CN111188128B - Preparation method of breathable film with micro-support - Google Patents
Preparation method of breathable film with micro-support Download PDFInfo
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- CN111188128B CN111188128B CN202010010230.1A CN202010010230A CN111188128B CN 111188128 B CN111188128 B CN 111188128B CN 202010010230 A CN202010010230 A CN 202010010230A CN 111188128 B CN111188128 B CN 111188128B
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- polyvinylpyrrolidone
- electrostatic spinning
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- breathable film
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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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- 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
- D01F6/02—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F6/26—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from other polymers
Abstract
The invention discloses a preparation method of a breathable film with micro-support, which comprises the following steps of: 8-9, adding a proper amount of polyvinylpyrrolidone, and dissolving uniformly to obtain a polyvinylpyrrolidone solution; setting parameters of an electrostatic spinning instrument, and adding a polyvinylpyrrolidone solution into the electrostatic spinning instrument for electrostatic spinning treatment to obtain polyvinylpyrrolidone electrostatic spinning fibers; weighing a proper amount of polyvinylpyrrolidone electrostatic spinning fibers, and placing the polyvinylpyrrolidone electrostatic spinning fibers in a vacuum freeze dryer for cooling treatment; and starting a vacuum pump of the vacuum freeze dryer, gradually increasing the pressure and the temperature, and sequentially drying and cooling the polyvinylpyrrolidone electrostatic spinning fibers to obtain the breathable film with the micro-support. The invention relates to a preparation method of a breathable film with micro-support, which solves the problem of poor breathability of a covering film in the prior art.
Description
Technical Field
The invention relates to the technical field of chemical manufacturing films, in particular to a preparation method of a breathable film with micro-support.
Background
The covering film has micropores, can play roles of covering, blocking and ventilating, and is widely applied to the fields of wound dressings, filter media, packaging materials and the like. The existing covering film has a symmetrical structure with smooth two sides, and in practical application, the ventilation quantity is reduced when the covering film is attached to a smooth surface; although the increase in the number of micropores can achieve the purpose of improving the ventilation amount, the excessively high number of micropores per unit area lowers the mechanical strength of the cover film.
Disclosure of Invention
The invention aims to provide a preparation method of a breathable film with micro-support, which solves the problem of poor breathability of a covering film in the prior art.
The technical scheme adopted by the invention is a preparation method of a breathable film with micro-support, which is implemented according to the following steps:
N, N-dimethylformamide and water are mixed according to a volume ratio of 1-2: 8-9, adding a proper amount of polyvinylpyrrolidone, and uniformly dissolving to obtain a polyvinylpyrrolidone solution for later use;
and 4, starting a vacuum pump of the vacuum freeze dryer, gradually increasing the pressure and the temperature, drying the polyvinylpyrrolidone electrostatic spinning fibers, and cooling the polyvinylpyrrolidone electrostatic spinning fibers to obtain the breathable film with the micro support.
The invention is also characterized in that:
in the step 1, N, N-dimethylformamide is replaced by dimethyl sulfoxide, and the volume ratio of the dimethyl sulfoxide to water is 1-2: 8-9, and uniformly mixing.
In the step 1, the mass concentration of the polyvinylpyrrolidone solution is 25-35%.
In the step 2, parameters of the electrostatic spinning instrument are voltage of 15-25 KV, spinning speed of 0.01-0.1 ml/h, and receiving distance of 5-15 cm.
In the step 3, the mass of the polyvinylpyrrolidone electrostatic spinning fiber is 0.5-1.0 g.
In the step 3, the temperature of the cooling treatment is-30-0 ℃.
In the step 4, the pressure of the vacuum freeze dryer is 10-30 Pa, and the temperature is 50-60 ℃.
In the step 4, the temperature of the cooling treatment is controlled to be 20-25 ℃.
The invention has the beneficial effects that:
according to the preparation method of the breathable film with the micro-support, the asymmetric phase-inversion organic film made of uniform materials is prepared by adopting an electrostatic spinning method, so that the porosity of the film is effectively improved, and the problem of film blockage caused by a bridging phenomenon is effectively avoided; the breathable film prepared by the invention has a porous surface layer and a fiber layer forming micro support, so that the number of micropores of the microporous film is effectively reduced, and the gas exchange efficiency of the covered interface is improved; the breathable film with the micro-support, prepared by the invention, can effectively improve the interface gas exchange capacity and can be widely applied to the oxidation healing and flavor packaging of wound covering.
