Method and apparatus for producing fine fibres

FIELD: chemistry.

SUBSTANCE: method and apparatus for producing fine fibres via fibre electrospinning by applying an electric field between a primary electrode and a counter electrode lying at a distance from the primary electrode and often parallel thereto. The working surface of the primary electrode is coated with a polymer solution. An electric field is created between the primary electrode and the counter electrode having sufficient strength to cause formation of fine fibres in the space between the electrodes. The working surface of the primary electrode coated with a polymer solution consists of corresponding parts of surfaces of a plurality of elements that are semi-submerged in the working state and are freely lying (not connected to anything), said elements resting at the bottom of a bath or tray or some other supporting structure(s). A tool is used, which enables to apply the polymer solution on the surface of the freely lying elements protruding from the solution via rotation thereof in the polymer solution, such that their surface is coated with a thin layer of the polymer solution.

EFFECT: method and apparatus according to the present invention enable to perform spinning with high efficiency while eliminating problems encountered in the previous technological level.

12 cl, 8 dwg

 

The technical field

This invention relates to a method and apparatus for producing fine fibers, in particular but not exclusively, very thin fibers belonging to the class, which is often referred to as nanofibers from various polymers, mixtures of polymers, mixtures of ceramic precursors and mixtures of metal precursors.

The level of technology

Obtained from solutions of the polymers of very thin fibers, which are often referred to as nanofibers suitable in a wide range of applications, including filtration media, frame structures and devices for tissue engineering, reinforced nanofiber composite materials, sensors, electrodes for batteries and fuel cells, materials carriers of catalysts, absorbent fabric, absorbent pads, agents, adhesion (bandages) after the operation, the electoral textiles, as well as in artificial cashmere and faux leather.

Electrostatic spinning of fibers was probably first described in U.S. patent 692631. In principle, a small drop of a solution or melt of the polymer is placed in a strong electric field, which causes repulsion between induced in drops charges of the same sign, which counteracts the surface tension of the liquid. If you make a strong enough electrical wiring in the practical field (typically 0.5 to 4 kV/cm), electrostatic forces can overcome the surface tension of the liquid, and droplets ejecting a jet of solution or melt of the polymer.

Electrostatic instability leads to a rapid, chaotic oscillation of the jet, which leads, in turn to fast evaporation of any solvent, and also to stretching and thinning of the remaining polymer fibers. The resulting fibers are then collected on the counter-electrode, usually in the form of nonwoven fabric. The collected fibers are usually fairly homogeneous and can have a diameter of fibres from several microns down to such low values as 5 nm.

Technical obstacles in the manufacture of large quantities of nanofibers using electroprecizia include low productivity and the fact that the spinning of most polymers is carried out on the solution.

In one of the conventional production methods use a multitude of channels, which, for example, can be made in the form of multi-needle nozzles. On average, electroprecizia from the solution using a multi-needle nozzles has a capacity solution of about 1 ml per hour per channel. Fibers with diameters of 50-100 nm is usually spun from solutions with relatively low concentrations, usually 5-10% of the mass, depending on the type of polymer and molecular weight. It is about the means, that is, assuming that the density of the polymer is about 1 g/ml, typical performance process electroprecizia based on multi-needle nozzles on solid matter ranges from 0.05 to 0.1 g of fiber per hour on one needle channel. At this speed the manufacture of cloth of nanofibres with surface weight 80 g/m2at a speed of 5 m2/s will require at least 14400000 needle channels.

In addition, the overlap of the electric fields between the different needle channels limits the minimum distance between them and, moreover, continuous multi-needle nozzles require frequent cleaning needle channels, because there is a tendency of driving multi-channel nozzles polymer. The General result is that the production on an industrial scale becomes almost prohibitively expensive for most applications in consumer products, such as fabrics for filtration and absorbent fabric.

