CN111068406A - Antibacterial nanofiber filtering material and preparation method thereof - Google Patents
Antibacterial nanofiber filtering material and preparation method thereof Download PDFInfo
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- CN111068406A CN111068406A CN201911362747.0A CN201911362747A CN111068406A CN 111068406 A CN111068406 A CN 111068406A CN 201911362747 A CN201911362747 A CN 201911362747A CN 111068406 A CN111068406 A CN 111068406A
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- antibacterial
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/14—Other self-supporting filtering material ; Other filtering material
- B01D39/16—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres
- B01D39/1607—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous
- B01D39/1623—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous of synthetic origin
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/0001—Making filtering elements
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/0027—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours with additional separating or treating functions
- B01D46/0028—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours with additional separating or treating functions provided with antibacterial or antifungal means
Abstract
The invention discloses a preparation method of an antibacterial nanofiber filtering material, which comprises the following steps: adding silver nitrate and a stabilizer into a liquid reducing agent, stirring until the silver nitrate and the stabilizer are dissolved, adding a polymer, stirring until the polymer is dissolved, standing and defoaming for 6-8 hours; preparing the defoamed polymer/silver solution into nano fibers by adopting an electrostatic spinning technology; and naturally drying the nano-fibers under the dark condition until the reducing agent is completely volatilized to obtain the antibacterial nano-fiber filtering material. The antibacterial nanofiber filtering material has high-efficiency filtering performance and long-acting antibacterial performance, and can be widely applied to the fields of masks for medical protection and high-efficiency air filtration.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a preparation method of a nano fiber filtering material with an antibacterial function.
Background
The air filtering materials commonly used at present are non-woven materials, have large fiber diameter and large pore diameter, do not have the antibacterial function, and have the PM resistance10And PM2.5The filtering effect is better, the interception effect is not good for dust particles with the particle size less than 2.5 mu m, and the dust particles with smaller particle size are easier to enter the human body through a respiratory system, so that the probability of lung cancer, cardiovascular diseases, respiratory tract infection and other diseases is increased, and in addition, the environmental pollution is causedAnd a large amount of harmful bacteria are bred in the air, so that the health of people is further harmed. Therefore, the prepared efficient air filtering material with the antibacterial function can effectively isolate harmful substances in the air from continuously causing harm to the health of people.
As a new material showing great potential in all aspects, a nano material has also been widely used in the research of air filtration materials, in which a nano fiber material prepared using an electrospinning technique exhibits excellent filtration performance in the air filtration field due to having a small fiber diameter, a large specific surface area, and a porosity.
Silver particles, as one of inorganic antibacterial materials, have been extensively used in the research of antibacterial materials due to their optimal antibacterial properties, ease of preparation and no other harmful side effects. Patent CN103520999B discloses a preparation method of an antibacterial composite nanofiber high-efficiency air filter material, which sequentially comprises a non-woven fabric support layer, an antibacterial fiber and micron fiber blended filter layer and a nanofiber filter layer. Patent CN108251965A discloses an antibacterial nanofiber membrane and a preparation method thereof, which is characterized in that a chitosan nanofiber membrane is prepared by using an electrostatic spinning technology, and antibacterial particles are loaded on the nanofiber membrane through cross-linking treatment, the preparation method is complex, the conditions are uncontrollable, and the antibacterial particles loaded on the nanofiber membrane are easy to fall off to lose antibacterial performance.
Disclosure of Invention
The invention aims to provide an antibacterial nanofiber filtering material and a preparation method thereof.
In order to solve the technical problems, the invention provides a preparation method of an antibacterial nanofiber filtering material, which comprises the following steps:
1) adding silver nitrate and a stabilizer into a reducing agent (a liquid reducing agent), and stirring under a dark condition (room temperature and no light condition) until the silver nitrate and the stabilizer are dissolved in the reducing agent to obtain a solution containing silver particles;
silver nitrate: stabilizer 1: 1-3 mass ratio;
2) according to the polymer: 0.06-0.16% of reducing agent: 1 (preferably 0.10-0.12: 1) by mass, adding the polymer into the silver particle-containing solution;
then stirring the mixture under a dark condition (without light at room temperature) until the polymer is completely dissolved, and standing and defoaming the mixture for 6 to 8 hours; obtaining a defoamed polymer/silver solution;
namely, the step 1) and the step 2) are carried out at room temperature and under the condition of keeping out of the sun;
3) preparing the defoamed polymer/silver solution into nano-fibers by adopting an electrostatic spinning technology;
4) and drying (naturally drying) the nano-fiber obtained in the step 3) under the dark condition until the reducing agent is completely volatilized (the drying time is about 12 hours), so as to obtain the antibacterial nano-fiber filtering material.
