WO1988002795A1

WO1988002795A1 - High-density polyethylene net-like fiber, nonwoven fabric made of the fiber and production of them

Info

Publication number: WO1988002795A1
Application number: PCT/JP1987/000765
Authority: WO
Inventors: Kohzoh Ito; Ikuo Ueno; Yoshiaki Nakayama; Katsuji Hikasa
Original assignee: Asahi Kasei Kogyo Kabushiki Kaisha
Priority date: 1986-10-13
Filing date: 1987-10-13
Publication date: 1988-04-21
Also published as: EP0285670B1; EP0285670A4; EP0285670A1; DE3751793T2; DE3751793D1

Abstract

A high-density polyethylene three-dimensional net-like fiber (26) obtained by supplying a polymer to a melting zone (compression portion 13, metering portions 14 - 16) while melting the polymer by use of a heated screw extruder, supplying a solvent (CCl3F) to the molten polymer (supply port 18), preparing a polymer solution by mixing and dissolving them under a high pressure and discharging the polymer solution from a nozzle (24) disposed in the melting zone into a low-pressure zone. The fiber (26) is caused to impinge against a skirt portion (33) having a fiber rocking surface (34) and a buffer surface (35) and is expanded and opened to obtain a nonwoven fabric. This nonwoven fabric is excellent in strength, coverability and whiteness.

Description

Description High density polystyrene network woven fabric, nonwoven fabric made of the woven fabric, and method of manufacturing them.

The present invention relates to a novel three-dimensional reticulated fiber, a nonwoven fabric composed of three-dimensional reticulated fibers, and a method for producing the same, which can be used as a special material for various applications. More specifically, the present invention is made from high density polyethylene, has a highly fibrillated three-dimensional network morphology, has extremely high strength and very high thermomechanical properties. A novel three-dimensional network fiber capable of suitably producing a nonwoven fabric having a mature adhesive property, a nonwoven fabric having excellent opacity, excellent covering power and high strength composed of the novel three-dimensional network fiber: The present invention relates to a high-strength nonwoven fabric having an unfused portion, a nonwoven fabric having excellent uniformity, and a novel method for producing the nonwoven fabric having the excellent uniformity.

Since the present application contains a large number of related inventions as described above, for convenience of explanation and easy understanding, the present invention is categorized by assigning the symbols A, and above as described below. In each of the descriptions above, this symbol will be appended to the beginning of the related description.

A New dimensional reticulated fiber.

B_ Melting zone melt polymer-A new three-dimensional netted fiber manufactured by a manufacturing method using the sealing method.

'' Manufactured by a manufacturing method using high pressure differential activation New three-dimensional net-like weave.

Ό_ A new method for producing three-dimensional network fibers using the melting zone melting polymer sealing method.

_Ε A new method for producing three-dimensional reticulated fibers using high pressure differential activation.

_F_ A new high-strength non-woven fabric made of three-dimensional mesh steel.

High-strength non-woven fabric with a new unfused part consisting of a three-dimensional network fabric. /

iL A new uniform non-woven fabric made of three-dimensional braided steel.

I New production method of uniform nonwoven fabric. Background technology.

As a technique for obtaining a three-dimensional network fiber, 'polymer and solvent at high temperature:' high pressure conditions apply to nozzle and heat; 'discharge to low pressure area, flush solvent to make iron fiber The spinning technology is known. This fiber is stretched in the fiber axis direction, as disclosed in, for example, US Pat. No. 3,081,519, and the fibrils are formed into a three-dimensional net-like structure, and are substantially free ends. Is not included in the fibre] It is a steel fiber with a size of 4 or less.

This Amibushi fiber has a characteristic net-like structure and a stable fibril, so it has the characteristic of high whiteness and high covering power by diffusely reflecting light, and it can be used for various purposes. Can be. Non-woven sheets are a particularly important application, and various polymers are used as the polymer used as the mesh steel, but polyolefins, especially high-density polyethylene Much research has been done on the use of carbon fibers for flash spinning.

Next, conventional techniques relating to the reticulated fiber and its production method will be described.

In addition, the principle of flash spinning is that the reticulation is caused by the structural change of the solution accompanying the transition from a high-temperature, high-pressure homogeneous solution to a low-pressure region, and the solidification of the flash and polymer of the solvent. It expresses structural fibers. Therefore, spinning from a homogeneous solution consisting of a polymer and a solvent is indispensable for continuously and stably producing Amibushi textile fabric.

Therefore, the solvent used in the spinning method is capable of dissolving the polymer at high temperatures and high pressures, and those having a comparatively low boiling point having a flash property are selected. Does not have the ability to dissolve lima: dissolving the polymer only at high temperature and high pressure.

As a process for obtaining flash spun fibers, as shown in USP 3,169,899, a polymer is heated in a pressure vessel having a stirrer. The method is known as a batch method. Various spinning processes are disclosed in US Pat. No. 3,227,794 as a method for obtaining textiles. That is, a predetermined amount of the molten polymer and the solvent are introduced into the screw mixer, and then the mixture is melted and spun in a dissolving tank having a stirring mechanism. There is a known method in which the slurry is fed into a melting tank with a baffle, melted and spun, or the slurry is melted and spun with a slurry pump and piping. You. Conventionally known three-dimensional mesh fibers are steel fibers manufactured by such a method.

__________________________________________ Conventionally known production methods when the production method is viewed from another viewpoint, and reticulated fibrils produced by the production method will be described. As an important technology in this furanosh spinning method, a technology of spinning a polymer solution from a one-liquid phase region to a two-liquid citrus region and then spinning the polymer solution is disclosed in Japanese Patent Publication No. 115-3, 227 _: 794. 23 ff, lines 43-49). That is, with this method,

① Make a uniform solution of polymer and binder

② By passing through the 减 -pressure office and moving to the decompression chamber, the pressure drops to change from one liquid phase region to two liquid phase region. ③ A flash spinning method that spins out from the spinning nozzle and solidifies the polymer is there. 'In addition, there have been proposed various types of spinner assemblies composed of a decompression orifice, a decompression chamber, and a spinning nozzle, which are used as a spinning unit for performing this method. Many studies have been made on these flash spinning methods, especially for polyolefin z halogenated hydrocarbons. For example, these methods are disclosed in US Pat. No. 3,227,794. Also, in these polymer / solvent systems, the boundary between one liquid phase and two liquid phases is limited in temperature and pressure, and it is of low temperature melting type and high pressure melting type. It is disclosed in the above-mentioned prior art that the change from one liquid phase to two liquid phases by descent and the necessity of extraction in two liquid phases are required. As described above, conventionally known reticulated fibers are fibers produced by changing a polymer solution into a two-liquid phase region and then spinning.

Next, a description will be given of a conventional technique relating to a three-dimensional net-like nonwoven fabric.

Non-woven fabrics made using a three-dimensional meshed steel fiber formed from a network of fibrils, as disclosed in δF 3,081,519, have been known. .

That is, as disclosed in Japanese Patent Publication No. 36-16460, a nonwoven fabric in which short fibers of the above-mentioned reticulated fiber are made into sheets, or as disclosed in USP 3,169,899. Non-woven fabrics using a melted filament as a sheet are known. In particular, apply the flash-spun textile shown in the latter to a baffle plate, etc., spread the net-like fibre, and deposit it on the non-woven fabric (hereinafter referred to as fiber sheet before mature bonding). Is referred to as a nonwoven web.) Is a preferred method. In other words: Flash spinning uses molten flash yuka. It is known that the spinning speed usually reaches 9,000 to 13,500 m / min at 4,900 m / min or more. It is extremely useful as a method for obtaining a nonwoven sheet with good productivity.

A nonwoven fabric in which the continuous spun net fabric as spun is spread and arranged in a random direction is formed as a nonwoven fabric (hereinafter, the nonwoven fabric obtained by joining the nonwoven fabrics is referred to as a nonwoven fabric). It is heat bonded according to the retention, strength development and other purposes. The mature bonding is performed by bonding with a force renderer, by embossing or by a felt calender. Thus, a nonwoven fabric with a paper-like surface with a flat surface and a nonwoven fabric with an embossed pattern Opacity due to the formation of fine fibrillar braided steel, covering power and degree, surface smoothness, i-fuzziness, or flexibility, and a certain level of It can be used for various purposes by utilizing the target strength. It is also known that the web is joined with an adhesive.

G. Further, as a non-woven fabric made of a mesh fabric, non-woven fabrics having various forms are known. That is, there are known a non-woven cloth which is softly raised, an α-like non-woven cloth, a lightly heat-bonded surface only, and a non-woven cloth which is not completely bonded at all. These nonwoven fabrics are used for various applications by utilizing their high covering power, whiteness, and strength. '

As the polymer used for producing the nonwoven fabric of the mesh fiber, various polymers are used, but a nonwoven fabric made of polyolefin, especially high-density polyethylene made of flash-spun iron fiber is used. Much research has been done to make this suitable.

As disclosed in USP 3, 169, 899, a bundle of mesh-shaped steel wire coming out of a spinning nozzle was used as a device for making a non-woven web from a 1L and steel mesh steel wire. 2. Description of the Related Art There has been known a device in which a silk fiber woven by widening and opening is made by colliding with a tub biasing device, and then deposited on a moving collecting surface to make a nonwoven fabric. -Also ^{: As} disclosed in SP 3, 497, 918, as a device to widen orchid and disperse the net-like weave, the disk part, the cylindrical part installed at the center of the disk, and the side of the cylindrical part From the top of the disk with an inclination A rotating collision plate having a spread polylobal seat is also known.