Formhals (U.S. patent 1975504) tried to increase the performance electroprecizia by applying as one of the electrodes gears. In later designs he used the installation with multi-needle nozzles (U.S. patent 2109333).

Reneker et al. (publication of International patent application WO 0022207) describe a process in which oterom nanofibres produced by filing solution for the formation of fibers in the column with circular cross-section and flow through this column of gas under pressure to form a ring-shaped film, which is then divided into numerous strands of fibre-forming material.

Nominated numerous other suggestions that are based on creating jets of fibre-forming solution using a needle channels and holes for receiving the fibers thus.

System with very high performance, known as the NanoSpider described in the published international patent application WO 05024101. In this system, the polymer solution for forming fibers is in a ditch (tub), and in the bath slowly rotates partially submerged in it conductive cylinder, to form on its surface a thin layer of solution. Above the cylinder 10-20 cm posted a counter-electrode, and in the process electroprecizia hundreds of jets flying from the surface of the cylinder and into the counter-electrode.

Publication of International patent application WO 2006131081 describes an improved type of NanoSpider technology, in which the electrically conductive cylinders replaced mounted on the same axis as the rotating cylindrical structures that provide a lot of "bit" of surfaces, from which the solution must flow with the formation of polymer fibers. This device is rather complicated and has a cylindrical structure, obviously, are very expensive.

Japanese patent JP 3918179 describes the pic is b, where on the surface of the polymer solution continuously generate bubbles by blowing into the solution of the compressed air through a porous membrane or through a thin tube. These bubbles are formed jet to electroprecizia, and the resulting fibers are collected on the counter-electrode. How is the author of this application, this system requires that the bubbles in the polymer solution formed in large quantities and so they quickly burst. In addition, most organic solvents are not enough to easily form the foam, and these examples demonstrate spinning only with solutions of polymers in water, 2-propanol and acetone. Moreover, this patent requires that the counter-electrode was placed at a sufficient distance from foam, as drops of spinning solution, which arise because of the constantly bursting bubbles can sprinkle the fibers formed on the counter-electrode, and damage or destroy them.

In our pending International patent application published under number WO 2008125971, the authors describe the improvement of the bubble process electroprecizia based on the stabilization of the formed bubbles using surface-active substances.

The objective of the invention

The objective of the invention is a method and apparatus for obtaining such fibers, is the quiet resolve, at least to some extent, one or more of the above-mentioned problems related to obtaining high-performance electrostatically spinning fibers.

The invention

In accordance with one aspect of the present invention, a method for obtaining fine fibers by electroprecizia fibers, by applying an electric field between the primary electrode and counter-electrode located at some distance from the primary electrode and generally parallel to it, in which at least the working surface of the primary electrode is covered with the polymer solution, and between the primary electrode and counter-electrode to create an electric field of sufficient magnitude to cause the formation of fine fibers in the space between the electrodes, the method characterized by the fact that the working surface of the primary electrode, which is covered with the polymer solution consists of the relevant portions of the surfaces of a number of freely available (not attached to anything) elements that are in working condition, partly submerged, resting on the bottom of the bath or shower tray or other support structure or structures, and the method used device, providing a coating solution of the polymer on the exposed surface free of service is the R elements, forcing them to rotate in the polymer solution so that their surfaces were covered with a thin layer of polymer solution.

These elements are usually rounded, and most usually round, at least one projection. It can be spheres, cylinders, or intermediate ellipsoidal shape, although currently it is preferable spherical shape.

The rotation can be accessed by tilting the pan or tub or inside the supporting element.

Alternatively, support plate or similar element can move relative to these elements to cause their rotation, in this case, usually so that it was the return movement backward and forward or rotational movement.

In another embodiment, the elements can be given a rotary movement, using rods or frame. For example, the elements can be placed in the natural frame to fill a certain area of these elements, supported on a support structure in the form under these elements moving surface, for example, a wide endless conveyor belt, while the entire Assembly is half immersed in the polymer solution.

