CN113463278A - Nano/micron composite fiber membrane and preparation method thereof - Google Patents
Nano/micron composite fiber membrane 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
- D04H13/00—Other non-woven fabrics
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
- B32B5/022—Non-woven fabric
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/22—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
- B32B5/24—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
- B32B5/26—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it also being fibrous or filamentary
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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
- D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
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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
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
- B32B2262/02—Synthetic macromolecular fibres
- B32B2262/0223—Vinyl resin fibres
- B32B2262/0238—Vinyl halide, e.g. PVC, PVDC, PVF, PVDF
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
- B32B2262/02—Synthetic macromolecular fibres
- B32B2262/0253—Polyolefin fibres
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- Nonwoven Fabrics (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
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Abstract
The invention provides a nano/micron composite fiber membrane and a preparation method thereof, and the prepared composite fiber membrane has the surface density of 21-25g/m2. Compared with the traditional medical protective mask material which adopts 50g/m2The PP electret melt-blown fabric has the same filtering efficiency as the PP electret melt-blown fabric meets the protection requirement, simultaneously not only greatly reduces the consumption of raw materials and saves resources, but also lightens the ring caused by discarding the maskAmbient pressure.
Description
Technical Field
The invention relates to the technical field of aerosol, in particular to a nano/micron composite fiber membrane and a preparation method thereof.
Background
At present, the core filtering material of the protective mask adopts micron-sized electret melt-blown cloth, so that the problems of fast reduction of the filtering efficiency and short service life exist. The filtering action of the material on the particulate matter mainly comprises medium filtration and filter cake filtration. The media filtration effectively captures particulate matter using the fiber surface through sedimentation, interception, brownian motion, gravity settling, and electrostatic interaction. Among them, the electrostatic effect plays a major role in trapping viruses having a diameter of 100nm in aerosol with a diameter of 0.3 μm or less. However, the water vapor generated by respiration causes electrostatic attenuation of the fiber surface, resulting in a decrease in filtration efficiency. And (3) filtering by using a filter cake, taking the initially captured particles as a collection point, accumulating the particles to form a dendritic structure, gradually connecting adjacent dendrites together, forming a filter cake at the upstream end of the filter, and mechanically capturing the particles. During the accumulation of particulate matter, the electrostatic effect is reduced rapidly due to the shielding effect of particle deposition on fiber charges, and the filtering effect is gradually changed from depth filtering to surface filtering. The filtration resistance gradually increases along with the accumulation of filter cakes, and the breathing comfort degree is reduced.
The nano-fiber has the advantages of large specific surface area, high porosity, good air and moisture permeability and the like, meets the requirements of novel biological protection materials, and has great market potential in the fields of fiber membrane materials, filter media and the like.
In order to solve the problems that the filtering efficiency of the existing protective mask is reduced quickly, the service life is short, the filtering resistance is increased gradually along with the accumulation of filter cakes, and the breathing comfort is reduced, the nano/micron composite fiber membrane is developed, the specific surface area of fibers is realized, the interception and Brownian motion effects in the filtering process of a medium are improved, the accumulation of particles with the particles as collection points is reduced, the high-efficiency and low-resistance performance of a filtering material is realized, the virus propagation path is cut off, and the health of a human body is protected.
Disclosure of Invention
The invention aims to provide a nano/micron composite fiber membrane, which increases the specific surface area of fibers, improves the effects of interception and Brownian motion in the filtering process of a medium, and reduces the accumulation of particles by taking the particles as collection points, thereby realizing the high-efficiency and low-resistance performance of a filtering material.
In order to solve the technical problem, the invention provides a preparation method of a nano/micron composite fiber membrane, which comprises the following steps:
firstly, preparing an organic high molecular polymer solution;
in the second step, the nano-fiber is prepared,
the prepared nano/micron composite fiber membrane surface density is 21-25g/m2。
The first step is to weigh the organic polymer material, dry the organic polymer material at 80 ℃ for two hours, remove residual moisture, add the dried organic polymer into an organic solvent, stir the organic solvent with a glass rod for preliminary dispersion, stir the organic polymer in a thermostatic water bath at 80 ℃ for 4 hours by magnetic force, dissolve the polymer by swelling, disperse the polymer in the solvent uniformly, prepare a spinning solution with a certain concentration, place the spinning solution at normal temperature for 1 hour, cool the spinning solution to room temperature, and keep the spinning solution still for defoaming.
