2 The fiber has excellent broad-spectrum antibacterial activity.
In the present specification, each embodiment is described in a progressive manner, and each embodiment is mainly described in a different point from other embodiments, and identical and similar parts between the embodiments are all enough to refer to each other.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. ZnO-loaded fluorinated SiO 2 A method of making a fiber comprising the steps of:
s1, mixing tetraethoxysilane, hydrochloric acid solution, ethanol and water, and reacting to obtain SiO 2 Sol;
S2、SiO 2 mixing sol and fluoride, reacting, and obtaining fluorinated SiO by using electrostatic spinning technology after the reaction is finished 2 A fiber;
s3, fluoridize SiO 2 Adding the fiber into Zn precursor solution to perform hydrothermal reaction to obtain ZnO-loaded fluorinated SiO 2 A fiber;
the fluoride is perfluorooctyl trimethoxysilane and/or 1H, 2H-perfluorooctyl triethoxysilane;
in the step S3, a Zn source in the Zn precursor solution is anhydrous zinc acetate and/or anhydrous zinc nitrate; the mass concentration of the Zn precursor solution is 0.1-0.5%.
2. The preparation method according to claim 1, wherein in the step S1, the volume ratio of the ethyl orthosilicate, the hydrochloric acid solution, the ethanol and the water is 60-80: 6-8: 20 to 27: 12-20.
3. The preparation method according to claim 2, wherein in the step S1, the mass concentration of the hydrochloric acid solution is 1 to 5%; the reaction temperature is 60-90 ℃, and the reaction time is 2-4 hours; the reaction is carried out under stirring conditions, and the stirring speed is 300-800 rpm.
4. A method according to any one of claims 1 to 3, wherein in step S2, the reaction time is 0.1 to 0.5h; the SiO is 2 The mass ratio of the sol to the fluoride is 1-5: 1.
5. the method according to claim 4, wherein in the step S2, the condition of the electrospinning technique is: the voltage of the positive electrode is 10-30 kV, the working distance is 10-20 cm, and the flow rate of the solution is 1-5 mL/h.
6. The method according to claim 1 or 5, wherein in the step S3, the hydrothermal reaction is performed at a temperature of 120 to 180 ℃ for a period of 10 to 20 hours.
7. The method according to claim 6, wherein in the step S3, siO is fluorinated 2 The mass volume ratio of the fiber to the Zn precursor solution is 1g: 1-5 mL.
8. ZnO-supported fluorinated SiO produced by the production method according to any one of claims 1 to 7 2 And (3) fibers.
9. The ZnO-supported fluorinated SiO of claim 8 2 Use of a fiber for the preparation of an antimicrobial fabric.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101481855A (en) * | 2008-11-27 | 2009-07-15 | 江南大学 | Preparation of silicon dioxide / polyvinylidene fluoride composite nano fiber film |
| CN102013516A (en) * | 2010-10-22 | 2011-04-13 | 浙江大学 | Porous fiber gel polymer electrolyte and preparation method thereof |
| CN102652903A (en) * | 2012-05-03 | 2012-09-05 | 东华大学 | Preparation method of high temperature resistant silicon dioxide nanometer fiber filtering membrane |
| CN103820945A (en) * | 2014-03-12 | 2014-05-28 | 东华大学 | Preparation method of organic/inorganic hybridization nano super-hydrophobic fiber film |
| CN108797094A (en) * | 2018-06-11 | 2018-11-13 | 成都新柯力化工科技有限公司 | A kind of composite membrane and preparation method for flexible piezoelectric material |
| CN112626641A (en) * | 2020-12-10 | 2021-04-09 | 新疆理工学院 | Method for preparing fluffy flexible three-dimensional silicon dioxide nano-fibers in one step by template-free method |
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- 2022-09-26 CN CN202211173238.5A patent/CN115613349B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101481855A (en) * | 2008-11-27 | 2009-07-15 | 江南大学 | Preparation of silicon dioxide / polyvinylidene fluoride composite nano fiber film |
| CN102013516A (en) * | 2010-10-22 | 2011-04-13 | 浙江大学 | Porous fiber gel polymer electrolyte and preparation method thereof |
| CN102652903A (en) * | 2012-05-03 | 2012-09-05 | 东华大学 | Preparation method of high temperature resistant silicon dioxide nanometer fiber filtering membrane |
| CN103820945A (en) * | 2014-03-12 | 2014-05-28 | 东华大学 | Preparation method of organic/inorganic hybridization nano super-hydrophobic fiber film |
| CN108797094A (en) * | 2018-06-11 | 2018-11-13 | 成都新柯力化工科技有限公司 | A kind of composite membrane and preparation method for flexible piezoelectric material |
| CN112626641A (en) * | 2020-12-10 | 2021-04-09 | 新疆理工学院 | Method for preparing fluffy flexible three-dimensional silicon dioxide nano-fibers in one step by template-free method |
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