In the case of steel elements or elements made of other magnetic material, they can be lead into rotation under wasastjerna magnetic fields.

The surface elements can usually be smooth, but it can also be textured in various ways, for example, in the form of pointed protrusions, grooves in the surface, or otherwise deforming the smooth surface of the element.

Elements can be of any size ranging from about 1 mm to 300 mm, usually from about 3 mm to 30 mm, the Elements may be made of steel, glass or any other suitable material, provided that they must be sufficiently stable in the polymer solution and is able to work with the relevant mechanisms of the device.

The polymer solution may be a solution of any natural or synthetic polymer in an appropriate solvent, or a mixture of different polymers or Sol-gel mixture, or any other combination of components, which can be used to produce fibers in the process of electroprecizia. The polymer solution may also contain additives necessary to modify the surface tension, viscosity and/or other rheological and electrical properties of solution.

According to the second aspect of the present invention, the proposed device for producing fine fibers as described above, in which the primary electrode is located at some distance from the counter-electrode and generally parallel to it, and the device characteristic is cherished fact, the working surface of the primary electrode, which should be covered with the applied polymer solution consists of the relevant portions of the surfaces of many emergent in working condition, readily available (not attached to anything) elements resting on the bottom of the bath or shower tray or other supporting element or elements, and in this device enabled device, allowing you to apply the polymer solution on the exposed surface of the readily available elements, bringing them into rotation in the polymer solution so that their surface was covered with a thin layer of polymer solution.

Additional features of this aspect of the present invention follow directly from the additional characteristics of the first aspect of the present invention.

The method is applicable also in combination with specialized collectors nanofibres for the production of geometrically more complex structures of the nanofibers, for example, with apparatus for forming strands of nanofibers described in our pending International patent application published under number WO 2008062264.

To provide a more complete understanding of this invention, hereinafter will be described some examples of its implementation, with reference to the accompanying drawings.

Brief description of drawings

On artiach:

Figure 1 is a schematic illustration of a side view of one example implementation of the present invention;

Figure 2 is a schematic illustration of a side view of a second example implementation of the present invention;

Figure 3 is a side view of a third example implementation of the present invention;

Figure 4 is a top view of the third example of implementation, illustrated in Figure 3;

Figure 5 is a schematic illustration of a side view of the fourth example implementation of the present invention; and

6 and 7 illustrate other possible forms of elements.

Detailed description with reference to the drawings

In the example implementation of the present invention, is illustrated in figure 1, numerous freely available elements (1), more specifically, a sphere located so as to constitute what in fact is the primary electrode; numerous readily available areas are organized so that they can roll under the force of gravity on an inclined located the bath (2)containing solution (3) polymer, if this tub is tilted accordingly. Thus, the tub tilt with the aim of creating a thin layer of polymer solution on the protruding surfaces of the spheres, which are only partially immersed in the solution.

Source (4) about who has the applying a high voltage between the primary electrode and counter-electrode (5), which is mainly parallel to the primary electrode, but is located some distance from him. Electrical contact with a solution of polymer deposited on the speakers from the solution surface areas, supported by the contact plate (6), upon which the sphere inside of the bath.

Periodic movement of the spheres is obtained by giving the tub tilt first in one direction and then in the opposite, or at least in the other direction, so that the spheres are moved one after another, and usually there and back, within the bath, each time rotating and collecting on its surface a thin layer of polymer solution. Giving a tilt tub can be done by any method, for example, by extending and retracting the supporting device (7), consisting of a piston and cylinder located at the corners of the bath or near the corners of the bath. The action of such device consisting of a piston and cylinder may be hydraulic or pneumatic and can be adjusted automatically, for example, using an appropriately set according to the time of the automatic valve device (8). Alternatively, the bath may be based on respective eccentrics, which upon rotation causes successive bends in different directions.