Wherein the second step further comprises:
step a, injecting the spinning solution prepared in the first step into a medical injector, placing the injector on a peristaltic pump, connecting the output end of the injector with a PTFE (polytetrafluoroethylene) tube through a luer connector, connecting the other end of the PTFE tube with a three-phase adapter, connecting the adapter to a needle plate through three PTFE short tubes respectively, and wrapping an aluminum foil on the surface of a roller by adopting a roller type grounding receiving device;
b, adjusting the distance between the spinning needle point and the roller, controlling the high-voltage direct-current output voltage, and controlling the flow rate of a single needle by constant-speed driving of a peristaltic pump;
step c, selecting a micron fiber film as electret meltblown base cloth, wrapping the micron fiber film on the surface of a roller, adjusting the moving speed of a horizontal sliding table for fixing the needle head in the step a, controlling the movement of the horizontal sliding table, setting the rotating speed of the roller, measuring and calculating the surface density of the nano fiber film on the surface of the electret meltblown base cloth of the micron fiber film actually collected, and preparing the nano/micron composite fiber film;
and d, placing the nano/micron composite fiber membrane obtained in the step C in a forced air drying oven, and drying.
Wherein, in the first step, the concentration of the spinning solution is 11-15%.
Wherein, in the step b, the distance between the spinning needle point and the roller is controlled within the range of 8-22 cm.
In the step b, the high-voltage direct current output voltage is controlled within the range of 20-29 kV.
Wherein, in the step b, the flow rate of the single needle is driven by a peristaltic pump at a constant speed and is controlled within the range of 0.5-2.5 ml/h.
Wherein in the step c, the area density of the nanofiber membrane is 1-5g/m2。
The invention also provides the nano/micron composite fiber membrane prepared by the method.
The invention also provides the application of the nano/micron composite fiber membrane as a core filter material of the medical protective mask.
The invention has the advantages of
The preparation method of the invention is adopted to prepare the nano-composite material with the surface density of 21-25g/m2The filtration efficiency of the nano/micro composite fiber membrane exceeds 95 percent, and is only 20g/m2Compared with 79.38 percent of filtering efficiency of the micron fiber film electret melt-blown fabric base cloth, the filtering efficiency is improved by more than 19.68 percent. Compared with the traditional medical protective mask material which adopts 50g/m2PP electret meltblown cloth (2 layers of filter material, 1 layer of 30 g/m)2Electret meltblown 1 layer of 20g/m2Electret meltblown fabric) using the nano/micro composite fiber membrane of the invention (2 layers of filter material, 1 layer of 20 g/m)2Electret meltblown 1 layer 2g/m2Nanofiber membrane), filtration efficiency also reaches the protection requirement, not only reduces the raw materials quantity by a wide margin simultaneously, resources are saved alleviates the environmental pressure that the gauze mask was abandoned and is brought simultaneously.
Drawings
FIG. 1 is a scanning electron microscope image of a nano/micro composite fiber film according to the present invention;
FIG. 2 is a diagram of a nano/micro composite fiber membrane of the present invention;
FIG. 3 shows the application of the nano/micro composite fiber membrane in the medical protective mask.
Detailed Description
The invention provides a preparation method of a nano/micron composite fiber membrane, which comprises the following steps:
firstly, preparing an organic high molecular polymer solution;
and secondly, preparing the nano fiber.
The first step is to weigh the organic polymer material, dry the organic polymer material at 80 ℃ for two hours, remove the residual moisture, add the dried organic polymer into the organic solvent, stir the organic solvent with a glass rod for preliminary dispersion, stir the organic polymer in a thermostatic water bath at 80 ℃ for 4 hours with magnetic stirring, dissolve the polymer by swelling, disperse the polymer in the solvent uniformly, prepare a spinning solution with a certain mass fraction, place the spinning solution at normal temperature for 1 hour, cool the spinning solution to room temperature, and keep stand for defoaming.
