JP4602752B2 - Twisted yarn, twisted yarn manufacturing method and twisted yarn manufacturing apparatus - Google Patents

Description

  The present invention relates to a twisted yarn, a manufacturing method thereof, and a manufacturing apparatus thereof. More specifically, the present invention relates to a twisted yarn as a fiber structure useful as a substrate for culturing cells, a method for producing the yarn, and a device for producing the yarn.

  In the field of regenerative medicine, a fiber structure may be used as a base material when culturing cells. As this fiber structure, for example, polyglycolic acid used for surgical sutures has been studied. (For example, see Non-Patent Document 1).

  However, since the fiber structure obtained by these usual methods has a fiber diameter that is too large, the effective area to which cells can adhere is small, and in order to increase the surface area, a fiber structure having a smaller fiber diameter is desired. It was.

  In general, an electrostatic spinning method is known as a method for producing a fiber structure having a small fiber diameter (see, for example, Patent Documents 1 and 2). The electrospinning method includes a step of introducing a liquid, for example, a solution containing a fiber-forming substance, into an electric field, thereby causing the liquid to flow toward an electrode and forming a fiber structure. Usually, the fiber-forming substance is cured while it is squeezed out of solution. Curing is performed, for example, by cooling (such as when the spinning liquid is a solid at room temperature), chemical curing (such as treatment with curing steam), or evaporation of the solvent. Moreover, the obtained fiber structure is collected on the electrode arrange | positioned suitably, and can also peel from there, if necessary.

  It is known to use a fiber structure obtained by an electrospinning method as a substrate for culturing cells. For example, the regeneration of blood vessels has been studied by forming a fiber structure made of polylactic acid by an electrospinning method and culturing smooth muscle cells thereon (see, for example, Non-Patent Document 2).

  However, in order to produce a fiber structure by an electrospinning method, an electrode for collection is required, so that many are planar bodies, and the shape that can be produced is limited. However, since there are tissues of various structures in the living body, it is very important to produce structures other than planar bodies by the electrospinning method. The demand for was great.

JP-A 63-145465 JP 2002-249966 A Noriya Ohno, Director of Masao Aizawa, “Regenerative Medicine”, NTS Corporation, January 31, 2002, page 258 “Journal of Biomaterials Applications” by Joel D. Stitzel, Kristin J. Pawlowski, Gary E. Wnek, David G. Simpson, Gary L. Bowlin. ), Sage Publications, 2001, 16, p. 22-33

  An object of the present invention is to provide a twisted yarn composed of multifilaments suitable for cell culture, having a large gap between fibers and a small fiber diameter, a method for producing the same, and a device for producing the same.

As a result of intensive studies in view of the above prior art, the present inventors have completed the present invention.
That is, the object of the present invention is to
This can be achieved by a twisted yarn which is composed of multifilaments having an average fiber diameter of 5 μm or less and substantially free of filaments having a fiber diameter of 10 μm or more.

Furthermore, another object of the present invention is to
A step of producing a solution by dissolving a fiber-forming solute in a solvent; a step of applying a high voltage to the solution; a step of ejecting the solution; and a fiber structure by evaporating the solvent from the ejected solution A step of eliminating the charge of the formed fiber structure, a step of accumulating the fiber structure due to the charge disappearance, and a step of extracting a fiber bundle from one end of the accumulated fiber structure. The twisted fiber bundle includes a step of twisting the drawn fiber bundle and a step of winding the twisted fiber bundle.

Finally, yet another object of the present invention is to
A solution supply device that supplies a solution in which a fiber-forming solute is dissolved to the tip of the nozzle, a fiber structure manufacturing device that produces the fiber structure by ejecting the solution from the tip of the nozzle, and the fiber structure on the stacking plate A fiber structure depositing device to be deposited on a fiber structure, a twisting device for pulling out a fiber bundle from the fiber structure deposited on the deposition board, twisting the fiber bundle, and a winding device for winding the twisted fiber bundle And achieved by a twisted yarn manufacturing apparatus.

The twisted yarn of the present invention has a small average fiber diameter of multifilaments constituting the yarn, and is effective as a base material for cell culture.
In addition, the obtained twisted yarn can be used as it is, and various structures can be formed by processing such as weaving, and it can be combined with other members according to handling characteristics and other requirements. Can also be used.

Hereinafter, the present invention will be described in detail.
In the twisted yarn of the present invention, first, the average fiber diameter of the multifilament to be formed is 5 μm or less, and a filament having a fiber diameter of 10 μm or more is substantially absent.

  Here, in the present invention, the “twisted yarn” is a substantially cylindrical structure in which multifilaments are ground and twisted. The diameter of the twisted yarn is not particularly limited as long as the target cells are cultured, but is preferably 0.1 mm to 10 mm, and more preferably 0.5 to 5 mm. In addition, the number of twists of the twisted yarn is not particularly limited as long as the target cells are cultured, but is preferably 10 to 2000 times / m, more preferably 100 to 1000 times / m. is there.

  Next, it will be described that the average fiber diameter of the multifilaments constituting the twisted yarn is 5 μm or less. When the average fiber diameter of the multifilament constituting the twisted yarn of the present invention exceeds 5 μm, the specific surface area of the fiber becomes too small, and as a result, the number of cells that can be cultured decreases. Moreover, if the average fiber diameter of a multifilament is 0.1 micrometer or more, the intensity | strength of the obtained twisted yarn will become sufficient. The average fiber diameter of the multifilaments constituting the twisted yarn is preferably in the range of 0.2 to 3 μm.