Drawings
FIG. 1 is a schematic structural view of a breathable film with micro-supports according to the present invention;
FIG. 2 is a scanning electron micrograph of a porous skin layer of a breathable film having micro-supports according to the present invention;
FIG. 3 is a scanning electron micrograph of a micro-supporting fibrous layer of an air permeable film having micro-supports of the present invention;
FIG. 4 is a schematic diagram of an application of a breathable film with micro-supports according to the present invention;
fig. 5 is a schematic diagram of an application of a conventional microporous membrane.
In the figure, 1 is a micro-supporting fiber layer, 2 is a micropore, 3 is a covering, and 4 is an air flow exchange.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention provides a preparation method of a breathable film with micro-support, which is implemented according to the following steps:
N, N-dimethylformamide and water are mixed according to a volume ratio of 1-2: 8-9, uniformly mixing the mixture to serve as a solvent, and then adding a proper amount of polyvinylpyrrolidone to uniformly dissolve the polyvinylpyrrolidone to obtain a polyvinylpyrrolidone solution with the mass concentration of 25-35% for later use;
wherein N, N-dimethylformamide is replaced by dimethyl sulfoxide, and the volume ratio of the dimethyl sulfoxide to water is 1-2: 8-9;
wherein the parameters of the electrostatic spinning instrument are voltage of 15-25 KV, spinning speed of 0.01-0.1 ml/h and receiving distance of 5-15 cm;
wherein the mass of the polyvinylpyrrolidone electrostatic spinning fiber is 0.5-1.0 g; the temperature of the cooling treatment is-30 to 0 ℃;
and 4, starting a vacuum pump of the vacuum freeze dryer, gradually increasing the pressure and the temperature, drying the polyvinylpyrrolidone electrospun fibers, and cooling the polyvinylpyrrolidone electrospun fibers to obtain the breathable film with the micro support, wherein the structure of the breathable film with the micro support is an asymmetric microporous film, one side of the breathable film is provided with a micro support fiber layer 1, and the body of the breathable film is provided with a plurality of micropores 2, so that the gas transmittance of the breathable film is effectively improved.
Wherein the pressure of the vacuum freeze dryer is 10-30 Pa, and the temperature is 50-60 ℃; the temperature of the cooling treatment is controlled to be 20-25 ℃.
The preparation method of the breathable film with the micro-support adopts the following principle:
1. the electrostatic spinning method is a common method for preparing the three-dimensional nano-structure film, the prepared film has the advantages of small aperture, high porosity, good fiber uniformity and the like, the membrane blockage caused by the problems of bridging phenomenon and the like is effectively avoided, and the method has huge application potential in the field of fluid filtration.
2. The asymmetric phase inversion membrane is one of asymmetric membranes, the epidermal layer and the supporting layer are made of the same material, and an asymmetric structure is formed through a phase inversion process; generally, the asymmetric phase inversion membrane is prepared by scraping a prepared polymer solution on a polished support, evaporating, and immersing in a precipitating agent for gelation; the obtained asymmetric phase inversion membrane has asymmetric structure skin and porous structure support.
3. The invention adopts the electrostatic spinning method to prepare the asymmetric phase inversion organic film of uniform material, and effectively combines the advantages of the electrostatic spinning method and the asymmetric phase inversion film. In the principle of gas exchange, the gas exchange capacity of the covering film and the interface of the covered object depends on the interface combination degree, the interface combination degree is small, the interface space is too large, and the covering object loses the isolated covering significance; the interface combination degree is large, the interface space is small, and effective gas exchange cannot be carried out. The surface of the breathable film prepared by the invention forms fibers capable of playing a supporting role, so that the coverage is not influenced, the interface space is effectively increased, and the gas exchange efficiency is improved.