The second step further comprises:
step a, injecting the spinning solution prepared in the first step into a disposable medical injector with the capacity of 20ml for later use, placing the injector on a peristaltic pump of nano/micron composite fiber membrane preparation equipment, connecting the output end of the injector with a PTFE (polytetrafluoroethylene) tube through a luer connector, connecting the other end of the PTFE tube with a three-phase adapter, connecting the adapter to a needle plate of the nano/micron composite fiber membrane preparation equipment through three PTFE short tubes respectively, selecting a needle head with the length of 37mm, the needle length of 25mm, the inner diameter of 0.413mm and the outer diameter of 0.7mm, adopting a roller type grounding receiving device, and wrapping an aluminum foil on the surface of a roller;
b, adjusting the distance from the spinning needle point to the roller, so that the fibers can be collected on the receiving device, the loss is reduced, the fibers fly in an electric field for enough time, the solvent is fully volatilized, the fiber solidification is ensured, and the adhesion of the fibers caused by a large amount of solvent collected on the receiving device is avoided; controlling high-voltage direct-current output voltage to enable high-molecular polymer liquid drops to be subjected to electric field force to form a Taylor cone, and performing spiral drafting to obtain nano fibers; the peristaltic pump is driven at a constant speed, the flow speed of a single needle is controlled, so that liquid drops are prevented from overcoming the electric field force due to the fact that the flow speed is too high, the liquid drops directly drop under the action of gravity, and fibers cannot be prepared;
step c, selecting a micron fiber membrane as a receiving material, wrapping the micron fiber membrane on an aluminum foil on the surface of a roller, adjusting the moving speed of a horizontal sliding table for fixing the needle head in the step a, ensuring that the nano fibers are uniformly collected on the base cloth, adjusting the position of a limiter, realizing that the moving range of a needle plate corresponds to the receiving surface of the roller, controlling the moving range of the horizontal sliding table, ensuring that the left end and the right end of the base cloth are uniform in thickness, setting the rotating speed of the roller, improving the orientation degree of the nano fibers, removing the nano fibers with loss by dissipation, weighing at regular time, measuring and calculating the surface density of the nano fibers actually collected on the surface of the melt-blown base cloth, and preparing the nano/micron composite fiber membrane;
and d, placing the nano/micron composite fiber membrane obtained in the step C in a 40 ℃ blast drying oven, and treating for 6 hours to ensure that the solvent is completely volatilized, improve the strength of the composite membrane, and simultaneously avoid the damage and the damage of the material caused by the fact that the temperature is too high to reach the glass transition temperature of the nano/micron material.
The high molecular polymer in the first step can be one or a mixture of several polymers randomly used for electrostatic spinning, and comprises polyurethane, polyvinylidene fluoride, polyacrylonitrile, polyvinyl chloride, polyvinyl alcohol, polystyrene, polyvinylpyrrolidone, polystyrene, polymethyl methacrylate, polycaprolactone, polysulfone and the like.
In the first step, the organic solvent is one or more of tetrahydrofuran, N-N dimethylformamide, chloroform, acetone, formic acid, acetic acid and the like.
In the first step, the concentration of the spinning solution (the mass fraction of the organic high molecular polymer in the sum of the masses of the organic high molecular polymer and the organic solvent) is 11-15%.
In the step b, the distance between the spinning needle point and the roller is controlled within the range of 8-22 cm.
In the step b, the high-voltage direct current output voltage is controlled within the range of 20-29 kV.
In the step b, the flow rate of the single needle is driven by a peristaltic pump at a constant speed and is controlled within the range of 0.5-2.5 ml/h.
In the step c, the surface density of the selected micrometer fiber film electret melt-blown fabric base cloth is 20-30g/m2And (3) polypropylene melt-blown cloth.
In the step c, the area density of the nanofiber membrane is 1-5g/m2。
In the step c, the moving speed of the horizontal sliding table is 50-100 mm/s.
In the step c, the rotating speed of the roller is set to be 50-100 r/min.
The nano/micron composite fiber membrane provided by the invention is used as a core filter material of a medical protective mask.
By adopting the preparation method, the high molecular polymer solution formula is prepared by blending the components and the proportion, and the spinnability of the precursor is ensured; by adjusting process parameters such as high-voltage direct-current voltage, receiving distance from a needle head to a roller, injection speed, environment temperature and humidity and the like, polymer liquid drops can be successfully drafted into nano fibers under the action of a high-voltage electric field; the collection range is changed by adjusting the moving speed of the motor of the transverse group of the needle plate and controlling the position of the limiter, and the base cloth is reasonably selected, so that the good online composite forming of the nano fiber and the micron melt-blown base cloth is ensured.