Receiving fibers regulate, in particular, agulira voltage, applied between the primary electrode and counter-electrode, so that under the influence of an applied high voltage from the surfaces of the spheres broke numerous jets (9) electroprecizia. Except for the design of the primary electrode, the device operates manufacturing principles, which are well known in the art, and further details are not necessary to include in the text of this patent description.

However, it should be noted that sometimes it may be necessary to initiate the formation of a jet at the fields by physical contact with the moistened surface, for example, touching the wetted surface with a glass rod. The result is the formation of the liquid surface of the liquid ledge pointed shape, for example, removing a glass rod. Then from this point erupt one or more jets. The high charge on the spheres leads then automatically splitting the first jet (or jets) into multiple streams that are distributed to other areas without additional external intervention. Such initiation can also be implemented in many other ways, including any physical deformation of the liquid layer on the sphere.

It should be understood that instead of spheres, you can use any suitable shape or combination of shapes, to whom that allow the elements to rotate. For example, the elements may be cylindrical in shape or even ellipsoidal shape.

Now consider Figure 2, where is illustrated a similar form in which the same sphere (11) rely on submerged horizontal supporting structure (12)that can move in the bath (13) back and forth or in a circle, which causes the sphere to roll in solution (14) of the polymer inside the bath. This movement is organized so as to cause the formation of a thin layer of polymer solution on the speakers from the solution the surfaces of the spheres, as described above.

In the course of work under the influence of an applied high voltage from the surfaces of the spheres are pulled out numerous jets (15) electroprecizia. The movement of the support structure can be achieved using any suitable mechanism; as one of the possibilities can be considered an electric motor driving the Cam, indicated by position (16).

Referring to Figure 3 and 4, a third form of the present invention sphere (17) partially immersed in a bath (19), and their support are parallel to each other rotating rods (18). The rods (18) are moved in unison by means of a chain (20), resulting in a sphere (17) are rotated. Part of the spheres (17)located between terminals (18), immersed in rest the R polymer, during rotation of the surface areas covered with a thin layer of polymer solution. Depending on the size of the rods and spheres and the distance between the terminals can be fully immersed or extend slightly above the surface of the polymer solution, while the sphere is immersed in the solution part.

In the example implementation of the present invention, is illustrated in Figure 5, the sphere (21) rely on a wide endless belt (conveyor) (22)located inside of the bath (23) so that when the tape spheres revolve, with the above result.

The method and apparatus according to this invention allow spinning with high performance without difficulties associated with the use of multi-needle nozzles. This is achieved by creating what can be described as solid, bubble-like surface. Covered with a film of solution elements mimic bubbles on the surface of the spinning solution of the polymer, but have the advantage that they do not burst, leading to harmful spray, and maintain a constant geometry, which leads to better regulation process, predictability and uniformity.

When using many freely available (not connected to anything) the rotating elements of the present invention overcome the limitations that Nala is my design mounted on the axis of the cylinder device NanoSpider. The application of the many freely available (i.e. not attached to the axis) of the rotating elements allows simultaneous use of rotating elements of different sizes, a more optimal use of the area of the spinning equipment in the more dense packing of rotating elements, and provides an additional degree of freedom with respect to maneuverability of rotating elements and greater freedom of possibilities when designing equipment.

It should be understood that within the scope of protection of the present invention can be implemented many different forms of its implementation, without going beyond the scope of this volume. In particular, numerous possible variations in the shape and configuration of the elements and how they support. For example, they may be generally cylindrical, as illustrated in Fig.6, although there may be elliptical, as illustrated in Fig.7. If desired, the elements may also have a textured surface, which may include many small ledges.

