CN112626710A - Filtering fiber membrane with antibacterial property and preparation method thereof - Google Patents
Filtering fiber membrane with antibacterial property and preparation method thereof Download PDFInfo
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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
- D04H1/40—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
- D04H1/4282—Addition polymers
- D04H1/4291—Olefin series
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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
- B01D46/54—Particle separators, e.g. dust precipitators, using ultra-fine filter sheets or diaphragms
- B01D46/543—Particle separators, e.g. dust precipitators, using ultra-fine filter sheets or diaphragms using membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/021—Carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/76—Macromolecular material not specifically provided for in a single one of groups B01D71/08 - B01D71/74
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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
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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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/46—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/39—Electrospinning
Abstract
The invention belongs to the technical field of electrostatic spinning, and discloses a filter fiber membrane with antibacterial performance and a preparation method thereof, wherein the preparation method comprises the following steps: mixing deionized water and isopropanol, and adding ethylene-vinyl alcohol copolymer to obtain ethylene-vinyl alcohol copolymer solution; adding silver nitrate particles into the ethylene-vinyl alcohol copolymer solution to obtain an ethylene-vinyl alcohol and silver nitrate blending solution; and preparing the ethylene-vinyl alcohol and silver nitrate blended liquid into a filtering fiber membrane by an electrostatic spinning method. Based on the advantages that the silver nitrate particles have high catalytic activity, high adsorption capacity, adjustable membrane density, high antibacterial performance and the like, the silver nitrate particles are selected as the antibacterial agent, silver nitrate is reduced into silver nanoparticles under a certain temperature condition through oxidation-reduction reaction, and meanwhile, the silver nitrate particles are generally deposited on carriers as load materials, so that the silver nitrate particles can be well adsorbed on the filter fiber membrane, and the antibacterial capacity of the filter fiber membrane is effectively improved.
Description
Technical Field
The invention belongs to the technical field of electrostatic spinning, and relates to a filtering fiber membrane with antibacterial performance and a preparation method thereof.
Background
Currently, with the rapid rise of industrial technology, the variety of pollutants emitted to the atmosphere by industry is large, with those fine particle pollutants (i.e., PM2.5) having particle diameters of less than 2.5 μm and being airborne being the most common. These pollutants seriously affect the health of human body, such as cancer, respiratory diseases and chronic lung diseases, so that the blocking of the pollutants by the filter material is one of the effective methods for protecting the health of human body.
However, the currently used filter material can only have a certain filtering capacity for micron-sized particles, and generally has no antibacterial effect, so that various bacteria easily penetrate through the filter material to harm the health of human bodies.
Disclosure of Invention
The invention aims to overcome the defect that the existing filter materials in the prior art generally do not have antibacterial effect, and provides a filter fiber membrane with antibacterial performance and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
in one aspect of the invention, a preparation method of a filter fiber membrane with antibacterial performance comprises the following steps:
mixing deionized water and isopropanol, and adding ethylene-vinyl alcohol copolymer to obtain ethylene-vinyl alcohol copolymer solution; adding silver nitrate particles into the ethylene-vinyl alcohol copolymer solution to obtain an ethylene-vinyl alcohol and silver nitrate blending solution; and preparing the ethylene-vinyl alcohol and silver nitrate blended liquid into a filtering fiber membrane by an electrostatic spinning method.
The preparation method of the filter fiber membrane with antibacterial performance of the invention is further improved in that:
before the ethylene-vinyl alcohol and silver nitrate blended liquid is prepared into a filter fiber membrane by an electrostatic spinning method, activated carbon is added into the ethylene-vinyl alcohol and silver nitrate blended liquid.
The specific method for adding the activated carbon into the ethylene-vinyl alcohol and silver nitrate blended solution comprises the following steps:
adding active carbon into the ethylene-vinyl alcohol and silver nitrate blended liquid according to the proportion of adding 0.15-0.85 g of active carbon into 10ml of the ethylene-vinyl alcohol and silver nitrate blended liquid.
When the ethylene-vinyl alcohol and silver nitrate blended liquid is prepared into the filter fiber membrane through the electrostatic spinning method, the spinning positive voltage of the electrostatic spinning method is 15-20 KV, the spinning negative voltage is 0.85-1.55 KV, the solution extrusion speed is 0.15-0.25 mL/min, the receiving distance is 8-15 cm, the temperature is 35-45 ℃, and the humidity is 20-30 ℃.