  Next, the fact that filaments having a fiber diameter of 10 μm or more are not substantially contained will be described. In the present invention, “substantially not contained” means that a filament having the above fiber diameter is not observed when an arbitrary portion of the twisted yarn is observed in an electron microscope.

  In addition, if the multifilament forming the twisted yarn of the present invention contains a filament having a fiber diameter of 10 μm or more, the specific surface area of the fiber is decreased, and the number of cells that can be cultured is reduced. This is also undesirable because flexibility suitable for the above is impaired. In order to obtain flexibility suitable for cell culture, it is more preferable that filaments having a fiber diameter of 8 μm or more are not substantially contained.

  The multifilament constituting the twisted yarn of the present invention may be composed of either an inorganic compound or an organic polymer, but is preferably composed of an organic polymer, and the organic polymer is soluble in an organic solvent. In particular, the organic solvent is preferably a halogen element-containing compound. Examples of such organic polymers include polyvinyl chloride, polyacrylonitrile, polylactic acid, polyglycolic acid, polylactic acid-polyglycolic acid copolymer, polycaprolactone, polybutylene succinate, polyethylene succinate, polystyrene, and polycarbonate. , Polyhexamethylene carbonate, polyarylate, polyvinyl isocyanate, polybutyl isocyanate, polymethyl methacrylate, polyethyl methacrylate, poly normal propyl methacrylate, poly normal butyl methacrylate, polymethyl acrylate, polyethyl acrylate, polybutyl acrylate, polyethylene terephthalate, poly Trimethylene terephthalate, polyethylene naphthalate, polyparaphenylene terephthalamide, polypara Enylene terephthalamide-3,4'-oxydiphenylene terephthalamide copolymer, polymetaphenylene isophthalamide, cellulose diacetate, cellulose triacetate, methylcellulose, propylcellulose, benzylcellulose, fibroin, natural rubber, polyvinyl acetate , Polyvinyl methyl ether, polyvinyl ethyl ether, polyvinyl normal propyl ether, polyvinyl isopropyl ether, polyvinyl normal butyl ether, polyvinyl isobutyl ether, polyvinyl tertiary butyl ether, polyvinylidene chloride, poly (N-vinyl pyrrolidone), poly (N-vinyl carbazole) ), Poly (4-vinylpyridine), polyvinyl methyl ketone, polymethyl isopropenyl ketone, polyethylene Oxide, polypropylene oxide, polycyclopentene oxide, polystyrene sulfone, nylon 6, nylon 66, nylon 11, nylon 12, nylon 610, nylon 612, as well as their copolymers.

  Of these, preferred are polylactic acid, polyglycolic acid, polylactic acid-polyglycolic acid copolymer, polycaprolactone, polybutylene succinate, and polyethylene succinate and aliphatic polyesters such as these copolymers, and Preferably, polylactic acid, polyglycolic acid, polylactic acid-polyglycolic acid copolymer, and polycaprolactone are used. Of these, polylactic acid is particularly preferred.

Next, an embodiment for producing the twisted yarn of the present invention will be described.
In order to produce the twisted yarn of the present invention, any method can be adopted as long as it can obtain a twisted yarn that satisfies the above-mentioned requirements at the same time, but a solution is produced by dissolving a fiber-forming solute in a solvent. A step of applying a high voltage to the solution, a step of ejecting the solution, a step of evaporating a solvent from the ejected solution to form a fiber structure, and a step of forming the fiber structure Erasing the charge, accumulating a fiber structure due to the loss of electric charge, extracting a fiber bundle from one end of the accumulated fiber structure, and twisting the drawn fiber bundle, A preferred embodiment is a method for producing a twisted yarn including a step of winding the twisted fiber bundle.

  First, a step of producing a solution by dissolving a fiber-forming solute in a solvent, a step of applying a high voltage to the solution, and a step of ejecting the solution from the solution will be described. Hereinafter, the step of producing a solution by dissolving a fiber-forming solute in a solvent, the step of applying a high voltage to the solution, and the step of ejecting the solution from the solution are collectively referred to as an electrostatic spinning method. I will do it.

  Electrospinning is a method in which a solution in which a fiber-forming substrate is dissolved is discharged into an electrostatic field formed between electrodes, the solution is spun toward the electrodes, and the fibrous material formed is collected It is a method of obtaining a fiber structure by accumulating on the fibrous material, and the fibrous substance is not only a state in which the solvent in which the fiber-forming substrate is dissolved is distilled off to form a fiber laminate, The state in which the solvent is contained in the fibrous material is also shown.

Next, an apparatus used in the electrostatic spinning method will be described.
The above-described electrode can be used as long as it has conductivity, and any metal, inorganic, or organic material has a thin film of conductive metal, inorganic, or organic material on an insulator. May be.

  The electrostatic field is formed between a pair or a plurality of electrodes, and a high voltage may be applied to any of the electrodes. This includes, for example, the case where two high-voltage electrodes with different voltage values (for example, 15 kV and 10 kV) and a total of three electrodes connected to ground are used, or when more than three electrodes are used. Shall also be included.

Next, a manufacturing method of the fiber structure constituting the twisted yarn of the present invention by the electrospinning method will be described step by step.
First, a solution is produced by dissolving a fiber-forming substrate. The concentration of the fiber-forming substrate with respect to the solvent in the solution in the production method of the present invention is preferably 1 to 30% by weight. If the concentration of the fiber-forming substrate is less than 1% by weight, it is not preferable because the concentration is too low to make it difficult to form a fiber structure. On the other hand, if it is greater than 30% by weight, the fiber diameter of the resulting fiber structure is undesirably large. The concentration of the fiber-forming substrate with respect to the solvent in the solution is more preferably 2 to 20% by weight.