Example 1
A method for preparing a breathable film with micro-supports comprises the following steps:
(1) preparation of a polyvinylpyrrolidone solution
Mixing N, N-dimethylformamide and water in a volume ratio of 1: 9, uniformly mixing the mixture to be used as a solvent, and then adding a proper amount of polyvinylpyrrolidone to uniformly dissolve the polyvinylpyrrolidone to obtain a polyvinylpyrrolidone solution with the mass concentration of 25% for later use;
(2) setting parameters of an electrostatic spinning instrument, and adding a polyvinylpyrrolidone solution into the electrostatic spinning instrument for electrostatic spinning treatment to obtain polyvinylpyrrolidone electrostatic spinning fibers for later use;
wherein the parameters of the electrostatic spinning instrument are voltage 15KV, spinning speed 0.01ml/h and receiving distance 5 cm;
(3) weighing 0.5g of polyvinylpyrrolidone electrostatic spinning fibers, and placing the polyvinylpyrrolidone electrostatic spinning fibers in a vacuum freeze dryer to reduce the temperature to-30 ℃;
(4) and starting a vacuum pump of the vacuum freeze dryer, gradually increasing the pressure and the temperature, drying the polyvinylpyrrolidone electrostatic spinning fiber, and cooling the polyvinylpyrrolidone electrostatic spinning fiber to 20 ℃ to obtain the breathable film with the micro support.
Wherein the pressure of the vacuum freeze dryer is 10Pa, and the temperature is 50 ℃.
Example 2
A method for preparing a breathable film with micro-supports comprises the following steps:
(1) preparation of a polyvinylpyrrolidone solution
Mixing N, N-dimethylformamide and water in a volume ratio of 2: 8, uniformly mixing the mixture to be used as a solvent, and then adding a proper amount of polyvinylpyrrolidone to uniformly dissolve the polyvinylpyrrolidone to obtain a polyvinylpyrrolidone solution with the mass concentration of 35% for later use;
(2) setting parameters of an electrostatic spinning instrument, and adding a polyvinylpyrrolidone solution into the electrostatic spinning instrument for electrostatic spinning treatment to obtain polyvinylpyrrolidone electrostatic spinning fibers for later use;
wherein the parameters of the electrostatic spinning instrument are voltage 25KV, spinning speed 0.1ml/h, and receiving distance 15 cm;
(3) weighing 1.0g of polyvinylpyrrolidone electrostatic spinning fibers, and placing the polyvinylpyrrolidone electrostatic spinning fibers in a vacuum freeze dryer to reduce the temperature to 0 ℃;
(4) and starting a vacuum pump of the vacuum freeze dryer, gradually increasing the pressure and the temperature, drying the polyvinylpyrrolidone electrostatic spinning fiber, and cooling the polyvinylpyrrolidone electrostatic spinning fiber to 25 ℃ to obtain the breathable film with the micro support.
Wherein the pressure of the vacuum freeze dryer is 30Pa, and the temperature is 60 ℃.
Example 3
A method for preparing a breathable film with micro-supports comprises the following steps:
(1) preparation of a polyvinylpyrrolidone solution
Mixing N, N-dimethylformamide and water in a volume ratio of 1.5: 8.5, uniformly mixing the components to serve as a solvent, and then adding a proper amount of polyvinylpyrrolidone to uniformly dissolve the polyvinylpyrrolidone to obtain a polyvinylpyrrolidone solution with the mass concentration of 30% for later use;
(2) setting parameters of an electrostatic spinning instrument, and adding a polyvinylpyrrolidone solution into the electrostatic spinning instrument for electrostatic spinning treatment to obtain polyvinylpyrrolidone electrostatic spinning fibers for later use;
wherein the parameters of the electrostatic spinning instrument are 20KV voltage, 0.05ml/h spinning speed and 10cm receiving distance;
(3) weighing 0.7g of polyvinylpyrrolidone electrostatic spinning fibers, and placing the polyvinylpyrrolidone electrostatic spinning fibers in a vacuum freeze dryer to reduce the temperature to-20 ℃;
(4) and starting a vacuum pump of the vacuum freeze dryer, gradually increasing the pressure and the temperature, drying the polyvinylpyrrolidone electrostatic spinning fiber, and cooling the polyvinylpyrrolidone electrostatic spinning fiber to 23 ℃ to obtain the breathable film with the micro support.
Wherein the pressure of the vacuum freeze dryer is 20Pa, and the temperature is 55 ℃.