The specific method for obtaining the ethylene-vinyl alcohol copolymer solution by mixing the deionized water and the isopropanol and then adding the ethylene-vinyl alcohol copolymer comprises the following steps:
deionized water and isopropanol were mixed as follows 2: 8 to obtain a solution A, adding 0.75-1.25 g of ethylene-vinyl alcohol copolymer into each 10ml of the solution A according to the proportion, and stirring the solution A under heating in a water bath to obtain the ethylene-vinyl alcohol copolymer solution.
The specific method for obtaining the ethylene-vinyl alcohol copolymer solution by mixing the deionized water and the isopropanol and then adding the ethylene-vinyl alcohol copolymer comprises the following steps:
deionized water and isopropanol were mixed as 3: 7 to obtain a solution A, adding 0.75-1.25 g of ethylene-vinyl alcohol copolymer into each 10ml of the solution A according to the proportion, and stirring the solution A under heating in a water bath to obtain the ethylene-vinyl alcohol copolymer solution.
The temperature of the water bath heating is 72-75 ℃.
The specific method for obtaining the ethylene-vinyl alcohol and silver nitrate blended liquid by adding silver nitrate particles into the ethylene-vinyl alcohol copolymer solution comprises the following steps:
adding silver nitrate particles into the ethylene-vinyl alcohol copolymer solution according to the proportion of adding 0.2-0.8 g of silver nitrate into every 10ml of the ethylene-vinyl alcohol copolymer solution, and stirring until the solution becomes yellow brown to obtain the ethylene-vinyl alcohol and silver nitrate blended solution.
When the ethylene-vinyl alcohol and silver nitrate blended liquid is prepared into the filter fiber membrane through the electrostatic spinning method, the spinning positive voltage of the electrostatic spinning method is 15-20 KV, the spinning negative voltage is 0.85-1.75 KV, the solution extrusion speed is 0.2-0.3 mL/min, the receiving distance is 17-20 cm, the temperature is 35-45 ℃, and the humidity is 20-30 ℃.
In a second aspect of the present invention, a filtration fiber membrane with antibacterial properties is prepared by the above preparation method of a filtration fiber membrane with antibacterial properties.
Compared with the prior art, the invention has the following beneficial effects:
according to the preparation method of the filtering fiber membrane with the antibacterial property, silver nitrate particles are selected as the antibacterial agent based on the advantages that the silver nitrate particles have high catalytic activity, high adsorption capacity, adjustable membrane density, high antibacterial property and the like, silver nitrate is reduced to silver nanoparticles under a certain temperature condition through oxidation-reduction reaction, and meanwhile, the silver nitrate particles are generally deposited on carriers as loading materials, so that the silver nitrate particles can be well adsorbed on the filtering fiber membrane, and the antibacterial property of the filtering fiber membrane is effectively improved.
Furthermore, based on the better adsorption and filtration effects of the activated carbon, the Activated Carbon Fiber (ACF) prepared by the activated carbon has the characteristics of large specific surface area, large adsorption capacity, good adsorption and the like, and further, the activated carbon is added into the ethylene-vinyl alcohol and silver nitrate blending liquid to deposit silver nitrate on the surface of the activated carbon, so that on one hand, the large pores in the activated carbon provide good carriers for the silver nitrate and help silver particles to play a role in sterilization; on the other hand, the good antibacterial property of the silver nitrate particles improves the antibacterial capability of the activated carbon. By combining the silver nanoparticles with the activated carbon, the filtering and antibacterial capabilities of the filtering fiber membrane are effectively improved, and the filtering material has great application value in the aspects of filtering and resisting bacteria of pollutants.
Drawings
FIG. 1 is a scanning electron microscope image of a calibration 1-C element of the present invention;
FIG. 2 is a scanning electron microscope image of a nominal 2-C element of the present invention.
Detailed Description
In order to make the technical solutions of the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in sequences other than those illustrated or described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
The invention is described in further detail below with reference to the accompanying drawings:
the embodiment of the invention provides a preparation method of a filtering fiber membrane with antibacterial performance, wherein the used solvent is mainly isopropanol, and the solute is ethylene-vinyl alcohol copolymer (EVOH), silver nitrate particles and powdered activated carbon. The electrostatic spinning method gives wide attention in various fields due to the advantages of simple and convenient preparation mode, various spinning substances, controllable process and the like. The electrostatic spinning method can be used for preparing the fiber with the diameter ranging from micron to nanometer, and the nanofiber has the characteristics of small volume, large specific surface area, economy, environmental protection and the like. At present, the method is widely applied to various fields such as biomedicine, filtration, food and the like. The invention realizes the preparation of the filter fiber membrane based on an electrostatic spinning method according to the prepared solution.