Furthermore, in order to improve the uniformity of the basis weight of the non-woven web, a technique for imparting electric charge to the fiber by corona discharge before depositing the three-dimensional network on the converging surface of the ura is described in Tokuho Shosho. It is disclosed in JP-A-44-21817. Further, US Pat. No. 3,593,074 and SP3,851,023 disclose methods of controlling a forward path of a collision-opened mesh-like fiber to a surface of a ura.

There are various problems, ie, disadvantages, in the conventionally known methods for producing reticulated fibers and reticulated fibers, nonwoven fabrics made of reticulated iron, and nonwoven fabric production methods described above. The following describes these problems.

It has also been clarified that conventionally known three-dimensional as-spun fibers are still unsatisfactory in performance even when a high-density polyethylene of a suitable material is used. c In other words, in USP 3,081,519, fibers produced by the 7 lash spinning method show molecular orientation even after being spun and have a certain degree of physical properties. The technology discloses that it is necessary to heat stretch this fiber in order to obtain new physical properties, and the technology is disclosed.

However, the spinning speed in flash spinning is extremely high as described above, and the gap between the spinning speed and the drawing speed is too large. It has various problems and is not practical. In particular, in a method in which a flash spun textile is used as a sheet, it is necessary to carry out mature drawing of a three-dimensional network fiber. Is virtually impossible. That is, an operation for giving a difference between the spinning speed and the drawing speed cannot be included in the process. Even if the ripening operation can be used, the ripening can increase the mechanical strength of ripening, but the whiteness and S-force, which are the characteristics of the three-dimensional netted fabric, decrease, and the wrapping becomes transparent. Nature occurs. In addition, there are many problems when the mesh-like steel cannot be spread, the uniform nib does not occur, and the shrinkage at the time of ripe bonding tends to occur. Therefore, in the case of producing a nonwoven fabric made of a three-dimensional reticulated fiber, as-spun fiber is used as shown in USP 3, 69, 899. In other words, a simple process is used in which the flash-spun creatures are spread with a barrier or the like to form a sheet, and then the adhesive is matured. However, it is clear that the physical properties of a nonwoven fabric basically depend on the properties of the fibers that make it up. The physical properties of the non-woven fabric obtained by devising a method of spreading fibers into a sheet or a method of thermally bonding the sheet are considered to be the mechanical, thermal, and optical properties of the constituent steel Sex Depends on S. In other words, the destructive properties of the heat-bonded non-woven fabric depend on the mechanical properties and thermal properties of the fibers to be formed. In addition, the optical properties of the non-woven fabric and the optical properties and thermal properties of the textile It depends on the nature. Therefore, a nonwoven fabric having excellent performance cannot be obtained. Various known methods can be used as a method for heat-bonding a sheet made of textile obtained by flash spinning. High-density polyethylene is bonded at a temperature close to the melting point of the crystal to develop strength and maintain shape as a nonwoven fabric and to prevent surface fuzz. Therefore, when considering a mature bonded nonwoven fabric, the thermal adhesion between fibers is strong. At the same time, it is required for the steel that the shrinkage does not easily occur during thermal bonding and that the mechanical strength of the textile is high at a high temperature near the bonding temperature.

From such a meaning, it is not known that dropping can be performed with a conventionally known three-dimensional mesh fiber as spun. That is, the thermal strength is inferior, the ripened mechanical properties are inferior, the deterioration near the bonding temperature is large, and the core strength (tension, tear, etc.) of the heat-bonded nonwoven fabric is low. Poor, whiteness · Insufficient covering power, spots are noticeable, etc.-And the actual situation is that the use is limited.

Therefore, one of the objects of the present invention is as-spun fabric, which has high mechanical strength and excellent three-dimensional properties near the bonding temperature suitable for forming a heat-bonded nonwoven fabric. The purpose is to provide a mesh fiber.

And — using a well-known manufacturing technique as described above to prepare a homogenous solution of the polymer, and performing flash spinning to form a reticulated fabric; There is a problem. When the known technique is used, it takes a long time to dissolve the polymer in the solvent. The reason for this is that in the autoclave-type stirring tank, the strong shearing force required for dissolution does not work, and the dissolution time is lengthened simply by increasing the residence time. To obtain a uniform polymer solution. Therefore, it is premised to use a large-capacity container, and the residence time is inevitably increased, and since the container has a large capacity, it is extremely difficult for the pressure in the container to exceed 200 ccl · G. In addition, polymer swollen using pie plies is mixed by laminar flow mixing. In the case of dissolution, only the shear force and the flow rate difference required for dissolution require an extremely long pipeline, which results in an increase in residence time. In addition, when turbulent mixing is performed, the polymer solution has a high viscosity of about 30: 100 centimeters, so that extremely high flow is required and a huge pump that is difficult to implement in practice is required. I need.

In any case, the solvent used for flash spinning must dissolve the polymer at normal and normal pressure, and must dissolve the polymer only at high pressure and high temperature. In flash spinning, high temperature and high pressure are indispensable. Therefore, the conventional known technology inevitably increases the Banning time, and conversely, the high pressure is limited. .

If the polymer 1 stays in the system for a long time at high temperature, this immediately leads to the deterioration of the polymer, and it is not possible to obtain good netted steel stably. This difficulty is increasingly compounded as the polymer becomes higher molecular weight, and becomes practically insoluble above a certain molecular weight. On the other hand, when fabricating fiber from flash yarn, it is necessary to use a high molecular weight polymer in consideration of the strength, toughness, and various properties of the product. Furthermore, spinning is performed as a solution in flash spinning: therefore, it is possible to use a high molecular weight polymer which is difficult to spin in ordinary melt spinning. On the other hand, the usefulness of flash spinning can be fully demonstrated only by using high molecular weight polymers that are difficult to melt spin.

—However, with the conventionally known technology, the dissolution of the polymer becomes more difficult as the molecular weight increases, and the usefulness of flash spinning is increased. As a result, it is not possible to continuously obtain the desired properties of the mesh-shaped steel wire stably.

The cause of this situation is thought to be the affinity between the polymer and the solvent. That is, as described in the flash spinning method. SP 3: 22: 794, a high-temperature, high-pressure homogeneous solution was depressurized by a decompression orifice. This is a technology that utilizes the structural change of the solution and the flushing force of the solvent and the solidification of the solvent by ejecting it from the spinning nozzle, and thus the affinity between the polymer and the solvent. Has a very important meaning. From this, the solvent used for flash spinning is selected so as not to dissolve the polymer at normal temperature and normal pressure and to form a uniform solution with the polymer at high temperature and high pressure. Therefore, the polymer solvents used for flash spinning do not dissolve each other unless the temperature and pressure are high, and the dissolving power decreases as the degree of polymerization of the polymer increases. Is also clear.

In order to continuously obtain the desired properties and form of reticulated fiber, it is essential that the spinning conditions be optimized and that a uniform solution of polymer / solvent be supplied. In particular, when a high molecular weight polymer is used, a technology different from the conventional technology is expected.

Another major problem of the prior art is the mixing ♦ dissolution tank and O stirring shaft. That is, according to the prior art, a uniform polymer solution is obtained by a stirring tank driven by an external driving source, or a long time is required by using a long pipe line. To obtain the desired polymer solution. For the latter, there is no forced mixing, so it is of practical value A substantially uniform solution of the polymer having a molecular weight as high as L2 cannot be obtained.

Therefore, the former method using a stirring shaft is more practical, but since this method also includes a sliding part in the device used, it cannot be made to have a certain high pressure or more, and it is special and expensive. There is a problem such as the necessity of a sealing device for a suitable sliding part.

The polymer solvent system that performs flash spinning forms a solution at high temperature and pressure, and in order to impeach the affinity between the polymer and the solvent, the higher the pressure, the higher the dissolution speed even at the same temperature. A uniform polymer solution can be obtained smoothly. -This is the same for the molecular weight of the polymer, which results in a high molecular weight and its dissolution requires high pressure. However, if the conventional method is used, it is not possible to obtain a high pressure enough to dissolve the high molecular weight polymer due to the problem of the sealing mechanism of the sliding part. Spinning the quantity polymer was virtually impossible.

As described above, there is a strong demand for a spinning method suitable for a high-pressure process from the viewpoint of preventing polymer deterioration and the use of a high molecular weight polymer.

As an important technique in the flash spinning method, USP3, 227, 794, which spins a polymer solution after changing the polymer solution from a liquid confinement region to a two liquid phase region (No. 23-43-49) According to the known technique of (1), if the polymer and the solvent are determined, there is an upper limit to the pressure in the vacuum chamber according to the temperature of the spinning liquid, that is, the flushing is performed on the low pressure side below the phase separation line. There is a problem in that spinning must be performed, which limits the use of the solvent, Yushuka. -This will be explained with reference to Fig. 1. This figure is an example showing the phase diagram of the high-density polyethylene chlorotrichloromethane phase. Line EF is the phase separation line (phase equilibrium line), from which it shows that the upper part is one liquid phase and the lower part is two liquid phases. In FIG. 5, changing from one liquid phase region to two liquid phase region in the prior art means transition from the state of point C to the state of point D. That is, the pressure in the decompression chamber immediately before the discharge is limited.

In the case of French spinning, a high speed can be obtained by flushing the agent, so that no drawing or drawing force is required and ordinary melt spinning or dry spinning is required. Unlike this, fiber formation, stretching and orientation are performed only by the energy of the solution.