As an improvement of the preparation method of the antibacterial nanofiber filter material, the preparation method comprises the following steps of 1):
the reducing agent is N, N-dimethylformamide, dimethylacetamide, tetrahydrofuran, dichloromethane, acetone or dimethyl sulfoxide;
the stabilizer is polyethylene glycol, polyvinylpyrrolidone, polymethyl methacrylate, and chitosan.
The preparation method of the antibacterial nanofiber filter material is further improved as follows:
the polymer in the step 2) is polyvinylidene fluoride.
In a preferred embodiment of the present invention, the amount of silver nitrate in 18g of N, N-dimethylformamide (as a reducing agent) is generally 0.04 to 0.2 g.
As a further improvement of the preparation method of the antibacterial nanofiber filter material, the step 3) is as follows:
extracting polymer/silver solution by using a medical sterile 10ml syringe, and preparing the nano-fiber by adopting an electrostatic spinning technology, wherein the spinning parameters are as follows: the voltage is 12-26 kv, the distance between electrodes is 13-20 cm, the spinning supply amount is 0.1-1 ml/h, the ambient temperature (spinning temperature) is 15-55 ℃, and the ambient humidity is 15-60%.
As a further improvement of the preparation method of the antibacterial nanofiber filter material, the stabilizer and the polymer are required to be dried in vacuum before use. For example, drying the mixture in a vacuum oven at 55-65 ℃ for 6-12 h; thus, the silver nitrate: after drying, stabilizer 1: 1-3 mass ratio; polymer after drying: 0.06-0.16% of reducing agent: 1, mass ratio.
As a further improvement of the preparation method of the antibacterial nanofiber filtering material, the stirring in the step 1) and the stirring in the step 2) are magnetic stirring, and the rotating speed is 300-1200 r/min.
As a further improvement of the preparation method of the antibacterial nanofiber filtering material, double-needle electrostatic spinning is adopted in the step 3), and 4mL of spinning solution is contained in each needle.
As a further improvement of the preparation method of the antibacterial nanofiber filter material, the nanofiber receiving base material adopted by the electrostatic spinning in the step 3) is aluminum foil, release paper, non-woven material and glass fiber mesh.
As a further improvement of the preparation method of the antibacterial nanofiber filter material of the present invention,
the stirring time of the step 1) is about (3 +/-1) hours; the stirring time in step 2) was about (6. + -. 1) hours.
The invention also provides an antibacterial nanofiber filtering material prepared by any one of the methods.
The step 1) of the invention is to prepare nano silver particles by a liquid phase reduction method: in order to prevent the silver particles from agglomerating in the reduction process and enhance the stability of the nano silver particles, a proper amount of stabilizer needs to be added, and strong magnetic stirring is carried out for 3 +/-1 hours at room temperature under the condition of no illumination. The particle size of the nano silver particles prepared by the liquid phase reduction method is about 10nm (obtained by testing the ultraviolet visible absorption spectrum analysis of the silver particle-containing solution).
The polymer spinning solution containing silver particles (polymer/silver solution after defoaming) prepared by the invention has the viscosity of 3700-3850 mPa.s and the conductivity of 25.8-76 mu s/cm; the average pore diameter of the prepared nanofiber filtering material is 2-10 mu m, a special dendritic fiber is formed due to the addition of nano-silver particles, the average diameter of the dendritic fiber is 20-50 nm, the average diameter of the lower-layer supporting fiber is 90-140 nm, the filtering efficiency of the material to NaCl aerosol particles with the particle size of 0.26 mu m is higher than 99.9% when the airflow speed is 32LPM, the filtering resistance is 130-220 Pa, the quality factor can reach 0.0575 at most, the hydrophobic angle is higher than 120 degrees, the material has a high-efficiency antibacterial function to staphylococcus aureus and escherichia coli, and the antibacterial rate of the material to the two strains is higher than 99% after the material is placed for 1 month under natural illumination; has high and lasting antibacterial performance.
The filtering mechanism of the filtering material is mainly interception effect, Brown diffusion effect and static effect.