Moreover, a solvent may be used individually by 1 type and may combine several solvent. The solvent is not particularly limited as long as it can dissolve a fiber-forming substrate and evaporates at the stage of spinning by an electrostatic spinning method to form a fiber. For example, acetone, chloroform, ethanol , Isopropanol, methanol, toluene, tetrahydrofuran, water, benzene, benzyl alcohol, 1,4-dioxane, propanol, methylene chloride, carbon tetrachloride, cyclohexane, cyclohexanone, phenol, pyridine, trichloroethane, acetic acid, formic acid, hexafluoroisopropanol, hexa Examples include fluoroacetone, N, N-dimethylformamide, acetonitrile, N-methylmorpholine-N-oxide, 1,3-dioxolane, methyl ethyl ketone, and mixed solvents of the above solvents.
Of these, methylene chloride, methanol, ethanol and a mixed solvent thereof are preferably used in view of handling properties and physical properties.

Next, the step of spinning the solution by the electrostatic spinning method will be described.
Any method can be used to eject the solution into the electrostatic field, for example, by feeding the solution to a nozzle, placing the solution in a suitable position in the electrostatic field, and applying the solution from the nozzle to the electric field. Can be made into a fiber by stringing.

Hereinafter, this electrostatic spinning method will be described in more detail with reference to FIG.
An injection needle-like solution ejection nozzle (in FIG. 1) in which voltage is applied to the tip of the cylindrical solution holding tank (3 in FIG. 1) of the syringe by an appropriate means such as a high voltage generator (5 in FIG. 1). 1) is installed, and the solution (2 in FIG. 1) is guided to the tip of the solution ejection nozzle. The tip of the solution ejection nozzle (1 in FIG. 1) is arranged at an appropriate distance from the grounded electrode (4 in FIG. 1), and the solution (2 in FIG. 1) is the tip of the solution ejection nozzle (1 in FIG. 1). The fiber structure can be formed between the nozzle tip and the electrode (4 in FIG. 1).

  When the solution is supplied from the nozzle into the electrostatic field, the production rate of the fiber structure can be increased by using several nozzles in parallel. Further, the distance between the electrodes depends on the charge amount, the nozzle size, the ejection amount of the solution from the nozzle, the solution concentration, etc., but when it is about 10 kV, the distance of 5 to 20 cm is appropriate. The applied electrostatic potential is generally 3 to 100 kV, preferably 5 to 50 kV, and more preferably 5 to 30 kV. The desired potential may be generated by any appropriate method known in the art.

  Further, the obtained fiber structure may be subjected to heat treatment or chemical treatment, and an emulsion, an organic substance, or an inorganic substance powder may be mixed with the fiber-forming substrate at any stage before spinning. .

  Next, a step of eliminating the charge of the jetted solution and a step of obtaining a fiber structure accumulated by the charge loss will be described. In the present invention, the fiber structure is deposited between the nozzle and the collection electrode by erasing the charge of the solution while spinning the solution toward the collection substrate. If the room temperature is normal, the solvent completely evaporates until the fibrous structure is deposited, but if the solvent evaporation is insufficient, the solvent may be drawn under reduced pressure. When this fiber structure is deposited, filaments satisfying at least the fiber average diameter are formed. Further, the temperature at which the spinning is performed depends on the evaporation behavior of the solvent and the viscosity of the spinning solution, but is usually in the range of 0 to 50 ° C.

  Next, the step of eliminating the charge of the solution will be described. The method of eliminating the charge of the solution is not particularly limited as long as the charge of the solution is eliminated and a fiber structure is formed, but a preferable method is a method of eliminating the charge with an ionizer. An ionizer is an apparatus that can generate ions by a built-in ion generator and discharge the charged substances to discharge the ions, thereby eliminating the charge of the charged objects. The ionizer used in the present invention is not particularly limited as long as the fiber structure is formed, but a preferable ion generator is a device that generates ions by applying a high voltage to a built-in discharge needle.

  Next, a step of drawing a fiber bundle from one end of the accumulated fiber structure, a step of twisting the drawn fiber bundle, and a step of winding the twisted fiber bundle will be described. In the present invention, by pulling out one end of the fiber structure accumulated by the above method, a fiber bundle can be continuously obtained by entanglement between the fiber structures. Furthermore, the obtained fiber bundle is twisted by various methods and wound to obtain a twisted yarn.

  In order to produce the twisted yarn of the present invention, any production device capable of obtaining a twisted yarn that simultaneously satisfies the above-mentioned requirements can be adopted, but a solution in which a fiber-forming solute is dissolved is used as a nozzle tip. A solution supply device for supplying the fiber structure, a fiber structure production device for producing a fiber structure by ejecting the solution from a nozzle tip, a fiber structure deposition device for depositing the fiber structure on a deposition plate, and the deposition disc One preferred embodiment is a twisted yarn production apparatus comprising a twisting device that pulls out a fiber bundle from the fiber structure deposited thereon and twists the fiber bundle, and a winding device that winds the fiber bundle that has been twisted. it can.