The following embodiments are described in detail to solve the technical problems by applying technical means to the present invention, and the implementation process of achieving the technical effects can be fully understood and implemented.
Example 1:
dissolving 6g of polyvinylidene fluoride in 44g of N-N dimethylformamide solvent, magnetically stirring for 4h in a constant-temperature water bath at 80 ℃ until the powder is completely dissolved, standing for 1h at normal temperature, cooling and defoaming to obtain a spinning solution with the mass fraction of 12%. A22-gauge needle head (37 mm in length, 25mm in needle length, 0.413mm in inner diameter and 0.7mm in outer diameter) is selected, the moving speed of the sliding table is set to be 20mm/s, and the rotating speed of the roller is 50 r/min. Spinning voltage is adjusted to be 25kV, the receiving distance from the needle point to the roller is 16cm, the driving flow rate of a single needle head is 1.5ml/h, and the preparation is 3g/m2Nanofiber membranes, with 20g/m2And (3) carrying out online compounding on the polypropylene melt-blown base fabric. The fiber membrane is placed in a forced air drying oven at 40 ℃ and treated for 6 hours to obtain the fiber membrane with the surface density of 23g/m2The nano/micro composite fiber membrane of (1).
TABLE 1 polyvinylidene fluoride Performance parameters
| High molecular polymer | Melting Point C | DHf[J/g] | Molecular weight [ Mw, Da ]] | Mw/Mn |
| PVDF | 170-175 | 55-65 | 670000-700000 | 2.1-2.6 |
TABLE 2N-N dimethylformamide Performance parameters
| Organic solvent | Specification of | Melting Point C | Boiling point of | Molecular weight [ Mw, Da ]] | Density g/mL |
| DMF | AR，99.5％ | -61 | 153 | 73.09 | 0.948 |
Example 2:
dissolving 6g of polyvinylidene fluoride in 44g of N-N dimethylformamide solvent, magnetically stirring for 4h in a constant-temperature water bath at 80 ℃ until the powder is completely dissolved, standing for 1h at normal temperature, cooling and defoaming to obtain a spinning solution with the mass fraction of 12%. Selecting a needle head with the number of 22, setting the moving speed of the sliding table to be 20mm/s, and setting the rotating speed of the roller to be 50 r/min. Spinning voltage is adjusted to be 28kV, the receiving distance from the needle point to the roller is 16cm, the driving flow rate of a single needle head is 1.5ml/h, and the preparation is 3g/m2Nanofiber membranes, with 20g/m2And (3) carrying out online compounding on the polypropylene melt-blown base fabric. The fiber membrane is placed in a forced air drying oven at 40 ℃ and treated for 6 hours to obtain the fiber membrane with the surface density of 23g/m2The nano/micro composite fiber membrane of (1).
Example 3:
dissolving 6g of polyvinylidene fluoride in 44g of N-N dimethylformamide solvent, magnetically stirring for 4h in a constant-temperature water bath at 80 ℃ until the powder is completely dissolved, standing for 1h at normal temperature, cooling and defoaming to obtain a spinning solution with the mass fraction of 12%. A22-gauge needle head (37 mm in length, 25mm in needle length, 0.413mm in inner diameter and 0.7mm in outer diameter) is selected, the moving speed of the sliding table is set to be 20mm/s, and the rotating speed of the roller is 50 r/min. Adjusting spinning voltage to 27kV, receiving distance from needle point to roller to 13cm, single needle driving flow rate to 1.5ml/h, preparing to 3g/m2Nanofiber membranes, with 20g/m2And (3) carrying out online compounding on the polypropylene melt-blown base fabric. The fiber membrane is placed in a forced air drying oven at 40 ℃ and treated for 6 hours to obtain the fiber membrane with the surface density of 23g/m2The nano/micro composite fiber membrane of (1).