Specifically, the preparation method of the antibacterial filter fiber membrane comprises the following steps: mixing deionized water and isopropanol, and adding ethylene-vinyl alcohol copolymer to obtain ethylene-vinyl alcohol copolymer solution; adding silver nitrate particles into the ethylene-vinyl alcohol copolymer solution to obtain an ethylene-vinyl alcohol and silver nitrate blending solution; and preparing the ethylene-vinyl alcohol and silver nitrate blended liquid into a filtering fiber membrane by an electrostatic spinning method.
Preferably, the specific method for obtaining the ethylene-vinyl alcohol copolymer solution by mixing deionized water and isopropanol and then adding the ethylene-vinyl alcohol copolymer comprises the following steps: deionized water and isopropanol were mixed as follows 2: 8 to obtain a solution A, adding 0.75-1.25 g of ethylene-vinyl alcohol copolymer into each 10ml of the solution A according to the proportion, and stirring the solution A under heating in a water bath to obtain the ethylene-vinyl alcohol copolymer solution. Wherein the temperature of the water bath heating is 72-75 ℃.
Preferably, the specific method for obtaining the ethylene-vinyl alcohol copolymer solution by mixing deionized water and isopropanol and then adding the ethylene-vinyl alcohol copolymer comprises the following steps: deionized water and isopropanol were mixed as 3: 7 to obtain a solution A, adding 0.75-1.25 g of ethylene-vinyl alcohol copolymer into each 10ml of the solution A according to the proportion, and stirring the solution A under heating in a water bath to obtain the ethylene-vinyl alcohol copolymer solution. Wherein the temperature of the water bath heating is 72-75 ℃.
Preferably, the specific method for obtaining the ethylene-vinyl alcohol and silver nitrate blended liquid by adding silver nitrate particles into the ethylene-vinyl alcohol copolymer solution comprises the following steps: adding silver nitrate particles into the ethylene-vinyl alcohol copolymer solution according to the proportion of adding 0.2-0.8 g of silver nitrate into every 10ml of the ethylene-vinyl alcohol copolymer solution, and stirring until the solution becomes yellow brown to obtain the ethylene-vinyl alcohol and silver nitrate blended solution.
Preferably, when the ethylene-vinyl alcohol and silver nitrate blended liquid is prepared into the filter fiber membrane by an electrostatic spinning method, the spinning positive voltage of the electrostatic spinning method is 15-20 KV, the spinning negative voltage is 0.85-1.75 KV, the solution extrusion speed is 0.2-0.3 mL/min, the receiving distance is 17-20 cm, the temperature is 35-45 ℃, and the humidity is 20-30 ℃.
According to the preparation method of the filtering fiber membrane with the antibacterial property, silver nitrate particles are selected as the antibacterial agent based on the advantages that the silver nitrate particles have high catalytic activity, high adsorption capacity, adjustable membrane density, high antibacterial property and the like, silver nitrate is reduced to silver nanoparticles under a certain temperature condition through oxidation-reduction reaction, and meanwhile, the silver nitrate particles are generally deposited on carriers as loading materials, so that the silver nitrate particles can be well adsorbed on the filtering fiber membrane, and the antibacterial property of the filtering fiber membrane is effectively improved.
Preferably, the inventors consider that the specific surface area of micropores in the activated carbon accounts for 95% or more of the specific surface area of the activated carbon, and largely determine the increase in the adsorption capacity of the activated carbon. Therefore, before the ethylene-vinyl alcohol and silver nitrate blended liquid is prepared into the filter fiber membrane by the electrostatic spinning method, activated carbon is added into the ethylene-vinyl alcohol and silver nitrate blended liquid. The active carbon used in the invention can be coconut shell powder active carbon which has stronger adsorption and filtration effects.