'Especially, the stretching and orientation of the textile is performed by the solvent, fluff, so that the higher the pressure, the higher the flash force.

1 5 Weave of performance. Therefore, in order to obtain highly oriented, high-strength fibers, the conditions of the decompression chamber immediately before the formation of the spun / textile are extremely important.

According to the above-mentioned known technology, there is an upper limit corresponding to each temperature in the pressure taken in the decompression chamber. Therefore, try increasing the solution temperature.

However, an increase in temperature causes the polymer Z solvent system to degrade rapidly. This thermal decomposition is due to the interaction of the polymer solvent, which releases halogen ions in the solvent, degrades by hydrogen abstraction in the polymer, and accelerates the rapid decomposition in the presence of each other. Is done. These thermal decompositions become more severe at higher temperatures. 5 Also, depending on the temperature to be adopted and the residence time of melting and spinning, etc. Stabilizers are used, and although they provide some effect, it is difficult to prevent substantial degradation. Therefore, for example, in the case of high-density polyethylene Z trichlorofluorometan (hereinafter abbreviated as fluoro-11), O-spinning is difficult at temperatures exceeding L9 Q ° c. is there.

As described above, the use of the flash yuka is restricted in the conventional technology, and further improvement is expected particularly in view of the strength of the mesh fabric.

Accordingly, the present invention provides a method for activating a solution in a flash spinning method using industrially useful high-density polyethylene 'and fluoro--11 to remove the solvent flusher. The aim of this paper is to make further use of a fully stretched and oriented higher-strength, high-density polyethylene reticulated fiber, and a new method for obtaining the reticulated fiber. One. ;

F_ Non-woven fabrics using a flash-spun woven fiber having a three-dimensional network structure are used for various applications by utilizing the unique properties of the woven fiber fabric. Then, the nonwoven fabric of the aforementioned US _P3:.. 169, as disclosed in 899 report, the Tetsu維spun used - i.e., spread was Furatsushu spun O維with baffle扳like sheet — A simple process of heat bonding is adopted.

Further, a paper-like nonwoven fabric having a certain degree of opacity and covering power and mechanical strength of a three-dimensional meshed steel is disclosed in US Pat. No. 3,532,589. In other words, this nonwoven fabric has a specific surface of 0.5 to 5.0 m / g in each of the layers arranged in the thickness direction of the sheet. It has a non-woven fabric structure composed of a three-dimensional net-like fiber having a specific surface area that is at least 0.3 m ² ng higher than that of any of the outer layers.

However, according to the meter of the present inventors, it has become clear that even with such a structure, the performance of the O-woven fabric is not satisfactory. Also, no conventional nonwoven fabric has been obtained, which satisfies both mechanical strength and covering power. That is, they were extremely dissatisfied with the opacity, covering power, tensile strength and tear strength, which are the physical properties expected of a three-dimensional reticulated fiber nonwoven fabric.

As is well known, in a nonwoven fabric, when heat bonding is performed on the same non-bonded fibrous sheet, the tensile strength and the tear strength of the obtained nonwoven fabric are substantially inversely correlated. Then, there is a problem that in order to increase the strength of one of these two strengths, the strength of the other must be sacrificed. In general, a non-bonded fiber sheet has a large tear strength, but a low tensile strength, and has no fuzz on the surface. This is thermally bonded-this can increase the tensile strength and improve the surface fluff, but the tear strength decreases. This tendency becomes stronger as the degree of mature bonding increases.

On the other hand, in a nonwoven fabric made of a net-like fabric, there are many uses that make use of the high covering power inherent in the fabric, and opacity is also an important physical property. As described above, for example, increasing the degree of thermal bonding with the aim of increasing the tensile strength impairs this opacity. And a very strong, mature bond is a transparent filter. It will be nolem-like.

Therefore, there is a demand for a mesh-like steel nonwoven fabric having a preferable relationship between tensile strength and tear strength and having excellent opacity. Particularly, the tensile strength and crack strength in a region with a large adhesion of 60 gZ <f or less are desired. strength δ is high, has been eagerly awaited is excellent nonwoven fabric opacity, hiding power, the present invention is one object that you provide such nonwoven _c

^ Non-woven sheets of three-dimensional silky fiber are subjected to various types of heat bonding for the purpose of maintaining shape, developing strength, and reducing surface fuzz. Normally, these sheets have a multi-layer structure in which three-dimensional mesh fibers are spread and deposited, and each layer in the cross-sectional direction of the sheet can provide a bonding state between different fibers. .

"The object of the present invention is to form a non-woven fabric as one of the non-woven fabrics. A non-woven fabric having at least a part of the non-woven fabric having at least a part of a loose layer with a low degree of adhesion is formed. That is, the surface of the nonwoven fabric, or the inner layer when the nonwoven fabric is exfoliated in layers, includes a partially non-fused nonwoven fabric having an independent reticulated 'state' of iron. Such a nonwoven fabric is a nonwoven fabric that is excellent in bulkiness, flexibility, covering power, and has high tear strength.

Example, in such a nonwoven fabric, a sheet-like material of a three-dimensional network woven 'Wei high density polyethylene Wechiren, partially thermally adhered Ty _{V e} k ® 14 type (E. I. Du pon t Is known. This nonwoven fabric consists of a surface layer that is relatively firmly heat bonded and an inner layer that is relatively loosely bonded, and that is partially pressed. It has a pattern. When the non-woven fabric is separated as a layer, it is possible to obtain an independent continuous net of 20 ™ or more from the inner layer which is relatively slowly bonded by heat.

However, such conventionally known nonwoven fabrics have various problems in performance. That is, they are extremely dissatisfied with the most basic physical properties of the three-dimensional network fiber fabric, that is, opacity, covering power, tensile strength, and tear strength.

Even with the use of known techniques for the production of nonwoven fabrics composed of reticulated fibers, it was not possible to obtain nonwoven fabrics with satisfactory uniformity. These nonwoven fabrics have large irregularities in the opening width of the opened three-dimensional mesh fibers constituting the nonwoven fabric, and contain many bundled bundles having an extremely large fiber density. For this reason, the nonwoven fabric has a non-uniform appearance in which a portion having a high fiber density and a portion having a low fiber density are mixed, and the nonwoven fabric has _one large spot.

Such nonwoven fabrics are unsuitable for use in filter fields and sanitary materials where uniformity of the nonwoven fabric is required. Pinholes were formed in small areas, and it was not possible to use them in fields requiring shielding properties such as liquids and batteries.

In addition, its use as a nonwoven fabric is extremely limited due to its uneven appearance and unevenness of the surface.

Therefore, while there is a need to improve the uniformity of non-woven fabrics made of flash-spun three-dimensional reticulated fibers, what can be achieved at present and how to achieve them have emerged. And Absent. —

An object of the present invention is to provide a uniformly spun flash-spun nonwoven fabric and a method for producing the same, which can be sufficiently used in the field of filters, sanitary materials and the like. Orchid of invention

An object of the present invention is to provide a novel tertiary fiber of high-density polyethylene, which is useful, a variety of nonwoven fabrics made of the fiber, and a method for producing the same. In addition, a three-dimensional morphology with extremely high maturation characteristics and extremely high strength (J,

Secondly, in the flash spinning method, a steel extruder (J_) manufactured using a screw extruder, which is manufactured by a manufacturing method in which the inlet of the ^ immersion region is sealed with a molten boiler,

Third, in the flash spinning method, a high pressure difference is generated,

Bollima—a textile manufactured by a liquid-activating manufacturing method,

Fourth, in the flash spinning method, the above-mentioned textile manufacturing method (D_) in which the entrance of the polymer dissolving area is sealed with a molten polymer using a screw extruder,

Fifth, in flash spinning, a high pressure difference is generated to activate the polymer liquid, and the above-mentioned () method for producing steel (),

First, the non-woven fabric (F), which has a high specific surface area and high mechanical strength of the inner layer produced from the fibers of the above (), Seventh, non-woven fabric (_G), which is manufactured from the fiber of (A) above and has excellent covering power and strength, from which independent m-fiber can be taken out,

Eighth, the nonwoven fabric (1L) consisting of the fibers described in (A) above,

Ninth, the object of the present invention is to provide a manufacturing method (! _) For manufacturing the non-woven fabric having high uniformity (-H-) using a dispersing device having a special structure and a dispersing condition. .

A first object of the present invention is to provide a fibrillated, high-density, polystyrene-based three-dimensional reticulated fiber characterized by having a long-period scattering intensity ratio of 40 or less. Is achieved.

A second object of the present invention is to continuously supply the polymer to the polymer dissolving zone while melting it by using a heated screw extruder, and to continuously enter the dissolving zone into the inlet. A solvent is added to the molten polymer while closing with the molten polymer supplied to the furnace, and the two are mixed and dissolved under high pressure to produce a polymer solution, which is used for the melting zone. Three-dimensional network of fibrillated high-density polyethylene obtained by the method of manufacturing a mesh-like fiber by the flash spinning method, in which a polymer solution is continuously discharged from a wool into a low-pressure region. Achieved by weaving.

A third object of the present invention is to provide a high-pressure homogeneous solution comprising a high-density polyethylene-based polymer and trichlorofluoromethane from a reduced-pressure orifice, a reduced-pressure chamber and a spinning nozzle. In the method of obtaining a net-like debris of a high-density polyethylene polymer by using a spinning device made of Achieved by a fibrillated, high-density polyethylene-based three-dimensional mesh fiber obtained by a method of manufacturing a mesh fiber by a flash spinning method that activates and activates a liquid. Is done.