Example 4
A method for preparing a breathable film with micro-supports comprises the following steps:
(1) preparation of a polyvinylpyrrolidone solution
Mixing dimethyl sulfoxide and water in a volume ratio of 1: 9, uniformly mixing the mixture to be used as a solvent, and then adding a proper amount of polyvinylpyrrolidone to uniformly dissolve the polyvinylpyrrolidone to obtain a polyvinylpyrrolidone solution with the mass concentration of 25% for later use;
(2) setting parameters of an electrostatic spinning instrument, and adding a polyvinylpyrrolidone solution into the electrostatic spinning instrument for electrostatic spinning treatment to obtain polyvinylpyrrolidone electrostatic spinning fibers for later use;
wherein the parameters of the electrostatic spinning instrument are voltage 15KV, spinning speed 0.01ml/h and receiving distance 5 cm;
(3) weighing 0.5g of polyvinylpyrrolidone electrostatic spinning fibers, and placing the polyvinylpyrrolidone electrostatic spinning fibers in a vacuum freeze dryer to reduce the temperature to-30 ℃;
(4) and starting a vacuum pump of the vacuum freeze dryer, gradually increasing the pressure and the temperature, drying the polyvinylpyrrolidone electrostatic spinning fiber, and cooling the polyvinylpyrrolidone electrostatic spinning fiber to 20 ℃ to obtain the breathable film with the micro support.
Wherein the pressure of the vacuum freeze dryer is 10Pa, and the temperature is 50 ℃.
Example 5
A method for preparing a breathable film with micro-supports comprises the following steps:
(1) preparation of a polyvinylpyrrolidone solution
Mixing dimethyl sulfoxide and water in a volume ratio of 2: 8, uniformly mixing the mixture to be used as a solvent, and then adding a proper amount of polyvinylpyrrolidone to uniformly dissolve the polyvinylpyrrolidone to obtain a polyvinylpyrrolidone solution with the mass concentration of 35% for later use;
(2) setting parameters of an electrostatic spinning instrument, and adding a polyvinylpyrrolidone solution into the electrostatic spinning instrument for electrostatic spinning treatment to obtain polyvinylpyrrolidone electrostatic spinning fibers for later use;
wherein the parameters of the electrostatic spinning instrument are voltage 25KV, spinning speed 0.1ml/h, and receiving distance 15 cm;
(3) weighing 1.0g of polyvinylpyrrolidone electrostatic spinning fibers, and placing the polyvinylpyrrolidone electrostatic spinning fibers in a vacuum freeze dryer to reduce the temperature to 0 ℃;
(4) and starting a vacuum pump of the vacuum freeze dryer, gradually increasing the pressure and the temperature, drying the polyvinylpyrrolidone electrostatic spinning fiber, and cooling the polyvinylpyrrolidone electrostatic spinning fiber to 25 ℃ to obtain the breathable film with the micro support.
Wherein the pressure of the vacuum freeze dryer is 30Pa, and the temperature is 60 ℃.
Example 6
A method for preparing a breathable film with micro-supports comprises the following steps:
(1) preparation of a polyvinylpyrrolidone solution
Mixing dimethyl sulfoxide and water in a volume ratio of 1.5: 8.5, uniformly mixing the components to serve as a solvent, and then adding a proper amount of polyvinylpyrrolidone to uniformly dissolve the polyvinylpyrrolidone to obtain a polyvinylpyrrolidone solution with the mass concentration of 30% for later use;
(2) setting parameters of an electrostatic spinning instrument, and adding a polyvinylpyrrolidone solution into the electrostatic spinning instrument for electrostatic spinning treatment to obtain polyvinylpyrrolidone electrostatic spinning fibers for later use;
wherein the parameters of the electrostatic spinning instrument are 20KV voltage, 0.05ml/h spinning speed and 10cm receiving distance;
(3) weighing 0.7g of polyvinylpyrrolidone electrostatic spinning fibers, and placing the polyvinylpyrrolidone electrostatic spinning fibers in a vacuum freeze dryer to reduce the temperature to-20 ℃;
(4) and starting a vacuum pump of the vacuum freeze dryer, gradually increasing the pressure and the temperature, drying the polyvinylpyrrolidone electrostatic spinning fiber, and cooling the polyvinylpyrrolidone electrostatic spinning fiber to 23 ℃ to obtain the breathable film with the micro support.
Wherein the pressure of the vacuum freeze dryer is 20Pa, and the temperature is 55 ℃.