The preparation process is simple and has controllable conditions. The invention firstly utilizes a liquid phase reduction method to prepare nano silver particles, and prepares the antibacterial nano fiber filter material with a special dendritic structure by mixing the nano silver particles with a polymer spinning solution and utilizing an electrostatic spinning technology one-step method.
In the invention, the electrostatic spinning technology is utilized to directly and uniformly load the nano silver particles on the surface and inside of the polymer fiber, so that the prepared nano fiber filter material has high-efficiency filtering performance and long-acting antibacterial performance.
In conclusion, the electrostatic spinning technology used in the invention is an effective method for preparing superfine fibers, and the preparation process is simple and short in flow. The composite of the silver nanoparticles and the electrostatic spinning nanofibers is realized by utilizing the electrostatic spinning technology, the composite process is simple, the composite effect is good, the composite nanofiber material has high-efficiency filtering performance and long-acting antibacterial performance, and the composite nanofiber material can be widely applied to the fields of masks for medical protection and high-efficiency air filtration.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
FIG. 1 is a scanning electron microscope (X30000) of fibers of an antibacterial nanofiber filter material prepared in example 1 when 0.04g of silver nitrate and polyvinylpyrrolidone powder are used as stabilizers.
Detailed Description
The invention will be further described with reference to specific examples, but the scope of the invention is not limited thereto:
in the following case, the relative molecular mass of the polyvinylidene fluoride powder was 60 ten thousand, and the relative molecular mass of the polyvinylpyrrolidone powder was 5.8 ten thousand.
Example 1, a method for preparing an antibacterial nanofiber filter material, sequentially comprising the following steps:
(1) pretreatment: respectively placing polyvinylidene fluoride powder and polyvinylpyrrolidone powder in a vacuum oven to dry for 12h at 60 ℃;
all of the polyvinylidene fluoride powder and polyvinylpyrrolidone powder subjected to the vacuum drying treatment are as follows.
(2) Preparing silver particles: accurately weighing 0.04g of silver nitrate, 18g of N, N-dimethylformamide (as a reducing agent) and 0.04g of polyvinylpyrrolidone (for preventing silver particles precipitated by reduction from agglomerating) as a stabilizer by using an electronic balance, and adding the silver nitrate, the N, N-dimethylformamide and the polyvinylpyrrolidone into a beaker together, wherein the silver nitrate, the polyvinylpyrrolidone and the polyvinylpyrrolidone are AgNO3The crystal is easy to oxidize under natural illumination, so the beaker is wrapped and sealed by the tinfoil paper and stirred for 3 hours at room temperature; obtaining a solution containing silver particles;
namely, the step (2) is carried out under the condition of room temperature and light shielding;
(3) preparation of spinning solution: weighing 2g of polyvinylidene fluoride powder, and adding the polyvinylidene fluoride powder into the silver particle-containing solution (yellow transparent solution) obtained in the step (2);
wrapping the beaker with tinfoil paper again, sealing, stirring at room temperature for 6h until the solution is clear and transparent, standing and defoaming for 6h for later use; obtaining a defoamed polymer/silver solution;
namely, this whole step (3) is carried out under a condition of room temperature and protection from light;
(4) electrostatic spinning: adopting double-needle spinning, wherein the outer diameter of a needle is 0.7mm, the inner diameter of the needle is 0.4mm, a single injector respectively absorbs 4mL of defoamed polymer/silver solution, the spinning voltage is 18kV, the distance between a receiving device (a receiving roller) and the needle is 15cm, the solution propelling speed is 0.3mL/h, the spinning temperature is 20 +/-5 ℃, the relative humidity is 30 +/-5%, and a glass fiber mesh is adopted as a receiving material;
(5) shearing the prepared nanofiber material from a receiving roller, and drying the nanofiber material in a dark and shady place to constant weight (about 12 hours), wherein the reducing agent is completely volatilized; and obtaining the antibacterial nanofiber filtering material.
Example 2, a method for preparing an antibacterial nanofiber filter material,
the step (2) is changed into the following steps: adding 0.12g of silver nitrate, 18g of N, N-dimethylformamide and 0.12g of polyvinylpyrrolidone into a beaker together, wrapping and sealing the beaker by using tin foil paper, and stirring for 3 hours at room temperature to obtain a solution containing silver particles;
the rest is equivalent to embodiment 1.
Example 3, a method for preparing an antibacterial nanofiber filter material,
the step (2) is changed into the following steps: adding 0.2g of silver nitrate, 18g N, N-dimethylformamide and 0.2g of polyvinylpyrrolidone into a beaker together, wrapping and sealing the beaker by using tin foil paper, and stirring for 3 hours at room temperature to obtain a solution containing silver particles;
the rest is equivalent to embodiment 1.