A production apparatus for producing the twisted yarn will be described with reference to FIG.
An injection needle-like solution ejection nozzle (in FIG. 1) in which voltage is applied to the tip of the cylindrical solution holding tank (3 in FIG. 1) of the syringe by an appropriate means such as a high voltage generator (5 in FIG. 1). 1) is installed, and the solution (2 in FIG. 1) is guided to the tip of the solution ejection nozzle. The grounded electrode (4 in FIG. 1), the ionizer (6 in FIG. 1), and the tip of the solution ejection nozzle (1 in FIG. 1) are installed at appropriate distances, respectively, and the solution (2 in FIG. 1) Is ejected from the tip of the solution jet nozzle (1 in FIG. 1) and placed on the fiber structure deposition disk (7 in FIG. 1) installed between the nozzle tip and the ionizer (6 in FIG. 1). A fiber structure is formed. The fiber bundle drawn from one end of the accumulated fiber structure is drawn into a winding device (11 in FIG. 1 and 11 in FIG. 2), and the fiber bundle is wound up by rotating a winding roller (12 in FIG. 2). . At that time, the fiber bundle is twisted by applying a rotation having a rotation axis perpendicular to the rotation axis of the winding roller (12 in FIG. 2) to the winding device (11 in FIG. 2, 11 in FIG. 2). Device for producing twisted yarn.

Further, another embodiment for producing the twisted yarn will be described with reference to FIG.
An injection needle-like solution ejection nozzle (in FIG. 3) in which a voltage is applied to the tip of the cylindrical solution holding tank (3 in FIG. 3) of the syringe by appropriate means, for example, a high voltage generator (5 in FIG. 3). 1) is installed, and the solution (2 in FIG. 3) is guided to the tip of the solution ejection nozzle. The grounded electrode (4 in FIG. 3), the ionizer (6 in FIG. 3), and the tip of the solution ejection nozzle (1 in FIG. 3) were installed at appropriate distances, respectively, and the solution (2 in FIG. 3) Is ejected from the tip of the solution jet nozzle (1 in FIG. 3) and placed on the fiber structure deposition disk (7 in FIG. 3) installed between the nozzle tip and the ionizer (6 in FIG. 3). A fiber structure is formed. A fiber bundle is pulled out from one end of the accumulated fiber structure, and at that time, the fiber structure deposition disk (7 in FIG. 3) is rotated relative to the take-up roller (12 in FIG. 3) to form the fiber bundle. It is an apparatus which twists and winds up the obtained twisted yarn with a winding roller (12 in FIG. 3).

Next, another embodiment for producing the twisted yarn will be described with reference to FIG.
An injection needle-like solution ejection nozzle (in FIG. 6) in which voltage is applied to the tip of the cylindrical solution holding tank (3 in FIG. 6) of the syringe by an appropriate means, for example, a high voltage generator (5 in FIG. 6). 1) is installed, and the solution (2 in FIG. 6) is guided to the tip of the solution ejection nozzle. The grounded electrode (4 in FIG. 6), the ionizer (6 in FIG. 6), and the tip of the solution ejection nozzle (1 in FIG. 6) were installed at appropriate distances, respectively, and the solution (2 in FIG. 6) Is ejected from the tip of the solution jet nozzle (1 in FIG. 6), and the fiber structure is placed on the fiber trapping device (17 in FIG. 6) installed between the nozzle tip and the ionizer (6 in FIG. 6). Form the body. The fiber bundle is drawn from one end of the accumulated fiber structure, and the fiber bundle is twisted by rotating the fiber capturing device (17 in FIG. 6) relative to the winding roller (12 in FIG. 6). It is an apparatus which winds up the obtained twisted yarn with a winding roller (12 in FIG. 6).

  Here, the fiber capturing device 17 is formed by bending a tube and joining a circular support and both ends of the tube. FIG. 6 of the present specification describes an example using three tubes. Needless to say, the same shape (for example, a combination of plates) can be used as long as it has a function of capturing (tangling or catching) the fibers.

Furthermore, another embodiment for producing the twisted yarn will be described with reference to FIG.
An injection needle-like solution ejection nozzle (in FIG. 8) in which voltage is applied to the tip of the cylindrical solution holding tank (3 in FIG. 8) of the syringe by appropriate means, for example, a high voltage generator (5 in FIG. 8). 1) is installed, and the solution (2 in FIG. 8) is guided to the tip of the solution ejection nozzle. A funnel-shaped fiber collecting container provided with a grounded electrode (4 in FIG. 8) and a discharge needle connected to an ionizer (6 in FIG. 8) and a tip of the solution ejection nozzle (1 in FIG. 8) are respectively connected appropriately. It installs so that it may become a distance, a solution (2 in FIG. 8) is ejected from the front-end | tip part of the said solution ejection nozzle (1 in FIG. 8), and a fiber structure is formed in a fiber collection container. Here, in the fiber collecting container, an air vortex is generated in the funnel shape through the compressed air supply nozzle (13 in FIG. 8) and the hole leading to the lower outlet of the funnel-shaped bottom is approximately centered. The fiber bundle drawn out from the funnel-shaped outlet portion by jetting compressed air as described above is twisted by the air flow, and the obtained twisted yarn is wound up by a winding roller (12 in FIG. 8). .

  Here, in FIG. 8 of the present specification, two compressed air supply nozzles are installed as shown in the figure, but an air vortex is generated around the hole connected to the lower outlet of the funnel-shaped bottom. As long as you do, you may install in any direction.

Further, in FIG. 8 of the present specification, the solution ejection nozzle and the lower outlet portion of the funnel-shaped bottom are described so as to overlap, but there is no problem even if there is a deviation.
Further, although one injection needle-like solution ejection nozzle (1 in FIG. 8) is installed in FIG. 8 of the present specification, a plurality of nozzles may be installed according to the production amount.