According to the preparation method of the filtering fiber membrane with antibacterial property, based on the good adsorption and filtration effects of the activated carbon, the Activated Carbon Fiber (ACF) prepared by the activated carbon has the characteristics of large specific surface area, large adsorption capacity, good adsorption and the like, and further, the silver nitrate is deposited on the surface of the activated carbon by adding the activated carbon into the ethylene-vinyl alcohol and silver nitrate blending liquid, so that on one hand, large pores in the activated carbon provide good carriers for the silver nitrate and help silver particles to play a role in sterilization; on the other hand, the good antibacterial property of the silver nitrate particles improves the antibacterial capability of the activated carbon. By combining the silver nanoparticles with the activated carbon, the filtering and antibacterial capabilities of the filtering fiber membrane are effectively improved, and the filtering material has great application value in the aspects of filtering and resisting bacteria of pollutants.
Preferably, the specific method for adding the activated carbon into the ethylene-vinyl alcohol and silver nitrate blended solution comprises the following steps: adding active carbon into the ethylene-vinyl alcohol and silver nitrate blended liquid according to the proportion of adding 0.15-0.85 g of active carbon into 10ml of the ethylene-vinyl alcohol and silver nitrate blended liquid.
Preferably, when the ethylene-vinyl alcohol and silver nitrate blended solution is prepared into the filter fiber membrane by an electrostatic spinning method, the spinning positive voltage of the electrostatic spinning method is 15-20 KV, the spinning negative voltage is 0.85-1.55 KV, the solution extrusion speed is 0.15-0.25 mL/min, the receiving distance is 8-15 cm, the temperature is 35-45 ℃, and the humidity is 20-30 ℃.
The following examples illustrate the preparation of the antibacterial filter fiber membrane.
Example 1
A preparation method of a filter fiber membrane with antibacterial performance comprises the following steps:
step 1: mixing 20ml of deionized water with 80ml of isopropanol to obtain a solution A; then 7.5g of ethylene-vinyl alcohol copolymer particles are added, the molecular weight of the ethylene-vinyl alcohol copolymer is 20 ten thousand, thereby ensuring that the material has better mechanical strength and is completely dissolved in the solvent. Heating in 72 deg.C water bath on magnetic stirrer, stirring for 110min until the solution is completely dissolved, and preparing ethylene-vinyl alcohol copolymer solution.
Step 2: and (3) adding 5g of silver nitrate particles on the basis of the step 1, stirring for about 60min, and obtaining the preparation of the ethylene-vinyl alcohol and silver nitrate blended liquid with the silver content of 0.05g/mL when the solution turns to tawny so as to show that the silver nitrate particles are completely dissolved.
And step 3: then preparing the nano fiber membrane containing the silver nano particles as a filter fiber membrane under the spinning conditions that the spinning positive voltage is 20KV, the spinning negative voltage is 0.85KV, the solution extrusion speed is 0.3mL/min, the receiving distance is 18cm, the temperature is 45 ℃ and the humidity is 20 ℃.
Example 2
A preparation method of a filter fiber membrane with antibacterial performance comprises the following steps:
step 1: mixing 20ml of deionized water with 80ml of isopropanol to obtain a solution A; then 10g of ethylene-vinyl alcohol copolymer particles are added, the molecular weight of the ethylene-vinyl alcohol copolymer is 120 ten thousand, so that the material is ensured to have better mechanical strength, and the material is completely dissolved in the solvent. Heating in 74 deg.C water bath on magnetic stirrer, stirring for about 115min until the solution is completely dissolved, and preparing ethylene-vinyl alcohol copolymer solution.
Step 2: and (2) adding 7g of silver nitrate particles on the basis of the step 1, stirring for about 50min, and when the solution turns to tawny, indicating that the silver nitrate particles are completely dissolved, so as to obtain silver-containing concentrations of 0.07g/mL respectively, thereby completing the preparation of the ethylene-vinyl alcohol and silver nitrate blending solution.
And step 3: then preparing the nano fiber membrane containing the silver nano particles as a filter fiber membrane under the spinning conditions that the spinning positive voltage is 15KV, the spinning negative voltage is 1.75KV, the solution extrusion speed is 0.2mL/min, the receiving distance is 20cm, the temperature is 40 ℃, and the humidity is 25 ℃.
Example 3
A preparation method of a filter fiber membrane with antibacterial performance comprises the following steps:
step 1: mixing 20ml of deionized water with 80ml of isopropanol to obtain a solution A; 12.5g of ethylene-vinyl alcohol copolymer particles are added, and the molecular weight of the ethylene-vinyl alcohol copolymer is 200 ten thousand, so that the material is ensured to have better mechanical strength and is completely dissolved in a solvent. Heating in 75 deg.C water bath on magnetic stirrer, stirring for about 120min until the solution is completely dissolved, and preparing ethylene-vinyl alcohol copolymer solution.