Example 4:
dissolving 6g of polyvinylidene fluoride in 44g of N-N dimethylformamide solvent, magnetically stirring for 4h in a constant-temperature water bath at 80 ℃ until the powder is completely dissolved, standing for 1h at normal temperature, cooling and defoaming to obtain a spinning solution with the mass fraction of 12%. Selecting a needle head with the number of 22, setting the moving speed of the sliding table to be 20mm/s, and setting the rotating speed of the roller to be 50 r/min. The spinning voltage was adjusted to 27kV, the receiving distance from the needle tip to the drum was 19cm, the single needle driving flow rate was 1.5ml/h, and a preparation of 3g/m2Nanofiber membranes, with 20g/m2The polypropylene melt-blown base fabric isAnd (6) compounding the wires. The fiber membrane is placed in a forced air drying oven at 40 ℃ and treated for 6 hours to obtain the fiber membrane with the surface density of 23g/m2The nano/micro composite fiber membrane of (1).
Example 5:
dissolving 6g of polyvinylidene fluoride in 44g of N-N dimethylformamide solvent, magnetically stirring for 4h in a constant-temperature water bath at 80 ℃ until the powder is completely dissolved, standing for 1h at normal temperature, cooling and defoaming to obtain a spinning solution with the mass fraction of 12%. Selecting a needle head with the number of 22, setting the moving speed of the sliding table to be 20mm/s, and setting the rotating speed of the roller to be 50 r/min. Adjusting spinning voltage to 27kV, receiving distance from needle point to roller to 16cm, single needle driving flow rate to 0.5ml/h, preparing to 3g/m2Nanofiber membranes, with 20g/m2And (3) carrying out online compounding on the polypropylene melt-blown base fabric. The fiber membrane is placed in a forced air drying oven at 40 ℃ and treated for 6 hours to obtain the fiber membrane with the surface density of 23g/m2The nano/micro composite fiber membrane of (1).
Example 6:
dissolving 6g of polyvinylidene fluoride in 44g of N-N dimethylformamide solvent, magnetically stirring for 4h in a constant-temperature water bath at 80 ℃ until the powder is completely dissolved, standing for 1h at normal temperature, cooling and defoaming to obtain a spinning solution with the mass fraction of 12%. Selecting a needle head with the number of 22, setting the moving speed of the sliding table to be 20mm/s, and setting the rotating speed of the roller to be 50 r/min. The spinning voltage was adjusted to 27kV, the receiving distance from the needle tip to the drum was 16cm, the single needle driving flow rate was 2.5ml/h, and a preparation of 3g/m2Nanofiber membranes, with 20g/m2And (3) carrying out online compounding on the polypropylene melt-blown base fabric. The fiber membrane is placed in a forced air drying oven at 40 ℃ and treated for 6 hours to obtain the fiber membrane with the surface density of 23g/m2The nano/micro composite fiber membrane of (1).
Example 7:
dissolving 5.5g of polyvinylidene fluoride in 44.5g of N-N dimethylformamide solvent, magnetically stirring for 4 hours in a constant-temperature water bath at 80 ℃ until the powder is completely dissolved, standing for 1 hour at normal temperature, cooling and defoaming to prepare a spinning solution with the mass fraction of 11%. Selecting a needle head with the number of 22, setting the moving speed of the sliding table to be 20mm/s, and setting the rotating speed of the roller to be 50 r/min. The spinning voltage was adjusted to 27kV, the receiving distance from the needle tip to the drum was 16cm, the single needle driving flow rate was 1.5ml/h, and a preparation of 3g/m2Nanofiber membranes, with 20g/m2PolypropyleneAnd (4) melt-blown base fabric online compounding. The fiber membrane is placed in a forced air drying oven at 40 ℃ and treated for 6 hours to obtain the fiber membrane with the surface density of 23g/m2The nano/micro composite fiber membrane of (1).
Example 8:
dissolving 7.5g of polyvinylidene fluoride in 42.5g of N-N dimethylformamide solvent, magnetically stirring for 4 hours in a constant-temperature water bath at 80 ℃ until the powder is completely dissolved, standing for 1 hour at normal temperature, cooling and defoaming to prepare a spinning solution with the mass fraction of 15%. Selecting a needle head with the number of 22, setting the moving speed of the sliding table to be 20mm/s, and setting the rotating speed of the roller to be 50 r/min. The spinning voltage was adjusted to 27kV, the receiving distance from the needle tip to the drum was 16cm, the single needle driving flow rate was 1.5ml/h, and a preparation of 3g/m2Nanofiber membranes, with 20g/m2And (3) carrying out online compounding on the polypropylene melt-blown base fabric. The fiber membrane is placed in a forced air drying oven at 40 ℃ and treated for 6 hours to obtain the fiber membrane with the surface density of 23g/m2The nano/micro composite fiber membrane of (1).