1. The method of obtaining thin fibers by electroprecizia fibers by applying an electric field between the primary electrode and counter-electrode (5), located at some distance from the primary electrode and generally parallel to it, which for men is our least the working surface of the primary electrode is covered with solution (3) polymer, and between the primary electrode and counter-electrode to create an electric field of sufficient magnitude to cause the formation of thin fibers (9) in the space between the electrodes, and the method, characterized in that the working surface of the primary electrode, which is covered with the polymer solution consists of the relevant portions of the surfaces of many emergent in working condition, readily available (not attached to anything) elements(1, 11, 17, 21), which rest on the bottom of the tub (2), or pallet, or other support structure or structures (12, 18, 22), and used the device, facilitating the application of the polymer solution on the speakers from the solution surface free hosted by bringing them into rotation in the polymer solution so that their surfaces become covered with a thin layer of polymer solution.

2. The way to obtain fine fibers according to claim 1, in which the elements are all at least one projection, and are selected from spherical, cylindrical, and ellipsoidal forms.

3. The method of obtaining thin fibers according to any one of claims 1 or 2, which used the device, facilitating the application of the polymer solution on the speakers from the solution surface free of floated elements, causing them to rotate in R is the target polymer, includes tools (7, 8) slant tray, tub or other structures supporting members to cause them to rotate in the polymer solution.

4. The method of obtaining thin fibers according to any one of claims 1 or 2, which used the device, facilitating the application of the polymer solution on the speakers from the solution surface free of floated elements, causing them to rotate in the polymer solution, includes rods (18).

5. The method of obtaining thin fibers according to any one of claims 1 or 2, which used the device, facilitating the application of the polymer solution on the speakers from the solution surface free of floated elements, causing them to rotate in the polymer solution includes a wide endless belt (22) under the elements are capable of movement to cause the rotation of the elements, half immersed in the polymer solution.

6. The method of obtaining thin fibers according to any one of claims 1 or 2, which used the device, facilitating the application of the polymer solution on the speakers from the solution surface free of floated elements, causing them to rotate in the polymer solution, in the case of steel or elements made of other magnetic material, includes means for creating a magnetic field that can cause the rotation of the elements under who is esteem variable magnetic fields.

7. The method of obtaining thin fibers according to any one of claims 1 or 2, in which the elements have a size in the range from 1 mm to 300 mm

8. The way to obtain fine fibers according to claim 7, in which the elements have a size in the range from 3 mm to 30 mm

9. Apparatus for producing fine fibers by the method described in any of the preceding paragraphs, in which the primary electrode is located at a distance from the counter-electrode and generally parallel to it, and the device, wherein the working surface of the primary electrode, which when used, must be covered with a polymer solution, consists of the relevant portions of the surfaces of many emergent in working condition, readily available (not attached to anything) elements that rest on the bottom of the tub, or pallet, or other support structure, or structures, with the device used device, facilitating the application the polymer solution on the surface of the protruding above the surface of the solution freely available elements, causing them to rotate in the polymer solution so that their surface was covered with a thin layer of polymer solution.

10. The device according to claim 9, in which the elements are all at least one projection and selected from spherical, cylindrical and ellipticus the x form.

11. Device according to any one of p or 10, in which the used device, facilitating the application of the polymer solution on the speakers from the solution surface free of floated elements, causing them to rotate in a polymer solution that includes tools slant tray, tub or other structures supporting members to cause them to rotate in the polymer solution.

12. Device according to any one of p or 10, in which the used device, facilitating the application of the polymer solution on the speakers from the solution surface freely spaced elements, causing them to rotate in the polymer solution, includes rods, frames or wide endless belt beneath the elements and in each case can be moved so as to cause the rotation of the elements, semi-immersed in the polymer solution.



 

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6 cl, 1 tbl

FIELD: electricity.

SUBSTANCE: fibre electrospinning is carried out from an electroconductive solution of polymer in presence of electric field between a nozzle and a source of earthing. In the method realisation the polymer before and after electrospinning process is exposed to linking reaction. At the same time the polymer contains linked silane groups along the length of the main chain of polymer, and the linked groups react with water, including water contained in air. The fibre made according to the method of electrospinning contains links -Si-O-Si-.