Step 2: and (3) adding 8g of silver nitrate particles on the basis of the step 1, stirring for about 53min, and obtaining the preparation of the ethylene-vinyl alcohol and silver nitrate blended liquid with the silver content of 0.08g/mL when the solution turns to tawny so as to show that the silver nitrate particles are completely dissolved.
And step 3: then preparing the nano fiber membrane containing the silver nano particles as a filtering fiber membrane under the spinning conditions that the spinning positive voltage is 18KV, the spinning negative voltage is 1KV, the solution extrusion speed is 0.25mL/min, the receiving distance is 17cm, the temperature is 35 ℃ and the humidity is 30 ℃.
Example 4
A preparation method of a filter fiber membrane with antibacterial performance comprises the following steps:
step 1: mixing 30ml of deionized water with 70ml of isopropanol to obtain a solution A; then 7.5g of ethylene-vinyl alcohol copolymer particles are added, the molecular weight of the ethylene-vinyl alcohol copolymer is 20 ten thousand, thereby ensuring that the material has better mechanical strength and is completely dissolved in the solvent. Heating in 72 deg.C water bath on magnetic stirrer, stirring for 110min until the solution is completely dissolved, and preparing ethylene-vinyl alcohol copolymer solution.
Step 2: and (3) adding 5g of silver nitrate particles on the basis of the step 1, stirring for about 60min, and obtaining the preparation of the ethylene-vinyl alcohol and silver nitrate blended liquid with the silver content of 0.05g/mL when the solution turns to tawny so as to show that the silver nitrate particles are completely dissolved.
And step 3: and (3) on the basis of the step 2, adding 3g of powdered activated carbon into the ethylene-vinyl alcohol and silver nitrate blended solution, stirring for about 5min without heating in a water bath, and obtaining the activated carbon-containing blended solution with the concentration of 0.3g/mL after the activated carbon powder is uniformly dissolved in the ethylene-vinyl alcohol and silver nitrate blended solution.
And 4, step 4: the nanofiber composite membrane containing the activated carbon and the silver nanoparticles is prepared under the spinning conditions that the spinning positive voltage is 15KV, the spinning negative voltage is 1.55KV, the solution extrusion speed is 0.25mL/min, the receiving distance is 8cm, the temperature is 35 ℃, and the humidity is 20 ℃ to serve as a filter fiber membrane.
Example 5
A preparation method of a filter fiber membrane with antibacterial performance comprises the following steps:
step 1: mixing 30ml of deionized water with 70ml of isopropanol to obtain a solution A; then 10g of ethylene-vinyl alcohol copolymer particles are added, the molecular weight of the ethylene-vinyl alcohol copolymer is 20 ten thousand, so that the material is ensured to have better mechanical strength, and the material is completely dissolved in the solvent. Heating in 74 deg.C water bath on magnetic stirrer, stirring for about 115min until the solution is completely dissolved, and preparing ethylene-vinyl alcohol copolymer solution.
Step 2: and (3) adding 7g of silver nitrate particles on the basis of the step 1, stirring for about 50min, and obtaining the preparation of the ethylene-vinyl alcohol and silver nitrate blended liquid with the silver content of 0.07g/mL when the solution turns to yellow brown to show that the silver nitrate particles are completely dissolved.
And step 3: on the basis of the step 2, 4g of powdered activated carbon is added into the ethylene-vinyl alcohol and silver nitrate blending solution, water bath heating is not needed, stirring is carried out for about 5min, and when the activated carbon powder is uniformly dissolved in the ethylene-vinyl alcohol and silver nitrate blending solution, the blending solution containing the activated carbon with the concentration of 0.4g/mL is obtained.
And 4, step 4: the nanofiber composite membrane containing the activated carbon and the silver nanoparticles is prepared under the spinning conditions that the spinning positive voltage is 13KV, the spinning negative voltage is 1.25KV, the solution extrusion speed is 0.20mL/min, the receiving distance is 12cm, the temperature is 40 ℃, and the humidity is 25 ℃ to serve as a filter fiber membrane.