Example 4, a method for preparing an antibacterial nanofiber filter material,
the step (2) is changed into the following steps: adding 0.12g of silver nitrate, 18g N, N-dimethylformamide and 0.24 of polyvinylpyrrolidone into a beaker together, wrapping and sealing the beaker by using tinfoil paper, and stirring for 3 hours at room temperature to obtain a silver particle-containing solution;
the rest is equivalent to embodiment 1.
Example 5a method of preparing an antibacterial nanofiber filter material,
the step (2) is changed into the following steps: adding 0.12g of silver nitrate, 18g of N, N-dimethylformamide and 0.36g of polyvinylpyrrolidone into a beaker together, wrapping and sealing the beaker with tinfoil paper, and stirring for 3 hours at room temperature to obtain a silver particle-containing solution;
the rest is equivalent to embodiment 1.
Experiment 1, viscosity and conductivity performance data of the polymer spinning solution containing silver particles (i.e., the defoamed polymer/silver solution) prepared in the above examples 1 to 5 are as follows:
TABLE 1
| Viscosity (mPa.s) | Conductivity (μ s/cm) | |
| Example 1 | 3850 | 25.8 |
| Example 2 | 3700 | 46 |
| Example 3 | 3800 | 76 |
| Example 4 | 3800 | 38 |
| Example 5 | 3750 | 37.5 |
Experiment 2, the antibacterial nanofiber filter materials prepared in the above examples 1 to 5 were subjected to fiber performance test according to the following method: analyzing the fiber diameter of the antibacterial nanofiber filtering material in a scanning electron microscope image by using imagepro-plus software, selecting 100 fibers for testing the fiber diameter and taking an average value, and taking 50 fibers for testing the dendritic fiber part and taking the average value; testing the filtering performance of the antibacterial nanofiber filtering material by adopting an American TSI8130 automatic filtering material detector; the antibacterial performance of the antibacterial nanofiber filter material is tested by GB/T21510-2008 'detection method of antibacterial performance of nano inorganic material-appendix B oscillation method'. The following table 2 shows the performance parameters of the composition:
TABLE 2 Performance parameters of antibacterial nanofiber Filter materials
The antibacterial nanofiber filter materials prepared in the above examples 1 to 5 still have the bacteriostasis rates of more than 99% to the above two strains after being placed for 1 month under natural illumination; therefore, the antibacterial agent has high-efficiency and durable antibacterial performance.
Comparative example 1, the polymer in example 2 is changed from polyvinylidene fluoride to polyvinyl alcohol, and the dosage is kept unchanged; the rest is equivalent to example 2.
Comparative example 2, the polymer in example 2 is replaced and polyvinylidene fluoride is changed into polyacrylonitrile, and the using amount is kept unchanged; the rest is equivalent to example 2.
Comparative example 1 and comparative example 2, tested according to the experimental procedure described above, the performance parameters are shown in tables 3 and 4 below:
TABLE 3
| Viscosity (mPa.s) | Conductivity (μ s/cm) | |
| Comparative example 1 | 3700 | 36 |
| Comparative example 2 | 3650 | 37.5 |
TABLE 4
The antibacterial nanofiber filter materials prepared in the comparative examples 1-2 have the antibacterial rates of the two strains which are lower than the antibacterial rate of the initial state to a certain extent after being placed for 1 month under natural illumination.
Therefore, the filtering performance and the bacteriostatic performance of the composite are inferior to those of the composite.
Finally, it is also noted that the above-mentioned lists merely illustrate a few specific embodiments of the invention. It is obvious that the invention is not limited to the above embodiments, but that many variations are possible. All modifications which can be derived or suggested by a person skilled in the art from the disclosure of the present invention are to be considered within the scope of the invention.
Claims (10)
1. The preparation method of the antibacterial nanofiber filter material is characterized by comprising the following steps of:
1) adding silver nitrate and a stabilizer into a reducing agent, and stirring in a dark condition until the silver nitrate and the stabilizer are dissolved in the reducing agent to obtain a solution containing silver particles;
silver nitrate: stabilizer 1: 1-3 mass ratio;
2) according to the polymer: 0.06-0.16% of reducing agent: 1, adding the polymer into a silver particle-containing solution;
then, stirring the mixture under a dark condition until the polymer is completely dissolved, and standing and defoaming the mixture for 6 to 8 hours; obtaining a defoamed polymer/silver solution;
3) preparing the defoamed polymer/silver solution into nano-fibers by adopting an electrostatic spinning technology;
4) and drying the nano-fiber obtained in the step 3) under the condition of keeping out of the sun until the reducing agent is completely volatilized, thereby obtaining the antibacterial nano-fiber filtering material.