  Further, in FIG. 8 of the present specification, a compressed air supply nozzle generates an air vortex that is substantially centered on a hole connected to the lower outlet of the funnel-shaped bottom, but from the lower outlet of the funnel-shaped bottom. By sucking in air, an air vortex may be generated with the hole connected to the lower outlet of the funnel-shaped bottom portion approximately at the center.

  In addition, in order to prevent the solution from solidifying at the tip of the solution jet nozzle by directly feeding the air from the compressed air feed nozzle to the injection needle-like solution jet nozzle in FIG. 8 of the present specification, An enclosure may be provided in the solution ejection nozzle.

  EXAMPLES Hereinafter, the present invention will be described more specifically with reference to examples. However, the present invention is not limited to these examples. The evaluation items in the following examples and comparative examples were carried out by the following methods.

Number of twisted yarns:
When the rotational speed of the winding device 11 or the rotational speed of the fiber structure deposition disk 7 or the fiber capturing device 17 is A (rpm) and the winding speed of the winding roller 12 is B (m / min), the following formula Was used to calculate the number of twists C (times / m).
[Equation 1]
C = A / B

Average fiber diameter of twisted yarn:
10 points are selected at random from the obtained twisted yarns, and when the cross section of the twisted yarn is a circle, the diameter is the fiber diameter, and when it is an ellipse, the average of the major axis and the minor axis is the fiber diameter, and all fiber diameters ( The average value of n = 10) was determined and used as the average fiber diameter of the twisted yarn.

Multifilament average fiber diameter:
The surface of the obtained twisted yarn was photographed with a scanning electron microscope (S-2400 manufactured by Hitachi, Ltd.) (magnification 2000 times), and randomly selected 20 points from the photograph to measure the diameter of the filament. The average value of the fiber diameters (n = 20) was determined and used as the average fiber diameter of the multifilaments.

[Example 1]
1 part by weight of polylactic acid (manufactured by Shimadzu Corporation: trade name “Lacty 9031”), 3 parts by weight of ethanol (made by Wako Pure Chemical Industries, Ltd., special grade), 6 parts by weight of methylene chloride (made by Wako Pure Chemical Industries, Ltd., special grade) The parts were mixed at room temperature (25 ° C.) to prepare a solution. A twisted yarn was obtained using the apparatus shown in FIGS. The inner diameter of the ejection nozzle 1 is 0.8 mm, the voltage is 15 kV, the distance from the ejection nozzle 1 to the fiber structure deposition disk 7 is 13 cm in height, and the horizontal distance is 25 cm. The distance from the fiber structure deposition disk 7 to the ionizer Is 10 cm, the distance from the ionizer to the electrode 4 is 5 cm, the distance from the fiber structure deposition disk 7 to the winding device 11 is 22 cm, the rotational speed of the winding device 11 is 37 rpm, The winding speed of the roller 12 was 0.19 m / min, and the number of twists was 195. The obtained twisted yarn had an average fiber diameter of 4 mm and a fineness of 470 dtex. When the surface of the twisted yarn was measured with a scanning electron microscope (“S-2400” manufactured by Hitachi, Ltd.), the average fiber diameter of the multifilament was 2.3 μm.

[Example 2]
1 part by weight of polylactic acid (manufactured by Shimadzu Corporation: trade name “Lacty 9031”), 3 parts by weight of ethanol (made by Wako Pure Chemical Industries, Ltd., special grade), 6 parts by weight of methylene chloride (made by Wako Pure Chemical Industries, Ltd., special grade) The parts were mixed at room temperature (25 ° C.) to prepare a solution. A twisted yarn was obtained using the apparatus shown in FIG. The inner diameter of the ejection nozzle 1 is 0.8 mm, the voltage is 15 kV, the distance from the ejection nozzle 1 to the fiber structure deposition disk 7 is 13 cm in height, and the horizontal distance is 1 cm, and from the fiber structure deposition disk 7 to the electrode 4 The distance is 7 cm, the distance from the fiber structure depositing disk 7 to the take-up roller 12 is 35 cm, the diameter of the fiber structure depositing board 7 is 14 cm, the rotation speed is 200 rpm, and the take-up roller 12 is wound up. The speed was 0.23 m / min and the number of twists was 870. The obtained twisted yarn had an average fiber diameter of 0.4 mm and a fineness of 420 dtex. When the surface of the twisted yarn was measured with a scanning electron microscope (“S-2400” manufactured by Hitachi, Ltd.), the average fiber diameter of the multifilament was 2.2 μm.

[Example 3]
1 part by weight of polylactic acid (manufactured by Shimadzu Corporation: trade name “Lacty 9031”), 3 parts by weight of ethanol (made by Wako Pure Chemical Industries, Ltd., special grade), 6 parts by weight of methylene chloride (made by Wako Pure Chemical Industries, Ltd., special grade) The parts were mixed at room temperature (25 ° C.) to prepare a solution. A twisted yarn was obtained using the apparatus shown in FIG. The inner diameter of the ejection nozzle 1 is 0.8 mm, the voltage is 15 kV, the distance from the ejection nozzle 1 to the apex of the fiber capturing device 17 is 5 cm in height, and the horizontal distance is 10 cm. From the center of the fiber capturing device 17 to the electrode 4 The distance from the top of the fiber capturing device 17 to the winding roller 12 is 25 cm, the diameter of the fiber capturing device 17 is 10 cm, the height is 22 cm, and the rotation speed is 320 rpm. The winding speed of the roller 12 was 0.43 m / min, and the number of twists was 749. The obtained twisted yarn had an average fiber diameter of 0.4 mm and a fineness of 140 dtex. When the surface of the twisted yarn was measured with a scanning electron microscope (“S-2400” manufactured by Hitachi, Ltd.), the average fiber diameter of the multifilament was 1.2 μm.