Example 9:
dissolving 6g of polyvinylidene fluoride in 44g of N-N dimethylformamide solvent, magnetically stirring for 4h in a constant-temperature water bath at 80 ℃ until the powder is completely dissolved, standing for 1h at normal temperature, cooling and defoaming to obtain a spinning solution with the mass fraction of 12%. Selecting a needle head with the number of 22, setting the moving speed of the sliding table to be 20mm/s, and setting the rotating speed of the roller to be 50 r/min. Adjusting spinning voltage to 27kV, receiving distance from needle point to roller to 16cm, single needle driving flow rate to 1.5ml/h, preparing to 1g/m2Nanofiber membranes, with 20g/m2And (3) carrying out online compounding on the polypropylene melt-blown base fabric. The fiber membrane is placed in a forced air drying oven at 40 ℃ and treated for 6 hours to obtain the fiber membrane with the surface density of 21g/m2The nano/micro composite fiber membrane of (1).
Example 10:
dissolving 6g of polyvinylidene fluoride in 44g of N-N dimethylformamide solvent, magnetically stirring for 4h in a constant-temperature water bath at 80 ℃ until the powder is completely dissolved, standing for 1h at normal temperature, cooling and defoaming to obtain a spinning solution with the mass fraction of 12%. Selecting a needle head with the number of 22, setting the moving speed of the sliding table to be 20mm/s, and setting the rotating speed of the roller to be 50 r/min. The spinning voltage was adjusted to 27kV, the needle tip to drum acceptance distance was 16em, the single needle drive flow rate was 1.5ml/h, and a preparation of 5g/m2Nanofiber membranes, with 20g/m2And (3) carrying out online compounding on the polypropylene melt-blown base fabric. The fiber membrane is placed in a forced air drying oven at 40 ℃ and treated for 6 hours to obtain the fiber membrane with the surface density of 25g/m2The nano/micro composite fiber membrane of (1).
Comparative example 1:
dissolving 4g of polyvinylidene fluoride in 46g of N-N dimethylformamide solvent, magnetically stirring for 4h in a constant-temperature water bath at 80 ℃ until the powder is completely dissolved, standing for 1h at normal temperature, cooling and defoaming to obtain a spinning solution with the mass fraction of 8%. Selecting a needle head with the number of 22, setting the moving speed of the sliding table to be 20mm/s, and setting the rotating speed of the roller to be 50 r/min. The spinning voltage was adjusted to 27kV, the receiving distance from the needle tip to the drum was 16cm, the single needle driving flow rate was 1.5ml/h, and a preparation of 3g/m2Nanofiber membranes, with 20g/m2And (3) carrying out online compounding on the polypropylene melt-blown base fabric. The fiber membrane is placed in a forced air drying oven at 40 ℃ and treated for 6 hours to obtain the fiber membrane with the surface density of 23g/m2The nano/micro composite fiber membrane of (1).
Comparative example 2:
dissolving 10g of polyvinylidene fluoride in 40g of N-N dimethylformamide solvent, magnetically stirring for 4h in a constant-temperature water bath at 80 ℃ until the powder is completely dissolved, standing for 1h at normal temperature, cooling and defoaming to obtain a spinning solution with the mass fraction of 20%. Selecting a needle head with the number of 22, setting the moving speed of the sliding table to be 20mm/s, and setting the rotating speed of the roller to be 50 r/min. The spinning voltage was adjusted to 27kV, the needle tip to drum acceptance distance was 16em, the single needle drive flow rate was 1.5ml/h, and a preparation of 3g/m2Nanofiber membranes, with 20g/m2And (3) carrying out online compounding on the polypropylene melt-blown base fabric. The fiber membrane is placed in a forced air drying oven at 40 ℃ and treated for 6 hours to obtain the fiber membrane with the surface density of 23g/m2The nano/micro composite fiber membrane of (1).
The performance parameters of the examples are shown in table 3.