In the fourth method of the present invention for producing a net-like textile by a flash spinning method, a matured screw extruder is used; A solvent is added to the molten polymer while the inlet of the melting area is closed with the molten polymer supplied continuously, and the two are mixed and dissolved under high pressure to produce a polymer solution. And a method for continuously producing high-density polyethylene-based three-dimensional reticulated fibers characterized by discharging the polymer solution from the nozzle used for the dissolution zone to the low-pressure zone in a continuous manner. Achieved. The fifth aspect of the present invention is that a high-pressure homogeneous solution comprising a high-density polyethylene-based polymer and trichlorofluoromethane is applied to a reduced-pressure orifice, a reduced-pressure chamber, and a spinning nozzle. In a method of obtaining a high-density polyethylene-based polymer network web by discharging a spinning device consisting of a spinning device comprising a high-pressure polyethylene, a high-pressure difference is generated before and after the high-pressure orifice. This is achieved by a method for producing a high-density polyethylene-based three-dimensional network fiber, which is characterized by activating a liquid.

According to a sixth aspect of the present invention, a high-density polyethylene-based fibrous continuous three-dimensional network fiber is deposited in a random direction and strongly heat-bonded to each other. An integrated nonwoven fabric comprising a surface layer and an inner layer that is weaker than the surface layer and is thermally bonded to the film-like textile layer, characterized in that the specific surface area of the inner layer exceeds 5 nf / g. High tear strength three-dimensional nonwoven fabric Achieved by cloth.

A seventh object of the present invention is to provide a high-density polyethylenic fibrillated three-dimensional network fiber which is arranged in a random direction, deposited in layers, and partially unfused. In nonwoven fabrics containing a layer of fibrous fibers in an independent mesh form, the

This is achieved by a nonwoven fabric made of a three-dimensional net-like fabric, which has a long-period scattering intensity ratio of 40 or less.

An eighth object of the present invention is to provide a nonwoven fabric in which an opened high-density polyethylene-based three-dimensional reticulated iron is deposited in a random direction, a bundle portion present in continuous reticulated fibers constituting the nonwoven fabric. Is 4 Q Deni

-If the bundle has a density of less than 100 mm / MI width or a bundle with a density of 40 denier Z mm or more, the width is 5 mm or less; F and length are 3 Achieved by a uniform non-woven fabric that is characterized by the following bundle.

A ninth object of the present invention is to provide a rotatable disk portion, a cylindrical portion extending vertically from the center of the disk portion and having a circular outer surface with a smaller diameter than the disk portion, and one surface of the disk portion And a skirt portion that is inclined and disposed in a space between the cylindrical portion and the circular eclectic surface of the cylindrical portion. The skirt portion comes into the skirt portion in a direction substantially parallel to the axis of the cylindrical portion. A plurality of oscillating surfaces for oscillating the unopened three-dimensional net-like fiber, and the oscillating direction of the three-dimensional net fibers which are alternately arranged with the oscillating surface and are oscillated by the oscillating surface. Of a three-dimensional mesh fabric composed of a cushioning surface that mitigates a rapid change in the size of the fabric. The center of the oscillating surface and the upper surface of the disk The angle of inclination formed is almost equal to the angle of inclination between the center of the airplane and the upper surface of the disk, and the cushioning surface has a fan-shaped shape whose width near the disk is wider than that near the cylinder. Achieved by a method for producing a uniform nonwoven fabric, which employs the use of a three-dimensional mesh fiber dispersion-rotational dispersion. BRIEF DESCRIPTION OF THE FIGURES

FIG. 1 is a view showing the principle for producing a high-performance, high-density polyethylene three-dimensional network key of the present invention. In the production method of the present invention, a polymer liquid is activated by a high force difference. This is a draft explaining the spinning method and the relationship between pressure and temperature in the conventional spinning method.

FIG. 2 is a diagram showing a small-angle X-ray scattering image of the reticulated fiber of the present invention.

FIG. 3 is a drawing for explaining a method for obtaining a long-period scattering intensity ratio in small-angle X-ray scattering PSPC. .

Figure 4 is a high density polyethylene ethylene (MI = 1. 2, weight average molecular weight of about 14 X 10 ^4, manufactured by Asahi Kasei Corporation Sante' click B - 161) and Application Benefits click throat Furuorome port Li Ma first solution consisting of data down FIG.

The fifth surface is a schematic flow sheet showing one embodiment of the method for producing a reticulated fiber of the present invention.

Fig. 6, Fig. 7 and Fig. 8 are schematic diagrams showing an example of the press, screw and special mixing structure (Dalmage-type, pin-type) used in this kikin. is there.

9 and 10 show other examples of the method for producing the reticulated fiber of the present invention. It is a schematic flow chart showing the implementation of Kiyoshi.

FIG. 11 is a flow sheet showing one embodiment of a method for producing a mesh fiber using a conventionally known screw mixer for comparison with the present invention.

FIG. 12 is a diagram showing the relationship between the tensile and tear strength of the nonwoven fabric of the present invention.

FIG. 13 is a schematic perspective view showing an example of a suitable shape of a rotational dispersion plate for producing the nonwoven fabric of the present invention. '' Fig. 14 is a diagram showing details of the rotational dispersion shape of Fig. 13; Fig. 14 (a) is a plan view, and Fig. 14 (b) is a line in Fig. 14). It is sectional drawing by A-A '.

FIG. 15 is a schematic front view for explaining the action of the rotary dispersion plate according to the present invention on a textile.

Fig. 16 (a) to Fig. 16 (d) show the three-dimensional case where the rotation dispersion plate according to the present invention is installed at a distance where the fluctuation change point of the three-dimensional network fiber is on the collection surface. FIG. 3 is a schematic view of a high-speed photographing apparatus for explaining the action on a reticulated fiber in detail in order of $ 0.

FIG. 17) to FIG. 17 (d) show three-dimensional images obtained when the rotational dispersion according to the present invention is installed at a distance where the swing change point of the three-dimensional mesh fabric is higher than the collecting surface. It is a high-speed imaging device observation schematic diagram explaining the effect | action on a reticulated fiber in detail.

FIG. 18 (a) to FIG. 18 (d) are schematic views of observations of a high-speed photographing device for sequentially explaining in detail the action of a conventionally known rotary dispersion plate on a textile.

FIG. 19 is a micrograph showing a cross section of the nonwoven fabric. FIG. 19 (a) shows a nonwoven fabric according to the present invention, and FIG. 19 (b) shows a cross section of a nonwoven fabric of a comparative example.

Fig. 20 is a photograph showing the surface condition of the nonwoven fabric. Fig. 20 (a) shows the nonwoven fabric according to the present invention, Fig. 20 (b) Fig. Shown respectively. BEST MODE FOR CARRYING OUT THE INVENTION

In order to facilitate the understanding of the present invention, reference is made to the accompanying drawings, which are useful for explaining a reticulated fiber according to the present invention, a method for producing the same, a nonwoven fabric made from the reticulated fiber, and a method for producing the nonwoven fabric. The present invention will be described in detail.

As described above, the textile of the present invention is a textile formed from a high-density polyethylene-based polymer. And, it is a connected three-dimensional net-like fiber made up of many fine fibrils and having substantially no free ends.

As is known, such three-dimensional network fibers are obtained from flash spinning. However, the three-dimensional reticulated fiber of the present invention is a novel three-dimensional silk-shaped fiber that is completely different from conventionally known fibers in the mosaic structure of the fiber and in the fibrous form. It is. Therefore, it has excellent mechanical strength and high-temperature properties, and is particularly suitable for producing a heat-bonded nonwoven fabric.

The fiber of the present invention has a special feature in long-period feeding in the direction of the fiber axis on a fine-grained structure. And this can be clearly understood by measuring small-angle X-ray scattering.

FIG. 2 schematically shows a small-angle scattering photograph of the textile of the present invention. On the equator near the direct beam 1, a scattered image 2 showing the presence of fibrils and voids is shown, and a laminar scattered image 3 is shown on the meridian. Generally, as a long-period small-angle X-ray scattering image of a polymer substance, circular scattering, layered linear scattering, layered two-point scattering, layered four-point scattering, and the like are known. It can be seen that the fibers resemble the long-period structure of the drawn and drawn yarns that are subjected to ordinary spinning and drawing.

Then, according to the analysis of the scattering peaks in the meridional position-sensitive proportional counter (PSPC) at the time of Kiyoshidori, the reticulated fiber of the present invention has a long period of 150 to 200 A. And, they have found an unexpected feature of the present invention that the scattering intensity due to the long period of the Amibushi fiber is not large. That is, from the viewpoint of the long-period scattering intensity, a small scattering intensity means that the long-period structure is not uniform. Or, it was thought that it was not clear, and it was expected that the iron and steel structure would be unfavorable in terms of mechanical properties and mature characteristics. However, the three-dimensional reticulated fiber excellent in these physical properties shown in the present invention does not unexpectedly have a high scattering intensity and provides a fiber having a novel structure. And, because of this structure, it excels in high-temperature characteristics near the melting point, and becomes a three-dimensional network fiber suitable for a heat-bonded nonwoven fabric.

In the present invention, in order to understand the characteristics of the reticulated fiber, the long period and the scattering intensity ratio are quantified. Then, these are explained.