Example 6
A preparation method of a filter fiber membrane with antibacterial performance comprises the following steps:
step 1: mixing 30ml of deionized water with 70ml of isopropanol to obtain a solution A; 12.5g of ethylene-vinyl alcohol copolymer particles are added, and the molecular weight of the ethylene-vinyl alcohol copolymer is 20 ten thousand, so that the material is ensured to have better mechanical strength and is completely dissolved in a solvent. Heating in 75 deg.C water bath on magnetic stirrer, stirring for about 120min until the solution is completely dissolved, and preparing ethylene-vinyl alcohol copolymer solution.
Step 2: and (3) adding 8g of silver nitrate particles on the basis of the step 1, stirring for about 53min, and obtaining the preparation of the ethylene-vinyl alcohol and silver nitrate blended liquid with the silver content of 0.08g/mL when the solution turns to tawny so as to show that the silver nitrate particles are completely dissolved.
And step 3: and (3) on the basis of the step 2, adding 5g of powdered activated carbon into the ethylene-vinyl alcohol and silver nitrate blended solution, stirring for about 5min without heating in a water bath, and obtaining the activated carbon-containing blended solution with the concentration of 0.5g/mL after the activated carbon powder is uniformly dissolved in the ethylene-vinyl alcohol and silver nitrate blended solution.
And 4, step 4: the nanofiber composite membrane containing the activated carbon and the silver nanoparticles is prepared under the spinning conditions that the spinning positive voltage is 10KV, the spinning negative voltage is 0.85KV, the solution extrusion speed is 0.15mL/min, the receiving distance is 15cm, the temperature is 45 ℃ and the humidity is 30 ℃ and serves as a filter fiber membrane.
The above examples 1 to X were repeated to obtain a sufficient number of filtration fiber membranes, which were subjected to a drying treatment. The common filter membrane without silver nano-particles is used as a control group 1, and the common filter membrane without activated carbon is used as a control group 2.
The antibacterial test was performed on the filtration fiber membranes prepared in the control group 1 and examples 1 to 3 of the present invention, each group of the fiber membranes was cut into disks having a diameter of 6mm, the two disks were placed on an agar plate of cultured staphylococcus aureus, and after incubation for a certain period of time, the diameters of the inhibition rings at 5, 10, 15 and 20 hours were measured, respectively. The formation of antibacterial rings was observed at the fiber membrane discs containing silver nanoparticles, and no antibacterial rings were formed around the fiber membrane discs containing no silver. The antibacterial effect of the silver nanoparticles on staphylococcus aureus was confirmed by the antibacterial effect of the size of the antibacterial ring of about 4mm in the petri dish containing the silver nanoparticles, and the formed antibacterial ring increased with the increase of the concentration of the silver nanoparticles from the initial 2mm to 6 mm.
The adsorption test was performed on the control group 2 and the filtration fiber membranes prepared in examples 4 to 6 of the present invention, each group of the fiber membranes was weighed to have a mass of 56mg, added to a lead ion solution having an initial concentration of 60mg/L and a volume of 30mL, adjusted to have a PH of 3, subjected to shaking adsorption for 4.5 hours, filtered, and tested for the concentration of heavy metal ions on an inductively coupled plasma emission spectrometer. The result shows that the adsorption rate of the filter fiber membrane prepared by the embodiment of the invention to lead ions is 32.6% higher than that of the common fiber membrane. The result proves that the filter fiber membrane prepared by the embodiment of the invention has good adsorption performance on heavy metal ions, and provides potential application value for the filter material.
Referring to fig. 1 and 2, it can be seen from the scanning electron microscope images of the filtration fiber membranes prepared by the method for preparing filtration fiber membranes having antibacterial properties according to the present invention that particulate matter is attached to almost every fiber surface, and from the energy dispersive X-ray spectrogram thereof, referring to table 1, the elemental measurement results table, the constituent elements of the particles embedded in the fiber surface contain C, O, Ag elements. The labeled portion in fig. 1 and 2 was detected as activated carbon, indicating that the fibrous membrane activated carbon was mostly uniformly distributed on the surface of the nanofiber membrane, and partially distributed in a blocky structure.
Table 1 table of measurement results of elements
| Element(s) | By weight percent | Atom weight% | Error% |
| C K | 52.94 | 70.39 | 9.07 |
| O K | 12.28 | 12.26 | 10.3 |
| AgL | 1.56 | 0.23 | 7.37 |
| PtL | 4.99 | 0.41 | 9.7 |
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (10)
1. A preparation method of a filter fiber membrane with antibacterial performance is characterized by comprising the following steps:
mixing deionized water and isopropanol, and adding ethylene-vinyl alcohol copolymer to obtain ethylene-vinyl alcohol copolymer solution; adding silver nitrate particles into the ethylene-vinyl alcohol copolymer solution to obtain an ethylene-vinyl alcohol and silver nitrate blending solution; and preparing the ethylene-vinyl alcohol and silver nitrate blended liquid into a filtering fiber membrane by an electrostatic spinning method.