[Example 4]
1 part by weight of polylactic acid (manufactured by Shimadzu Corporation: trade name “Lacty 9031”), 3 parts by weight of ethanol (made by Wako Pure Chemical Industries, Ltd., special grade), 6 parts by weight of methylene chloride (made by Wako Pure Chemical Industries, Ltd., special grade) The parts were mixed at room temperature (25 ° C.) to prepare a solution. Using the apparatus shown in FIG. 8, a fiber structure is formed between the ejection nozzle 1 and the discharge needle 14, and a twist is applied by applying compressed air to the formed fiber structure, and the twist is applied. The fiber structure was continuously ejected by compressed air, and the ejected fiber structure was wound up by a winding roller to obtain a twisted yarn. The inner diameter of the ejection nozzle 1 was 0.8 mm, the voltage was 15 kV, and the winding speed of the winding roller 12 was 0.80 m / min. The obtained twisted yarn had an average fiber diameter of 0.3 mm and a fineness of 70 dtex. When the surface of the twisted yarn was measured with a scanning electron microscope (“S-2400” manufactured by Hitachi, Ltd.), the average fiber diameter of the multifilament was 1.1 μm. Further, in the method of this example, the winding number 11, the fiber structure deposit board 7, and the fiber trapping device 17 used in Examples 1 to 3 were not used, so the number of twists could not be calculated.

[Example 5]
1 part by weight of polycaprolactone (manufactured by Daicel Chemical Industries, Ltd .: trade name “PLACCEL H7”), 3.6 parts by weight of ethanol (special grade, manufactured by Wako Pure Chemical Industries, Ltd.), methylene chloride (manufactured by Wako Pure Chemical Industries, Ltd., 5.4 parts by weight of special grade was mixed at room temperature (25 ° C.) to prepare a solution. A twisted yarn was obtained using the apparatus shown in FIGS. The inner diameter of the ejection nozzle 1 is 0.8 mm, the voltage is 15 kV, the distance from the ejection nozzle 1 to the apex of the fiber capturing device 17 is 5 cm in height, and the horizontal distance is 10 cm. From the center of the fiber capturing device 17 to the electrode 4 The distance from the top of the fiber capture device 17 to the take-up roller 12 is 25 cm, the diameter of the fiber capture device 17 is 10 cm, the height is 22 cm, and the rotation speed is 330 rpm. The winding speed of the roller 12 was 0.25 m / min, and the number of twists was 1310. The obtained twisted yarn had an average fiber diameter of 0.5 mm and a fineness of 430 dtex. When the surface of the twisted yarn was measured with a scanning electron microscope (“S-2400” manufactured by Hitachi, Ltd.), the average fiber diameter of the multifilament was 1.0 μm.

[Example 6]
1 part by weight of a polylactic acid-polyglycolic acid copolymer (copolymerization ratio 50/50, manufactured by Birmingham Polymers, Inc .: trade name “lactel”), 2 parts by weight of ethanol (made by Wako Pure Chemical Industries, Ltd., special grade), 7 parts by weight of methylene chloride (made by Wako Pure Chemical Industries, Ltd., special grade) was mixed at room temperature (25 ° C.) to prepare a solution. A twisted yarn was obtained using the apparatus shown in FIG. The inner diameter of the ejection nozzle 1 is 0.8 mm, the voltage is 15 kV, the distance from the ejection nozzle 1 to the apex of the fiber capturing device 17 is 5 cm in height, and the horizontal distance is 10 cm. From the center of the fiber capturing device 17 to the electrode 4 The distance from the top of the fiber capture device 17 to the take-up roller 12 is 25 cm, the diameter of the fiber capture device 17 is 10 cm, the height is 22 cm, and the rotation speed is 330 rpm. The winding speed of the roller 12 was 0.38 m / min, and the number of twists was 878. The obtained twisted yarn had an average fiber diameter of 0.5 mm and a fineness of 450 dtex. When the surface of the twisted yarn was measured with a scanning electron microscope (“S-2400” manufactured by Hitachi, Ltd.), the average fiber diameter of the multifilament was 0.9 μm.

[Example 7]
1 part by weight of a polylactic acid-polycaprolactone copolymer (copolymerization ratio 74/26, Mn = 146000, Mw = 215000), 3.6 parts by weight of ethanol (made by Wako Pure Chemical Industries, Ltd., special grade), methylene chloride (sum A solution was prepared by mixing 5.4 parts by weight of Kojun Pharmaceutical Co., Ltd., special grade) at room temperature (25 ° C.). A twisted yarn was obtained using the apparatus shown in FIG. The inner diameter of the ejection nozzle 1 is 0.8 mm, the voltage is 15 kV, the distance from the ejection nozzle 1 to the apex of the fiber capturing device 17 is 5 cm in height, and the horizontal distance is 10 cm. From the center of the fiber capturing device 17 to the electrode 4 The distance from the top of the fiber capturing device 17 to the winding roller 12 is 25 cm, the diameter of the fiber capturing device 17 is 10 cm, the height is 22 cm, the rotation speed is 300 rpm, and the winding is The winding speed of the roller 12 was 0.25 m / min, and the number of twists was 1200. The obtained twisted yarn had an average fiber diameter of 0.3 mm and a fineness of 400 dtex. When the surface of the twisted yarn was measured with a scanning electron microscope (“S-2400” manufactured by Hitachi, Ltd.), the average fiber diameter of the multifilament was 1.8 μm.