Figure 3 shows the measured scattering intensity vs. angle plot by the PSPC in the meridian direction. The position showing the maximum scattering intensity at the peak of the scattering intensity curve or the shoulder is defined as the long-period scattering angle (2). Let this value be M. Draw a common tangent P to the inflections at both ends of the long-period scattering peak or shoulder in FIG. The measured scattering intensity value of the angle ί is G, and the value on the line Η is Η. One angle

(25) · The measured scattering intensity (blank) value of 2.5 ° is defined as I, and the scattering intensity ratio R is determined as R = (G-Η) Ζ I.

λ

-For long period, insert 2 Θ = M into Bragg's equation L =

2 s I η σ

Required by

The three-dimensional reticulated fiber of the present invention has a long-period of L50 to 200 A and a long-period scattering intensity ratio of 40 or less.

The X-ray 'small-angle scattering described above was measured using the following apparatus and method. X-ray diffractometer RU-200-PL.X manufactured by Rigaku Denki Co., Ltd. ■ X-rays were Cu—K with 1.54 persons and 1st SLIT 0.5 mm φ2nd SLIT 0.3 dragon was used as the pinhole slit. The measurement voltage was 45 kV, the current was UOmA, and the irradiation time was 2 x 10 ³ sec. The sample for the measurement was made such that the sample width of the irradiated part was about 2.5 by aligning the mesh fibers.

The mature nature of this fiber can be determined by various methods of measurement. Then, this thermophysical measurement is performed without feeling, assuming use as nonwoven fabric.

The reticulated fiber of the present invention is characterized by excellent ripening mechanical properties near a ripening bonding temperature and a low elongation rate upon heating. In other words, in the test of a thermomechanical test machine (TMA), the temperature of 130 at the time of heating under a constant load of 1/10 of denier is preferable. 3% or less, more preferably 2% or less. The measurement was performed at a rate of temperature increase of 2 ° C using “T-3000” manufactured by Vacuum Riko Co., Ltd.

In addition, thermal and dynamic properties can be determined by measuring with a piperon. That is, the reticulated fiber of the present invention shows a high dynamic elastic modulus even at a high temperature. For example, the temperature at which the dynamic elastic modulus becomes 101 ^Q dyn / afl is preferably 115 ° C or more.

In addition, the stability of the crystal at high temperatures is evaluated at the onset temperature of the crystal dispersion of tan5. Further, the fiber of the present invention exhibits a high starting temperature of the stuffing crystal dispersion, preferably 123 ° C. or more, and more preferably 125 or more, and shows that the crystal stability near the bonding temperature is high. You can see that she is overkill in sex. These measurements were carried out using an active viscoelasticity measuring device.

Using “RHE0VIB O 'DDV-Π — ΕΑ”, frequency 110 Hz, heating i. I went for C minutes.

As described above, the three-dimensional reticulated fiber of the present invention is excellent in ripening stability at high temperatures and ripening mechanical properties, and is suitable for a ripened nonwoven fabric. Caused by the structure.

The reticulated fiber of the present invention is also a highly oriented fiber, which becomes clear by measuring the crystal orientation angle by X-ray diffraction. That is, the orientation angle of the textile of the present invention by X-rays is 30. The following are preferred: 20 is more preferable. It is as follows. It is also known that the orientation of the crystalline part and the amorphous part of the polymer can be measured from the infrared absorption dichroism, and is evaluated by the dichroic ratio orientation coefficient F °. '' A parallel dichroic band for polystyrene, 2017 cm— ¹ The dichroic ratio orientation coefficient of the textile of the present invention is preferably 0.3 or more. In the present invention, the measurement was performed by using a JIR-100 JFT-100 IS FT-IS apparatus manufactured by JEOL Ltd. and using KRS-5 as an ATR crystal.

Furthermore, birefringence measurement of fibers using microwaves can also be used as a measure of the degree of molecular orientation. The birefringence of the present invention is preferably 0.13 or more in the birefringence of 4 GHz using the Micron π-wave molecular orientation meter j M0A-2001.4 manufactured by Shinwa Paper Co., Ltd. You.

Thus, the three-dimensional network fiber of the present invention is a highly oriented fiber and has extremely good properties.

The three-dimensional network fiber of the present invention has extremely excellent mechanical strength. In the case of a three-dimensional net-like fiber, the fiber is branched into a net, and when measuring the high elongation of the yarn as it is, a slip-through or the like occurs between the fiber elements, resulting in a large variation in the value. Therefore, in the present invention, in the tensile test, the measurement was performed by burning four times in cm. The steel $ ί of the present invention measured under such conditions has an initial modulus of 15 to 50 g Zd, preferably 20 to 50 g Zd, and a breaking strength of 4 g / d or more. Or more than 7 g / d.

As for the three-dimensional reticulated fiber as-spun, a high-strength fiber as shown in the present invention is not known.

The three-dimensional mesh steel of the present invention is preferably made of extremely fine fibrils in the form of fibrillation. It is preferable that the specific surface area of the three-dimensional network fiber is 30 irf / g or more. The use of the specific surface area as a scale for expressing the fineness of the fibrils constituting a three-dimensional network fiber is publicly known as disclosed in USP 3: 169,899. It is. The three-dimensional network fiber of the present invention is composed of a fiber which is clearly evident as compared with a known fiber. The specific surface area of the mesh镞維of the present invention is 3 0 rrf / _g on than is rather preferred, is rather to favored by al 3 5 rrf Roh g or more,

It is also possible to obtain reticulated fibers having a value of 100 m / g or more.

Two

As described above, since the mesh fiber is composed of 9 finer fibers, the reticulated fiber of the present invention is less than the conventionally known fibers in terms of whiteness, covering power, and adsorption performance. I'm stray. When non-woven fabrics using these fibers are manufactured, the fine fibrils can spread the fibers easily and form a uniform sheet. It has many excellent properties such as large surface area, good ripe adhesion, high whiteness and high opacity, and excellent adsorption and filtration performance.

The specific surface area was determined by a nitrogen adsorption method, and in the present invention, the specific surface area was measured using “Soft Tomato 180” manufactured by Carlo Elba.

As a method for measuring the fineness of the fiber, a pore-sigma meter for measuring pore distribution by a mercury intrusion method into fiber may be used. In this case, the fiber of the present invention may be used. It can be seen that the amount of mercury intrusion is larger than that of conventionally known textiles, and that it is composed of fine fibrils.

As described above, the three-dimensional reticulated fiber of the present invention has a unique long-period fiber, despite being composed of extremely fine fibrils. It has structure. It has excellent properties at high temperatures close to the melting point, and also has useful properties such as higher mechanical strength than ever before. In general, in textiles, an increase in the specific surface area of the fiber indicates an increase in the cross-sectional irregularity, and the mechanical strength decreases. However, in the three-dimensional silk-like textile according to the present invention, the increase in the specific surface area and the increase in the mechanical strength are simultaneously performed, which cannot be achieved from the conventional concept.

The textile of the present invention is a three-dimensional netted iron fiber and is obtained by a spinning method known as franosch yarn. Hereinafter, preferred examples for obtaining the three-dimensional silk-like fiber of the present invention will be described.

The three-dimensional reticulated fiber of the present invention can be obtained from fluffy yarn using a polymer and a solvent. However, the flash spinning mechanism for obtaining the woven fabric i of the present invention is conventionally known, and is completely different from that.

As an important technology of flash spinning for obtaining a conventionally known three-dimensional netted iron fiber, US Pat. No. 3,227,794 discloses that a polymer solution is subjected to a pressure drop at a pressure of a pressure. Thus, there is disclosed a technique in which a liquid phase is changed from a single liquid phase to a two liquid phase region and then discharged from a spinning nozzle.

The present inventors have determined that the fiber structure of the flash-spun textile fiber is determined by the fact that the polymer and the solvent have a citrus separation structure. The discovery of the spinning mechanism has led to the completion of the novel three-dimensional network shown in the present invention. The new flash spinning mechanism provides instantaneous activation of a homogeneous solution of the polymer, and is a two-step process from the previously known one-liquid phase. After forming an activation structure different from the phase separation structure due to the change to the liquid phase, spinning nozzles are spun out to form a knowledge structure based on the activation structure. "Activation" as used herein refers to increasing the pressure loss of the polymer-liquid through the decompression orifice, ie, before and after the decompression orifice. To increase the pressure difference by at least 80 kg, more preferably

Activation is performed by setting the pressure difference to more than 120 kg /. This activation is caused by large fluctuations in the density and concentration of the polymer solution, and temporarily gives the solution a structure as if it were extremely difficult to separate.

Then, by discharging from the spinning nozzle in this state, the three-dimensional network fiber of the present invention is obtained. In other words, the solvent that has been released to the low-pressure region rapidly evaporates from this condensed activation structure, and the flashing force that expands causes the polymer to begin to solidify, causing the polymer to start to solidify. To form a highly oriented three-dimensional mesh fabric.