EFFECT: using linking reaction before and during the process of electrospinning results in increased viscosity of polymer solution, making it possible to form the fibre and to reduce usage of thickeners to the minimum.

14 cl, 2 dwg, 1 tbl, 3 ex

FIELD: electricity.

SUBSTANCE: method includes spinning of electroconductive solution of organic and non-organic polymers and predecessor of organic polymer in presence of electric field between tip and earthing source till composite fiver is received. At that organic and non-organic phases of composite fibres are mixed and react with each other with production of -Si-O-M- links, where M is selected from the group consisting of Si, Ti, Al and Zr. The author offers composite fibre received by the above method and composite product including polymer matrix and composite fibres introduced to it.

EFFECT: improvement of method.

28 cl, 2 dwg, 1 tbl, 5 ex

FIELD: chemistry.

SUBSTANCE: electrostatic field is formed in fibre-forming space between the fibre-forming element of a fibre-forming electrode, which is connected to one terminal of a high-voltage source and is located in a fibre-forming position, and a precipitation electrode connected to the second terminal of the high-voltage source to which a polymer matrix is fed from a reservoir with the matrix in an electrostatic field for forming fibre on the surface of the fibre-forming element of the fibre-forming electrode, wherein temperature of the fibre-forming elements of the fibre-forming electrode is raised higher than ambient temperature by direct contact heating of the fibre-forming elements.

EFFECT: more technologically effective method, and simple and efficient design of the apparatus.

8 cl, 2 dwg

FIELD: medicine.

SUBSTANCE: invention relates to chemical-pharmaceutical industry and represents artificial dura mater, produced from electrospinning layers by technology of electorspinning, with electrospinning layer, consisting of, at least, hydrophobic electrospining layer, which is produced from one or several hydrophobic polymers, selected from polylatic acid and polycaprolactone.

EFFECT: invention ensures creation of artificial dura mater, which has good tissue compatibility, anti-adhesiveness and possibility of introducing medications, preventing cerebrospinal fluid outflow during regeneration of person's own dura mater.

30 cl, 7 ex, 11 dwg

FIELD: chemistry.

SUBSTANCE: method and apparatus for producing fine fibres via fibre electrospinning by applying an electric field between a primary electrode and a counter electrode lying at a distance from the primary electrode and often parallel thereto. The working surface of the primary electrode is coated with a polymer solution. An electric field is created between the primary electrode and the counter electrode having sufficient strength to cause formation of fine fibres in the space between the electrodes. The working surface of the primary electrode coated with a polymer solution consists of corresponding parts of surfaces of a plurality of elements that are semi-submerged in the working state and are freely lying (not connected to anything), said elements resting at the bottom of a bath or tray or some other supporting structure(s). A tool is used, which enables to apply the polymer solution on the surface of the freely lying elements protruding from the solution via rotation thereof in the polymer solution, such that their surface is coated with a thin layer of the polymer solution.

EFFECT: method and apparatus according to the present invention enable to perform spinning with high efficiency while eliminating problems encountered in the previous technological level.

12 cl, 8 dwg

FIELD: chemistry.

SUBSTANCE: invention relates to technology of obtaining ultrathin polymer fibres by method of electrospinning and can be used for spinning non-woven porous fibrous materials, applied as separating partitions, for instance, for filtration of gases and liquids, for manufacturing diffusion partitions, separators of chemical sources of current, etc. Solution for spinning contains 2.5-4 wt.p. of phenolformaldehyde resin, 2.5-4 wt.p. of polyvinyl butyral, 92-95 wt.p. of ethyl alcohol and as modifying additives 0.02-0.2 wt.p. of tetrabutylammonium iodide or 0.01-0.1 wt.p. of lithium chloride.

EFFECT: invention provides increase of solution electroconductivity, increased output of ultrathin fibres with diameter less than 0,1 mcm.

1 tbl, 7 ex

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