[Example 8]
Cellulose triacetate (Daicel Chemical Industries, Ltd .: trade name “LT-35”) 0.55 parts by weight, ethanol (Wako Pure Chemical Industries, special grade) 1.89 parts by weight, methylene chloride (Wako Pure Chemical Industries, Ltd.) 7.56 parts by weight (manufactured by Co., Ltd.) was mixed at room temperature (25 ° C.) to prepare a solution. A twisted yarn was obtained using the apparatus shown in FIG. The inner diameter of the ejection nozzle 1 is 0.8 mm, the voltage is 15 kV, the distance from the ejection nozzle 1 to the apex of the fiber capturing device 17 is 5 cm in height, and the horizontal distance is 10 cm. From the center of the fiber capturing device 17 to the electrode 4 The distance from the top of the fiber capturing device 17 to the winding roller 12 is 25 cm, the diameter of the fiber capturing device 17 is 10 cm, the height is 22 cm, and the rotation speed is 220 rpm. The winding speed of the roller 12 was 0.25 m / min, and the number of twists was 876. The obtained twisted yarn had an average fiber diameter of 0.3 mm and a fineness of 100 dtex. When the surface of the twisted yarn was measured with a scanning electron microscope (“S-2400” manufactured by Hitachi, Ltd.), the average fiber diameter of the multifilament was 2.0 μm.

[Comparative Example 1]
1 part by weight of polylactic acid (manufactured by Shimadzu Corporation: trade name “Lacty 9031”), 3 parts by weight of ethanol (made by Wako Pure Chemical Industries, Ltd., special grade), 6 parts by weight of methylene chloride (made by Wako Pure Chemical Industries, Ltd., special grade) The parts were mixed at room temperature (25 ° C.) to prepare a solution. When spinning is performed using the apparatus shown in FIGS. 1 and 2 with the power of the ionizer 6 turned off, the fiber structure is not deposited on the fiber structure deposition disk 7 but deposited on the electrode 4. A twisted yarn could not be obtained.

It is the figure which showed typically the manufacturing apparatus for manufacturing the twisted yarn of this invention. It is the figure which showed typically the inside of the winding apparatus 11 in the manufacturing apparatus of FIG. It is the figure which showed typically the manufacturing apparatus for manufacturing the twisted yarn of this invention. It is the photograph figure obtained by image | photographing (2000 times) the surface of the twisted yarn obtained by operation of Example 1 with a scanning electron microscope. It is the photograph figure obtained by image | photographing (2000 times) the surface of the twisted yarn obtained by operation of Example 2 with a scanning electron microscope. It is the figure which showed typically the manufacturing apparatus for manufacturing the twisted yarn of this invention. It is the figure which showed typically a mode that the fiber capture | acquisition apparatus 17 of FIG. 6 was seen from upper part. It is the figure which showed typically the manufacturing apparatus for manufacturing the twisted yarn of this invention. It is the figure which showed typically a mode that the fiber collection container of FIG. 8 was seen from upper part. It is the photograph figure obtained by image | photographing (100 time) the surface of the twisted yarn obtained by operation of Example 3 with a scanning electron microscope. It is the photograph figure obtained by photographing the surface of the twisted yarn obtained by operation of Example 3 with a scanning electron microscope (2000 times). It is the photograph figure obtained by image | photographing (100 time) the surface of the twisted yarn obtained by operation of Example 4 with a scanning electron microscope. It is the photograph figure obtained by photographing the surface of the twisted yarn obtained by operation of Example 4 with a scanning electron microscope (2000 times). It is the photograph figure obtained by image | photographing (100 time) the surface of the twisted yarn obtained by operation of Example 5 with a scanning electron microscope. It is the photograph figure obtained by image | photographing (2000 times) the surface of the twisted yarn obtained by operation of Example 5 with a scanning electron microscope. It is the photograph figure obtained by image | photographing (100 time) the surface of the twisted yarn obtained by operation of Example 6 with a scanning electron microscope. It is the photograph figure obtained by photographing the surface of the twisted yarn obtained by operation of Example 6 with a scanning electron microscope (2000 times). It is the photograph figure obtained by photographing the surface of the twisted yarn obtained by operation of Example 7 with a scanning electron microscope (100 times). It is the photograph figure obtained by photographing the surface of the twisted yarn obtained by operation of Example 7 with a scanning electron microscope (2000 times). It is the photograph figure obtained by image | photographing (100 time) the surface of the twisted yarn obtained by operation of Example 8 with a scanning electron microscope. It is the photograph figure obtained by photographing the surface of the twisted yarn obtained by operation of Example 8 with a scanning electron microscope (2000 times).