This activation is instantaneous, and a spinning from within one liquid phase region of a phase diagram measured in a static equilibrium state can obtain a preferable three-dimensional network fiber. Therefore, unlike the conventionally known fibers, the fibers obtained from this activated structure are made of extremely fine fibrils having a specific surface area of 30 of / g or more, and are unique to the present invention. This is a high-strength three-dimensional network fiber with a long-period structure. The activation of a solution composed of this polymer and a solvent causes the polymer to have a high degree of polymerization and a narrow molecular weight distribution. difference It has been clarified in the study of the present inventors that increasing the value effectively works. . - O維of this investigation can be a density 0.94 above dense Helsingborg Wechiren not particularly limited _a predominantly high density polyethylene ethylene used which is made from high-density board ethylene interconnection. In addition to a polymer composed of 100% ethylene units, a polymer obtained by randomly or block copolymerizing monomer components other than polyethylene in 10 mol% K may be used. (Of course, the polymer may optionally contain additives, and ripening stabilizers, ultraviolet stabilizers, lubricants, pigments, and the like may be contained in amounts not to impair the present invention.) Naturally, it is also possible to blend this high-density polyethylene with another polymer, and it can be used in a huge manner. In particular, the three-dimensional mesh fabric of the invention of the present invention has a high strength due to its special structure, and the conventional high-density polyethylene cannot be put into practical use due to a decrease in strength by blending with a polymer. It is also possible to blend different types of polymers. Polymers blended with high-density polyethylene include low-density polyethylene, ethylene copolymers, vinyl copolymers, ionomers, polypropylene, polystyrene, and polymethylene. Tactylate and the like.

As mentioned earlier, the textile of the present invention is based on a new mechanism for forming a fiber, and the high-density polyethylene constituting the net-like steel of the present invention preferably has a high degree of polymerization. The melt index (MI) I1 of the fiber to be spun is preferably 1 or less. More preferably, it is 0.5 or less (MI measurement is based on iSTM D-1238-5TT condition E). Also, the molecular weight of the polymer that composes the textile It is also important that the distribution is narrow. That is, even with similar MI, if the molecular weight distribution is wide, the performance tends to be inferior. The molecular weight distribution of the protein of the present invention is 15 or less in _Mw / n, and more preferably 10 or less. Naturally, the MI of the raw material polymer used for obtaining the fiber of the present invention is equal to or less than the MI of the fiber of the present invention.

The lysis process for obtaining the IS fiber of the present invention is not particularly limited, and a conventionally known lysis process can be used. However, it is preferable to use a method in which the polymer is fed while being melted by a screw extruder, and then mixed and dissolved with a solvent in a mixing tube. The textile of the present invention is made of high-density polyethylene having a high molecular weight and a narrow molecular weight distribution, and the raw material polymer is dissolved in a solvent in a short time, spun, and the polymer is dissolved. It is preferable to prevent any deterioration. Further, dissolution at a high pressure is preferable from the viewpoint of the dissolution rate and the spinning mechanism of the present invention.

The solvent used for obtaining the fiber of the present invention is not particularly limited as long as it can be used for fiber spinning, and a conventionally known solvent may be used. Preferably, it is Fluorone-1i, such as methylene chloride, tricyclo mouth trifluorene, etc., or hydrogenated hydrocarbons, cyclohexane, etc. A hydrocarbon or a mixture thereof is used.

The spinning assembly for obtaining the fiber of the present invention is not limited as long as it can take the above-described spinning mechanism. That is, the orifice for decompression, the decompression chamber, and the nozzle for activating the homogeneous solution may have any conventionally known shape. Next, a method for producing the three-dimensional silk-like iron fiber of the present invention will be described.

First, a production method using the melting method melting polymer-sealing method belonging to the above classification will be described.

As described above, the production method of the present invention, which belongs to Class II, melts using a heated screw extruder and supplies the polymer intermittently to the polymer dissolution area while melting the polymer. A solvent is added to the molten polymer while sealing the inlet of the melting zone with the continuously supplied molten polymer, and the two are mixed and dissolved under high pressure to produce a polymer solution. It specially discharges the polymer solution from the used nozzle to the low pressure region.

A method for continuous production of reticulated fibers, wherein the method is carried out by using a mechanical mixing region provided in the extruder screw at least in the polymer dissolving zone with little mixing and dissolving. It is preferable that :::: It is more preferable that the above method is a continuous production method of a network fiber in which the mixing and dissolution of a polymer and a solvent are performed in multiple stages in a polymer dissolution region.

It is preferable that the above-mentioned method is a continuous production method of a reticulated fiber in which the addition of a solvent and the mixing and dissolution of a polymer and a solvent are performed in multiple stages in a polymer dissolution region.

In the above method, when adding a solvent and mixing and dissolving a polymer and a solvent in multiple stages, each time a solvent is added, the polymer is mixed and dissolved in a polymer dissolving zone, and the polymer is sequentially dissolved. It is preferable to use a continuous method for producing a mesh fabric with a reduced degree. · More preferably, the above method uses a screw extruder to continuously supply the melted polymer, and the supplied polymer melts the polymer melt zone. When the polymer and solvent are mixed and dissolved under pressure, multi-stage addition of the solvent to the polymer in the polymer dissolution zone causes less mixing. In particular, the first stage is continuously melted by screw extruder. For the lined polymer, it is attached to the extruder screw. Reticulation of the network so as to be carried out in the area of mechanical mixing: a special production method, and even more preferably, the method comprises the step of dissolving the solvent for the polymer in the polymer dissolving zone. At least the first stage of multi-stage addition, mixing, and dissolution involves pressing the molten polymer continuously supplied by a screw extruder. When the mixing is performed in the area of the active mixing attached to the screw of the machine, the solvent is added in the second and subsequent stages. The mixing and dissolution are performed using the static mixing element. This is a continuous production method for net fiber.

The most significant feature of the present invention is that a high-temperature and high-pressure uniform polymer solution can be easily and stably obtained by using a screw extruder. . The consequence of this is that the solution leaks at high pressure can be resolved, the pressure can be easily increased, and a screw extruder can easily supply the polymer, even if it has a high molecular weight. It can be dissolved.

In addition, by using the mechanical mixing area attached to the extruder, the polymer and the solvent can be rapidly mixed under high agitation by a large shear force under forced agitation. I made it. Therefore, the pole Dissolution occurs in a short period of time, and it also has the effect of significantly preventing polymer degradation.

By using such a method of synthesizing, a high molecular weight polymer, particularly a high molecular weight polymer which is easily deteriorated in flash spinning, can be used for the first time according to the present invention.

The terms used in the description of the production method of the present invention will be briefly described. "Polymer dissolution zone J is defined as a state in which the polymer is in a molten state, and a state in which the solvent and the polymer begin to dissolve in a state in which the solvent and the polymer begin to dissolve from a state without the solvent to a state with a predetermined amount of the solvent. An area that contains the polymer in a dissolved state and is in a mixed state.

“Seal” means that the gap is filled with molten polymer and contains no flutes, and no flutes can enter.

“Mixing / dissolving” refers to a state in which the polymer and the melt are mixed and both are melting. ,

—Mechanical mixing ”refers to the mixing that occurs when an element is forcibly agitating the liquid and that element is driven by an external drive source.

In the production method of the present invention, high-density polyethylene is used as the polymer, and the continuous supply means is a screen commonly used in the production of textiles and other various extruded products. An extruder can be used.

That is, the screw press machine is composed of a driving motor, a high-speed machine, a hopper for supplying polymer, and a barrel section for ripening and melting the polymer. Power, become. This knurl has a structure that can be ripened by mounting a heater. A screw is installed inside the barrel, and this screw is connected to the drive motor through a thrust bearing and reduction gear.

The screw can be divided into three main areas: the supply section, the E 缩 section, and the measurement section.The polymer is propelled to the exit while being pre-ripened in the supply section. . It melts while being compressed in the compression section and reaches the measuring section. 'The extruder used in the present invention is provided with a container injection port at the measuring section where the polymer is completely melted, and the check valve is grounded. This valve is connected to a high-pressure metering pump for supplying the solvent. The solvent is injected into the metering section filled with the molten polymer coming from the screw pouring section, and the polymer and the solvent are mixed and dissolved by the screw in this metering section. . ', In order to facilitate the addition of the solvent in the screw at the solvent injection portion; it is preferable to slightly increase the groove depth of the screw to the front and rear groove depths. By doing so, the pressure inside the barrel becomes lower than in the case of supplying the screw, and the backflow and ejection of the solvent to the supplied portion of the screw can be prevented. This mixing ♦ The pressure in the melting section can be freely changed by changing the nozzle size on the outlet side of the extruder. As a result, a pressure suitable for the type and molecular weight of the polymer can be obtained. In addition, the residence time of the polymer in this part can be freely changed by controlling the length of the screw. In other words, in order to optimize the state of the extruder in the mixing / dissolving area, which is a polymer / solvent system that dissolves, the pressure * temperature * mixing shear force * residence time can be set freely. result As a result, a uniform polymer solution can be easily and stably obtained.

Flash spinning solvents and polymers dissolve only after high pressure. Therefore, it is necessary to use a high-pressure vessel instead of adjusting the volume of the solution. In particular, it requires a high-pressure vessel under temperature conditions up to 350 ° c. In addition, a high-E container with stirring is required.

At this time, he encounters a difficult task called the sealing of the movable eclipse. Use a high molecular weight in the franchiss spinning system, for example, a high-density polyethylene with a melt index (Ml) of 4 or less (weight-average molecular weight of 10 10 ⁴ or more). If so, it is necessary to increase the pressure. If the pressure is not high, the molecular weight used is not only limited, but also a relatively low molecular weight takes a long time to dissolve, causing deterioration of the polymer. -The present invention developed a technique called liquid sealing with a molten polymer, and-solved this problem. More specifically, the space formed by the extruder barrel and the screw is filled with a polymer to prevent the ejection of the solvent gas. What is important in this case is that the space is filled with the molten polymer and flowing toward the front of the screw, and therefore a pressure gradient is created.

The details of the situation during this period are as follows.