TABLE 3
In examples 1 to 10, the lower the filtration resistance, the better the breathing comfort, on the basis of the filtration efficiency of 95%. The quality factor is a dimensionless coefficient for comprehensively evaluating the filtration efficiency and the filtration resistance, and the higher the quality factor is, the better the comprehensive filtration performance of the fiber membrane is. The quality factor of example 9 is at most 0.0416, and the air permeability is as high as 381.22 mm/s.
In comparative example 1, the concentration of the spinning solution was too low, and the nanofiber membrane obtained had a beaded structure, and the thickness of the fibers was not uniform, which was not favorable for reducing the filtration resistance. In comparative example 2, since the concentration of the spinning solution was too high and the viscosity of the polymer solution was too high, the solution was difficult to flow and block the needle, and thus a nanofiber membrane could not be obtained.
All of the above mentioned intellectual property rights are not intended to be restrictive to other forms of implementing the new and/or new products. Those skilled in the art will take advantage of this important information, and the foregoing will be modified to achieve similar performance. However, all modifications or alterations are based on the new products of the invention and belong to the reserved rights.
The foregoing is directed to preferred embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.
Claims (10)
1. A method for preparing a nano/micron composite fiber membrane is characterized by comprising the following steps:
firstly, preparing an organic high molecular polymer solution;
in the second step, the nano-fiber is prepared,
the prepared nano/micron composite fiber membrane surface density is 21-25g/m2。
2. The method for preparing a nano/micro composite fiber membrane according to claim 1, wherein: the first step is to weigh the organic polymer material, dry the organic polymer material at 80 ℃ for two hours, remove the residual moisture, add the dried organic polymer into the organic solvent, stir the organic solvent with a glass rod for preliminary dispersion, stir the organic polymer in a thermostatic water bath at 80 ℃ for 4 hours with magnetic stirring, dissolve the polymer by swelling, disperse the polymer in the solvent uniformly, prepare a spinning solution with a certain mass fraction, place the spinning solution at normal temperature for 1 hour, cool the spinning solution to room temperature, and keep stand for defoaming.
3. The method for preparing a nano/micro composite fiber membrane according to claim 1 or 2, wherein: the second step further comprises:
step a, injecting the spinning solution prepared in the first step into a medical injector, placing the injector on a peristaltic pump, connecting the output end of the injector with a PTFE (polytetrafluoroethylene) tube through a luer connector, connecting the other end of the PTFE tube with a three-phase adapter, connecting the adapter to a needle plate through three PTFE short tubes respectively, and wrapping an aluminum foil on the surface of a roller by adopting a roller type grounding receiving device;
b, adjusting the distance between the spinning needle point and the roller, controlling the high-voltage direct-current output voltage, and controlling the flow rate of a single needle by constant-speed driving of a peristaltic pump;
step c, selecting a micron fiber membrane as a receiving material, wrapping the micron fiber membrane on the surface of a roller, adjusting the moving speed of a horizontal sliding table for fixing the needle head in the step a, controlling the moving stroke of the horizontal sliding table, setting the rotating speed of the roller, measuring and calculating the surface density of the nano fiber membrane on the surface of the melt-blown base cloth actually collected, and preparing the nano/micron composite fiber membrane;
and d, placing the nano/micron composite fiber membrane obtained in the step C in a forced air drying oven, and drying.
4. The method for preparing a nano/micro composite fiber membrane according to claim 1 or 2, wherein: in the first step, the mass fraction of the organic high molecular polymer is 11-15%.
5. The method for preparing a nano/micro composite fiber membrane according to claim 1 or 2, wherein: in the step b, the distance between the spinning needle point and the roller is controlled within the range of 8-22 cm.
6. The method for preparing a nano/micro composite fiber membrane according to claim 1 or 2, wherein: in the step b, the high-voltage direct current output voltage is controlled within the range of 20-29 kV.
7. The method for preparing a nano/micro composite fiber membrane according to claim 1 or 2, wherein: in the step b, the flow rate of the single needle is driven by a peristaltic pump at a constant speed and is controlled within the range of 0.5-2.5 ml/h.
8. The method for preparing a nano/micro composite fiber membrane according to claim 1 or 2, wherein: in the step c, the area density of the nanofiber membrane is 1-5g/m2。
9. A nano/micro composite fiber membrane prepared by the method of any one of claims 1 to 8.
10. The nano/micro composite fiber membrane according to claim 9, which is used as a core filter material of a medical protective mask.
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