2. The method for preparing antibacterial nanofiber filter material as claimed in claim 1, wherein in the step 1):
the reducing agent is N, N-dimethylformamide, dimethylacetamide, tetrahydrofuran, dichloromethane, acetone or dimethyl sulfoxide;
the stabilizer is polyethylene glycol, polyvinylpyrrolidone, polymethyl methacrylate, and chitosan.
3. The method for preparing antibacterial nanofiber filter material according to claim 2, characterized in that:
the polymer in the step 2) is polyvinylidene fluoride.
4. The method for preparing antibacterial nanofiber filter material as claimed in claim 3, wherein the step 3) is:
extracting polymer/silver solution by using a medical sterile 10ml syringe, and preparing the nano-fiber by adopting an electrostatic spinning technology, wherein the spinning parameters are as follows: the voltage is 12-26 kv, the distance between electrodes is 13-20 cm, the spinning supply amount is 0.1-1 ml/h, the ambient temperature is 15-55 ℃, and the ambient humidity is 15-60%.
5. The method for preparing an antibacterial nanofiber filter material as claimed in any one of claims 1 to 4, wherein the method comprises the following steps:
the stabilizer and the polymer are dried in vacuum before use.
6. The method for preparing an antibacterial nanofiber filter material as claimed in any one of claims 1 to 4, wherein the method comprises the following steps:
the stirring in the step 1) and the step 2) is magnetic stirring, and the rotating speed is 300-1200 r/min.
7. The method of claim 4, wherein the antibacterial nanofiber filter material is prepared by the following steps: in the step 3), double-needle electrostatic spinning is adopted, and 4mL of spinning solution is contained in each needle.
8. The method of claim 4, wherein the antibacterial nanofiber filter material is prepared by the following steps: the nanofiber receiving base material adopted by the electrostatic spinning in the step 3) is aluminum foil, release paper, non-woven material and glass fiber grids.
9. The preparation method of the antibacterial nanofiber filter material as claimed in claims 1-4, wherein the preparation method comprises the following steps: the stirring time in the step 1) is (3 +/-1) hours;
the stirring time of the step 2) is (6 +/-1) hours.
10. An antibacterial nanofiber filter material prepared by the method as claimed in any one of claims 1 to 9.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111514659A (en) * | 2020-05-04 | 2020-08-11 | 南通大学 | Nano cobweb antibacterial composite air filtering material and preparation method thereof |
| CN113789589A (en) * | 2021-10-08 | 2021-12-14 | 晋江市滨浪制衣织造有限公司 | Antibacterial protective knitted fabric and preparation process thereof |
| CN114875497A (en) * | 2022-04-28 | 2022-08-09 | 内蒙古工业大学 | Metal nano self-assembly fiber material, and preparation method and application thereof |
| WO2022189522A1 (en) * | 2021-03-09 | 2022-09-15 | Esmail Issa | Face mask for protection against viral or bacterial infections |
| CN115976735A (en) * | 2022-12-19 | 2023-04-18 | 南京理工大学 | Composite polylactic acid fiber membrane containing self-charged nano antibacterial agent, preparation method and application thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111514659A (en) * | 2020-05-04 | 2020-08-11 | 南通大学 | Nano cobweb antibacterial composite air filtering material and preparation method thereof |
| WO2022189522A1 (en) * | 2021-03-09 | 2022-09-15 | Esmail Issa | Face mask for protection against viral or bacterial infections |
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| CN114875497A (en) * | 2022-04-28 | 2022-08-09 | 内蒙古工业大学 | Metal nano self-assembly fiber material, and preparation method and application thereof |
| CN115976735A (en) * | 2022-12-19 | 2023-04-18 | 南京理工大学 | Composite polylactic acid fiber membrane containing self-charged nano antibacterial agent, preparation method and application thereof |
| CN115976735B (en) * | 2022-12-19 | 2023-12-08 | 南京理工大学 | Composite polylactic acid fiber membrane containing self-charged nano antibacterial agent, preparation method and application thereof |
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Application publication date: 20200428 |