2. The method for preparing a filtering fiber membrane with antibacterial property according to claim 1, wherein before the blending solution of ethylene-vinyl alcohol and silver nitrate is prepared into the filtering fiber membrane by the electrostatic spinning method, activated carbon is added into the blending solution of ethylene-vinyl alcohol and silver nitrate.
3. The preparation method of the antibacterial filter fiber membrane as claimed in claim 2, wherein the specific method for adding the activated carbon into the ethylene-vinyl alcohol and silver nitrate blended solution comprises the following steps:
adding active carbon into the ethylene-vinyl alcohol and silver nitrate blended liquid according to the proportion of adding 0.15-0.85 g of active carbon into 10ml of the ethylene-vinyl alcohol and silver nitrate blended liquid.
4. The method for preparing a filtration fiber membrane having antibacterial properties according to claim 2, wherein when the ethylene-vinyl alcohol/silver nitrate blend solution is prepared into a filtration fiber membrane by an electrospinning method, the electrospinning method has a spinning positive voltage of 15 to 20KV, a spinning negative voltage of 0.85 to 1.55KV, a solution extrusion speed of 0.15 to 0.25mL/min, a receiving distance of 8 to 15cm, a temperature of 35 to 45 ℃, and a humidity of 20 to 30 ℃.
5. The method for preparing the antibacterial filtering fiber membrane of claim 1, wherein the specific method for mixing deionized water and isopropanol and then adding ethylene-vinyl alcohol copolymer to obtain the ethylene-vinyl alcohol copolymer solution comprises the following steps:
deionized water and isopropanol were mixed as follows 2: 8 to obtain a solution A, adding 0.75-1.25 g of ethylene-vinyl alcohol copolymer into each 10ml of the solution A according to the proportion, and stirring the solution A under heating in a water bath to obtain the ethylene-vinyl alcohol copolymer solution.
6. The method for preparing the antibacterial filtering fiber membrane of claim 1, wherein the specific method for mixing deionized water and isopropanol and then adding ethylene-vinyl alcohol copolymer to obtain the ethylene-vinyl alcohol copolymer solution comprises the following steps:
deionized water and isopropanol were mixed as 3: 7 to obtain a solution A, adding 0.75-1.25 g of ethylene-vinyl alcohol copolymer into each 10ml of the solution A according to the proportion, and stirring the solution A under heating in a water bath to obtain the ethylene-vinyl alcohol copolymer solution.
7. The preparation method of the antibacterial filter fiber membrane as claimed in claim 5 or 6, wherein the water bath heating temperature is 72-75 ℃.
8. The method for preparing a filtering fiber membrane with antibacterial performance according to claim 1, wherein the specific method for adding silver nitrate particles into the ethylene-vinyl alcohol copolymer solution to obtain the ethylene-vinyl alcohol and silver nitrate blended solution comprises the following steps:
adding silver nitrate particles into the ethylene-vinyl alcohol copolymer solution according to the proportion of adding 0.2-0.8 g of silver nitrate into every 10ml of the ethylene-vinyl alcohol copolymer solution, and stirring until the solution becomes yellow brown to obtain the ethylene-vinyl alcohol and silver nitrate blended solution.
9. The method for preparing a filtration fiber membrane having antibacterial properties according to claim 1, wherein when the ethylene-vinyl alcohol/silver nitrate blend solution is prepared into a filtration fiber membrane by an electrospinning method, the electrospinning method has a spinning positive voltage of 15 to 20KV, a spinning negative voltage of 0.85 to 1.75KV, a solution extrusion speed of 0.2 to 0.3mL/min, a receiving distance of 17 to 20cm, a temperature of 35 to 45 ℃, and a humidity of 20 to 30 ℃.
10. A filtration fiber membrane having antibacterial properties produced by the method for producing a filtration fiber membrane having antibacterial properties according to any one of claims 1 to 9.
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Cited By (1)
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| CN113634134A (en) * | 2021-08-13 | 2021-11-12 | 江苏威久科技发展有限公司 | Carbon fiber composite filtering membrane for sewage treatment and preparation method thereof |
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