And (3) experimental verification:
the average pore size, pore occupied membrane surface area, and gas permeability of a commercially available 0.45 μm cellulose acetate microporous membrane were compared with those of the breathable films prepared according to the present invention, as shown in table 1:
TABLE 1 comparison of the Performance of microporous cellulose acetate membranes to breathable films with micro-support
| Average pore diameter | The channels occupy the membrane surface area | Gas permeability | |
| Microporous cellulose acetate film | 0.45μm | 55-80％ | 60-80％ |
| Breathable film with micro-support | 0.45μm | 3-7％ | 90-100％ |
As can be seen from table 1, a breathable film with micro-support according to the present invention has an average pore size consistent with that of a cellulose acetate microporous membrane; on the premise that the occupied membrane surface area of the pore channels of the breathable film with the micro support is much smaller than that of the microporous cellulose acetate membrane, the gas permeability of the breathable film with the micro support is higher than that of the microporous cellulose acetate membrane. Thus, it is demonstrated that the breathable film with micro-support prepared by the present invention has better gas transmission rate than microporous film.
FIG. 2 is a scanning electron microscope image of a porous skin layer of a breathable film with micro-supports of the present invention, and it can be seen from FIG. 2 that the breathable film with micro-supports of the present invention has uniform pore diameter, flat and smooth surface, and average pore diameter of 0.45 μm, and the micro-supported fiber layer 1 on the other side of the breathable film can be observed from the micropores 2, which illustrates that the breathable film with micro-supports prepared by the present invention has good gas permeability.
FIG. 3 is a scanning electron microscope image of a micro-supporting fiber layer of a micro-supporting air-permeable film according to the present invention, and it can be seen from FIG. 3 that the micro-supporting fiber layer 1 of a micro-supporting air-permeable film according to the present invention has uniform fiber diameter and length of 0.2-0.5. mu.m.
Fig. 4 is a schematic diagram of an application of a breathable film with micro-support according to the present invention, and fig. 5 is a schematic diagram of an application of a conventional microporous film. As can be seen from the comparison between fig. 4 and fig. 5, after the air-permeable film with micro-support of the present invention covers the covering 3, the micro-support of the micro-support fiber layer 1 extends the gas exchange space to the whole interface between the air-permeable film and the covering 3, so as to enhance the gas flow exchange 4, enlarge the gas exchange space, and effectively increase the gas transmittance. The existing microporous membrane has less gas flow exchange 4 and small gas exchange space, and is only limited around micropores.
Claims (4)
1. A preparation method of a breathable film with micro-support is characterized by comprising the following steps:
step 1, preparing polyvinylpyrrolidone solution
N, N-dimethylformamide and water are mixed according to a volume ratio of 1-2: 8-9, adding a proper amount of polyvinylpyrrolidone, and uniformly dissolving to obtain a polyvinylpyrrolidone solution for later use;
step 2, setting parameters of an electrostatic spinning instrument, and adding the polyvinylpyrrolidone solution into the electrostatic spinning instrument for electrostatic spinning treatment to obtain polyvinylpyrrolidone electrostatic spinning fibers for later use;
step 3, weighing a proper amount of the polyvinylpyrrolidone electrostatic spinning fibers, and placing the polyvinylpyrrolidone electrostatic spinning fibers in a vacuum freeze dryer for cooling treatment; the mass of the polyvinylpyrrolidone electrostatic spinning fiber is 0.5-1.0 g, and the temperature of the cooling treatment is-30-0 ℃;
step 4, starting a vacuum pump of the vacuum freeze dryer, gradually increasing the pressure and temperature, drying the polyvinylpyrrolidone electrospun fibers, and cooling the polyvinylpyrrolidone electrospun fibers to obtain the breathable film with the micro support; the pressure of the vacuum freeze dryer is 10-30 Pa, and the temperature is 50-60 ℃; and the temperature of the cooling treatment is controlled to be 20-25 ℃.
2. The method for preparing the breathable film with the micro-support according to claim 1, wherein in the step 1, the N, N-dimethylformamide is replaced by dimethyl sulfoxide, and the volume ratio of the dimethyl sulfoxide to water is 1-2: 8-9, and uniformly mixing.
3. The method for preparing the breathable film with the micro-support according to claim 1 or 2, wherein in the step 1, the mass concentration of the polyvinylpyrrolidone solution is 25-35%.
4. The method for preparing the breathable film with the micro-support according to claim 1, wherein in the step 2, the electrostatic spinning apparatus has parameters of voltage of 15-25 KV, spinning speed of 0.01-0.1 ml/h, and receiving distance of 5-15 cm.
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