US Zeher of Tadmor and Im Rich Klein Author "Engineering Princi les or P las tica tx ng B trudor" (Van Nars trand Reinhold Company issued) of p79~ pl07 and _{P 359~} P400 to as more information has been properly also described, Depending on operating conditions, a maximum of pressure always occurs in the extruder. More specifically, the screw supply unit, When divided into a compression section and a measurement section, a local maximum of pressure occurs before and after the starting point of the measurement section after the polymer melts. The pressure gradually decreases after this maximum. In particular, if the depth of the screw section of the metering section is made deeper than the pressure end point corresponding to the minimum guide depth of the compression section, the pressure often drops, and in that case, the compression section ends. A pressure maximum occurs near the point. This pressure is used to seal the solvent.

Therefore, it is necessary to devise the dimensions of the screw used. That is, the length of the supply section is increased to some extent in order to complete the melting. In most cases, the diameter of the extruder is the same as the screw screw's pinch. The length of the feed section is at least Ί pitch, preferably at least 9 pitch. ,

In addition, the compression ratio of the screw is important for pressure build-up. When the polymer supply form is a pellet, the compression ratio is 3.0 or more, and when the powder supply is powder, it is 4.0 or more. Is good.

Generally, the length of the compression section is sufficient to be 5 pitches, but it is preferable that the length be 7 pitches or more. As for the end point of the compression section, a so-called mixing zone (mixing zone) may be provided near the start point of the measurement section. This part is short and should be subjected to high shear.

The form of the metering section is preferably longer because a solvent supply port is provided in this section. That is, it is 7 pitches or more, preferably 8 pitches or more. It is better to install the solvent supply port at the third or fourth pitch after the start of the metering section. Of course, even if it is longer than this Good. Further, to facilitate the introduction of the solvent, the diameter of the screw at the portion where the solvent is introduced is reduced. In other words, it is better to increase the groove depth. It is desirable that the length of this portion be at least two pitches, including a little or an increase in the screw diameter.

Further, the groove depth of the metering section is 1 mm if the extruder diameter is 35 ™ ø. 3 mm density, 65 mm-2 mm: about mm, 90 ma. ¾ ¾> 2 .5 ヽ ¾ 4.5, 120 mm φ ¾Γ 刀 ram sword; ^ ο am, 150 Φ 3 mm to -6 mm is preferred.

Furthermore, the gap between the outer diameter of the screen and the barrel diameter of the extruder is usually 0.1 to 0.8 mm. The smaller the bore, the better the gap. . Also,揉作conditions, scan click Li Interview - a in terms of the above dimensions, temperature, disk re-menu rpm -., By discharge amount constant circle _P that is, to start the extrusion operation, to a predetermined temperature - Te Solvent is determined by trial and error method. Calculate the screw rotation speed and discharge rate conditions that do not blow out from the mouth. As an example of the discharge temperature, 200 for polyethylene. 280 is selected from c. At this time, the pressure at the maximum pressure point in the pressing machine is preferably at least 100 kg. This does not mean that operation is not possible even under pressure, but the pressure may fluctuate further due to fluctuations in the discharge amount and the solvent may be ejected.

This method is for obtaining a net-like fiber from flash spinning, and after performing this step,

① Immediately supply to the spinning device,

② After introducing to the next mixing device, supply to the spinning device,

Mixing with new solvent in the next mixing device, spinning device Supply to the

Are selected.

In the step (1), it is necessary to increase the hole-up volume of the mixing section of the present invention in consideration of the residence time required for mixing, but this is the simplest process and is preferable. is there.

In the present invention, the high-temperature and high-pressure solution of the polymer and the solvent is flash-flushed by a spinning device to obtain a mesh fabric. This flash discharge method uses a well-known technique, and often uses a depressurizing orifice, a depressurizing chamber, and a spout assembly composed of a spinning nozzle. Discharge is preferred. The shape and structure of these devices can be arbitrarily selected.

The polymer solvent system used in the present invention does not dissolve at normal temperature and normal pressure, but dissolves only at high temperature and high pressure. Therefore, as a general feature, they belong to mutually insoluble systems, and do not easily dissolve even at high temperatures and high pressures. For this reason, it is preferable to provide a region for mechanical mixing by attaching to the screw of the extruder. That is, by increasing the contact area between the polymer and the solvent, the dissolving area is increased and the polymer is rapidly dissolved. One way to do this is to provide a special mechanical mixing section on the same floor as the extruder-the term "special" refers to the extruder screw feed, compression section It also means a structure that is different from the screw structure of the measuring section and aims to improve the mixing and stirring effects. For example, a structure called dalmage corresponds to this.

In the present invention, the drive system of the extruder is one, and the screw of the extruder has a melting supply section and a special mechanical mixing section with a solvent, and In addition, it has a solvent injection part in the barrel of the middle part. In this machine, a feeder, a presser, and a meterer, which are used for normal melt molding, are added to the front of the normal screw, which has a mixing function. It can be formed by adding a barrel having a special mechanical mixing section provided with a solvent injection port. Also, it may be one uniquely designed for use in the present invention.

In this preferred embodiment, the molten polymer is supplied by the rotation of the extruder screw, and the molten polymer is surrounded by a solvent provided separately by a metering pump or the like. Is mixed mechanically. The extruder and the structure have a drive system. The sliding part of the extruder has the same structure as that of a normal extruder, and the low-viscosity 'solvent' solvent is blocked by the molten polymer. It does not reach this part in shape.

There are various types of silica structures having a mixing function used for mixing the molten polymer and the solvent, and these have various shapes, and these can be used in the present invention.

That is, it may be of a dal-mage type, of a multi-threaded structure with a notch, of a dam structure, of a multi-row pin structure, or a combination thereof. Further, dams, grooves and pins may be provided on the barrel side to combine with the above-mentioned structure. Furthermore, the revolving body and the barrel may be polygonal, aiming at the second impeachment. These are selected according to the type of polymer used, melt viscosity, type of solvent, mixing ratio, and the like. -This preferred practice makes it easy to use high molecular weight polymers, It can be dissolved in a solvent in a short period of time without deterioration, and a more preferable fabric can be obtained stably and continuously. An even more preferred embodiment is a method of mixing in multiple stages, and a more preferred method is to add a solvent in multiple stages and mix and dissolve.

As the most suitable practice, the first stage involves adding one part of the solvent to the mechanical mixing area attached to the screw, mixing and dissolving it, and then mixing the second and subsequent stages. 'There is a method in which a static mixing element is used as a dissolving means, and the remaining solvent is sequentially added to each of the static mixing elements to mix and dissolve.

In the above-mentioned conventionally known technique, a required amount of a polymer and a solvent are mixed and dissolved at a stroke in order to obtain a solution having a predetermined concentration. In this method, however, mixing and dissolving, especially dissolving, require a considerable amount of time1, and it is not easy to obtain a uniform polymer solution. '

The present inventors have considered this problem in various ways, and as a result, have found that the polymer solvent system used for flash spinning is more easily dissolved as the polymer concentration is higher. And found that it was easier to dissolve. As a result, a more preferable method of the extruder dissolution method of the present invention has been invented.

In other words, if we explain using a high-density polystyrene / fluorocarbon —11 (trichloro mouth fluorometer) system as a matrix, the phase of the graph in FIG. As shown in the figure, it can be seen that the polymer concentration is more easily dissolved at 15 wt% than at 12 wt%. Furthermore, it was found that the higher the concentration of the polymer, the easier the dissolution. This The rough shows that it has an LC ST-type citrus diagram in polymer solution theory, and the behavior is consistent with the results of the present inventors' research (Polymer Science Society, published by Kyoritsu Shuppan, Polymer Experimental Science , Vol. 11, ^K- Polymer Solution ^P139-20 ). -Therefore, the effect of the present invention will be exerted more and more if the solvent is sequentially added in multiple stages to the molten polymer, and the polymer concentration is reduced sequentially in multiple stages.

In the present invention, the solvent is added in multiple stages using a pump or the like, but it is preferable to add a polymer and solvent mixing operation after each addition of the solvent. This mixing operation can be performed by any technique, such as mechanical stirring using a stirring blade or a mixing screw, or static mixing. Etc. may be employed. Also, by combining these, it is possible to make a very preferable process. :

In the present invention, the multi-stage addition of a solvent means an addition divided into two or more stages, where the portion where the polymer and the solvent first merge is one step, and the limit is two steps or more. Not done.

The means for adding the solvent after the second stage is not particularly limited, but it is preferable to use a static mixing element. In other words, these are assumed to be devices that have sufficient mixing capacity and do not have a sliding part. The type of the static mixing element is not particularly limited, and may be a conventionally known type or an improved type thereof. Examples of known types include Kenix's Static Mixer, Sulza's Mixer, and Toray's High Mixer. ' • In the present invention, the polymer is preliminarily mixed with a part of the solvent in the early stage of mixing, the viscosity is reduced, and the affinity with the added solvent is also increased. The pressure loss in the static mixing element is small, and a uniform solution can be easily obtained. Therefore, the degree of freedom with respect to the shape and the number of stages of the static mixing element is large and can be selected as appropriate.

Further, in the method of the present invention, an arbitrary solvent is employed depending on the polymer used. That is, a combination of a well-known polymer and a Z solvent used for obtaining a network fiber from a flash spinning can be used. Examples of the solvent include methylene chloride, and trichloride. Fluoromethane (b), Tricyclone trifrenoleuroethane, hydrogenated hydrocarbons, etc. are used. And these can be mixtures

An object of the present invention is to obtain a reticulated fiber from flash spinning, and the ratio of the polymer and the solvent in the present invention can be arbitrarily selected within the range of the object. You. From this viewpoint, the polymer concentration of the spinning solution for obtaining the network is preferably 5 to 20 wt%.