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Solution ejection nozzle 2 Solution 3 Solution holding tank 4 Electrode 5 High voltage generator 6 Ionizer 7 Fiber structure deposit board 8 Motor 9 Rotating shaft 10 Transmission 11 Winding device 12 Winding roller 13 Compressed air air supply nozzle 14 Discharge needle 15 Fiber collection container side plate 16 Fiber collection container top plate 17 Fiber capture device

Claims (26)

A step of producing a solution by dissolving a fiber-forming solute in a solvent; a step of applying a high voltage to the solution; a step of ejecting the solution; and a fiber structure by evaporating the solvent from the ejected solution Forming a fiber bundle from one end of the accumulated fiber structure, a step of eliminating the charge of the formed fiber structure by charging air, a step of accumulating the fiber structure by the charge loss, A method for producing a twisted yarn, comprising a step of drawing, a step of twisting the drawn fiber bundle, and a step of winding up the twisted fiber bundle. Fiber-forming solute is an organic polymer, the production method according to claim 1, wherein. The solvent for dissolving the fiber-forming solute is a volatile organic solvent The process according to claim 1, wherein. The manufacturing method of Claim 3 whose volatile organic solvent is an organic solvent containing a halogen element containing compound. The production method according to claim 4 , wherein the halogen element-containing compound contains a halogenated hydrocarbon. The production method according to claim 5 , wherein the halogenated hydrocarbon is dichloromethane. The manufacturing method of Claim 4 whose organic solvent containing a halogen element containing compound is a mixed solvent containing a polar compound. The manufacturing method of Claim 7 whose polar compound is alcohol. The production method according to claim 8 , wherein the alcohol is methanol and / or ethanol. The manufacturing method of Claim 2 whose organic polymer is aliphatic polyester. The production method according to claim 10 , wherein the aliphatic polyester is at least one organic compound selected from the group consisting of polylactic acid, polyglycolic acid, and polylactic acid-polyglycolic acid copolymer. A solution supply device that supplies a solution in which a fiber-forming solute is dissolved to the tip of the nozzle, a fiber structure manufacturing device that produces the fiber structure by ejecting the solution from the nozzle tip , and charging of the fiber structure by a static elimination device A fiber structure deposition apparatus that deposits the fiber structure on a deposition board by causing loss of the fiber structure, and a twisting apparatus that draws a fiber bundle from the fiber structure deposited on the deposition board and twists the fiber bundle, A twisted yarn manufacturing apparatus, comprising: a winding device that winds up the twisted fiber bundle. The fiber structure manufacturing apparatus is an apparatus that forms a fiber structure by applying a high voltage to a solution in which a fiber-forming solute is dissolved and ejecting the solution to a grounded electrode. 12. Twisted yarn manufacturing apparatus of 12 . The winding device is a device that winds the fiber bundle while twisting it by giving the winding roller itself a rotation having an axial direction perpendicular to the rotation axis of the winding roller installed in the winding device. The twisted-yarn manufacturing apparatus of Claim 12 which is. An apparatus for winding a fiber structure depositing device while twisting the fiber bundle by applying a rotation having an axial direction perpendicular to the rotation axis of a winding roller installed in the winding device to the deposition disk itself. The twisted-yarn manufacturing apparatus of Claim 12 which is. The twisted-yarn manufacturing apparatus according to claim 12 , wherein the static eliminator is an ionizer. A solution supply device that supplies a solution in which a fiber-forming solute is dissolved to the tip of the nozzle, a fiber structure manufacturing device that produces the fiber structure by ejecting the solution from the nozzle tip, and a fiber that captures the fiber structure A twisted yarn comprising: a capturing device; a twisting device that draws a fiber bundle from the fiber structure captured by the fiber capturing device; twists the fiber bundle; and a winding device that winds the twisted fiber bundle. In the production apparatus , a twisted yarn production apparatus in which the fiber capture device is a device that captures fibers whose charge of the fiber structure has been lost by an ionizer. The fiber structure manufacturing apparatus is an apparatus that forms a fiber structure by applying a high voltage to a solution in which a fiber-forming solute is dissolved and ejecting the solution to a grounded electrode. 17. The twisted yarn manufacturing apparatus according to 17 . The winding device is a device that winds the fiber bundle while twisting it by giving the winding roller itself a rotation having an axial direction perpendicular to the rotation axis of the winding roller installed in the winding device. The twisted-yarn manufacturing apparatus of Claim 17 which is. A device in which the fiber trapping device winds up while twisting the fiber bundle by giving the fiber trapping device itself a rotation having an axial direction perpendicular to the rotation axis of the winding roller installed in the winding device. The twisted yarn manufacturing apparatus according to claim 17 . A solution supply device for supplying a solution in which a fiber-forming solute is dissolved to the nozzle tip, a fiber structure manufacturing device for producing a fiber structure by ejecting the solution from the nozzle tip, and a funnel-shaped fiber provided with electrodes A collection container, a device for generating a vortex flow of fluid in the collection container and twisting the collected fibers to obtain a fiber bundle, and a fiber having the twist applied from the lower outlet of the fiber collection container A twisted yarn manufacturing apparatus comprising a winding device for winding a bundle. The fiber structure manufacturing apparatus is an apparatus that forms a fiber structure by applying a high voltage to a solution in which a fiber-forming solute is dissolved and ejecting the solution to a grounded electrode. 21. The twisted yarn manufacturing apparatus according to 21 . The twisted yarn manufacturing apparatus according to claim 21 , wherein the fiber collection container is a device that collects fibers whose electrification of the fiber structure has been lost by the static eliminator. The twisted yarn manufacturing apparatus according to claim 23 , wherein a discharge needle connected to the slow current device is provided in the fiber collection container. The twisted yarn manufacturing apparatus according to claim 21 , wherein the static eliminator is an ionizer. The twisted yarn manufacturing apparatus according to claim 21 , wherein the air jetted through the compressed air nozzle is jetted into the collection container to generate a fluid vortex flow.

Images