Therefore, in the method of adding a solvent in multiple stages according to the present invention, the amount of the solvent necessary for achieving the final polymer concentration of the spinning solution is determined for the continuously supplied polymer. Divide and inject. Since the addition is carried out in substantially multiple stages, it is preferable to add a solvent amount in the range of 1 to 99% of the total solvent amount in each stage. Preferably, 1 to 90% of the solvent is added in the first stage, more preferably 5 to 80%. Then, the necessary remaining solvent is added at a later stage. However, it is also optional to add these in a more divided manner, and the dividing method may be arbitrarily selected. '

The above-mentioned conditions will be specifically described for flash spinning of a system of high-density polyethylene and F-11. The molecular weight of the polymer, expressed in melt index (.I.), Is

I 0 (weight average molecular weight of about 7 × 10 ⁴ ) or less, preferably 1 (weight average molecular weight of about 15 × 10 or less, more preferably 0.8 (weight average molecular weight of 16 × 10 ⁴ ) or less; It can be used up to 0.05 (weight-average molecular weight of about 40 × 10 ⁴ ). 'A melt index of 1.0 to 0.1 can be recommended as a particularly preferred range. The polymer is melted in an extruder in the range of 200 to 300. The melt index is increased by 0.8 as the force decreases. The ripening temperature needs to be set high The screw shape used may be a pitch structure with the same screw screw pitch and screw diameter that are usually used, but the high molecular weight (Ml is small) Polymer requires a longer feed section In addition, there may be a screw mixing zone that applies a special shearing action at the end of the compression section and at the beginning of the metering section in order to make the melting easier and faster, thereby completing the melting. When the polymer has completely melted, it enters the polymer dissolution zone.The polymer dissolution zone has a solvent inlet through which solvent is injected.The solvent injection pressure depends on the pressure of the polymer dissolution zone. The pressure in this polymer dissolution zone is used to create a homogeneous polymer solution. It is important and therefore depends on the molecular weight of the polymer. The pressure in the polymer dissolution zone is determined according to the molecular weight of the polymer, and the solvent injection pressure is determined correspondingly. Therefore, it is advisable to use a pump that raises the maximum shochu pressure (approximately 500 kg / cm ² · G in a row) and pumps out a constant volume regardless of the pressure. There is a pump.

The solvent to be injected may be ripened or may not be ripened. A little heating is preferred because mixing and dissolving can be performed stably. For example, the force depending on the type of the solvent is within a temperature range of 50 ° to 200 ° C. for fluorocarbons.

It is advisable to install a check valve at the filler inlet to prevent polymer backflow. The check valve may be of a commonly used structure, but preferably has a structure that is easy to clean when the boiler is clogged. Further heating this valve is recommended.

Next, the pressure in the polymer dissolution zone, the pressure in this area is the point at which it is completely filled with the decayed vol- ume, that is, shortly before the solvent inlet, the screw in the screw of the screw. In terms of the number of pitches, it is the pressure in the area starting from two to three pitches before reaching the decompression chamber orifice.

This pressure is as follows when the polymer is a high-density polyethylene. In other words, if it is a polymer with a mole index of 5.0 (M i), it is about 150 kg / crf · G to 350 kg Z cn! Ma in a flat et 1 60~ 360 kg cm ² - about G, 0. 8 the volume Li Ma - if 1 70~ 400 kg / ci 'G , 450 200~ if port re-mer 0. 3 kg d - G, if it goes beyond 0.3 and reaches 0.03rd place, 250 Mixing and dissolving can be performed sufficiently by applying a pressure of ~ 500 kg / dG.

In general, not only high-density polyethylene, but also the higher the molecular weight of the polymer, the higher the pressure in the polymer dissolution zone. Therefore, it is necessary to ensure that the withstand pressure of each device such as a special mixer, static mixer, etc. is sufficiently high, including the screw unloader-and the Sf pressure strength is 200 to 750 g / οέ. · G is preferred.

Therefore, it is necessary to pay close attention to the seals of each flange and the detectors for the pressure and tinge. A hollow metal 0 ring type is easy to use as a seal for the flange. The metal seal is convenient for the seal of the detector.

In addition, the sealing in the direction of the end of the screw ¹ is performed with a fluid sealing force of the melted vol- mer, so that at least the number of screws of the screw of the screw is used. The pressure at the position before the touch must be higher than the pressure at the solvent injection section. For this reason, the space volume of the solvent injection section should be larger than the space volume of the extruder hopper side. That is, the groove depth may be increased. Due to such a structure, the pressure immediately before the solvent injection port is higher than the pressure in the polymer dissolution zone. Due to this pressure gradient, the solvent is completely sealed and does not flow back to the hopper or blow out. As a preferred method to keep the pressure in this area always maximum, a gear pump should be installed at any point in the polymer melting zone. The most preferred installation point is after the special equipment mixing section. With such a configuration, a fluid seal made of a polymer melter is more complete. · At the solvent injection section, the polymer and solvent merge and pull into a special mechanical mixing section. This 0 portion has the same shape as the screw as a preferable form. Therefore, the rotation speed is the same as the screw rotation speed. However, in the case of the mixing unit of this type, the pump capacity is not provided, and the mixing and stirring function is mainly used.

In this case, the pump capacity will be borne by the screw extruder and the ';' Bump capacity of screw extruder It is in the metering section of the screw extruder. Therefore, it is necessary to increase the length of this part as the pressure in the polymer solution becomes higher. '

The temperature of the destructive mixing section is preferably set lower than the temperature of the screw extruder. As described above, the solvent system used for flash spinning is a LCST-type solution as described in the polymer solution theory. There is no need to increase the temperature of this part. The appropriate temperature is also preferable from the viewpoint of preventing polymer deterioration. For high-density polyethylene, 170-

220, more preferably 180-200.

Although the length and form of the special mechanical mixing section are various as described above, it is preferable to increase the length in terms of mixing capacity. The form is preferably a dull-mage type, or a kneader type or a rear type, but this type is adopted. In particular, if the length is increased, the load becomes large, and a large amount of heat is generated. It tends to be. In order to suppress this heat generation, a part thereof may be changed to a pin-type mixed structure.

In general, it is preferable to increase the length of this portion as the discharge rate increases and as the molecular weight of the polymer increases. When adding a solvent in multiple stages, go to this special mechanical mixing section. Is the first stage. In this case, it is necessary to consider the distribution of the amount of solvent added.

In general, the larger the molecular weight of the polymer, the better it is to increase the amount of solvent added in the first stage. If there is no major obstacle,-In order to make the solvent pump type used at each addition point the same, it is better to add a solvent of equal distribution method.

In the high-density polyethylene-i 1 system, the addition amount in the first stage should be 10 to 70% of the total addition amount.

A gear port and a pump may be provided next to the special local mixing section. The form of the gear pump may be the one usually used for extrusion molding. Of particular note is the shaft seal of the gear pump. The viscosity of the mixed polymer solution in this part is about 30 to 500 centipoise, which is higher than that of the fluid on the port side. Therefore, it can be used with a normal ground seal.

A better sealing method is to allow a small amount of the solution to leak at the beginning-because the leak precipitates and fills the erosion gap with the polymer, which encourages the lubricant. ■ ο

Further, by installing a gear-pump, the pressure in the subsequent area can be further increased, and the degree of dissolution can be freely controlled.

In particular, the pressure of the special mechanical mixing section can be freely controlled by the rotation speed of the gear-pump. Therefore, by increasing the pressure in this part, dissolution at a higher pressure can be performed, and dissolution can be accelerated. The setting of these pressures depends on the type and amount of polymer 'solvent Since it changes, an optimum value may be set by a trial and error method.

Pull into the second stage static mixing section. It is more preferable to provide a solvent injection unit in front of the second-stage static mixing unit. However, the inlet may not be provided.

It is important to design the structure of this solvent injection port so that the mixed polymer solution from the previous stage and the newly added solvent are powerful and evenly distributed over the entire cross section of the piping. is there.

Because the static mixture becomes laminar mixing, mix

Five

-1

If the viscosity ratios of the liquids are significantly different, concentrated addition of the solvent will result in inadequate mixing and incomplete dissolution, giving unfavorable results. For this reason, it should be distributed uniformly over all sections. For example, using a perforated plate, the mixed polymer solution from the previous stage may be discharged into the solvent as if it were "Sou", or a number of solvent jets D. may be provided in the piping cross section. I prefer to do it.

At least 40 stages are required for the static mixing element. Therefore, even if the pressure loss per static mixing element is small, the total pressure loss is as follows. Therefore, it is recommended to collectively support each unit, collect all stages and collectively support at the outlet side. Unless such measures are taken, buckling may occur at the final stage.

The temperature of the piping system including this static mixing element may be lower than that of the previous stage. Since the temperature of the polymer solution is determined in this part, it is preferable to lower the temperature unless a trouble occurs. 160-200 for high density polystyrene examples, preferably '170-180 It is.

Of further note is the pressure of the polymer solution leaving the final mixing section. The pressure in this area directly affects the pressure in the decompression chamber and immediately affects the spinning state.

Significant fluctuations in pressure at the exit of the final mixing zone indicate that the polymer has not yet completely dissolved into the melt. Therefore, if the pressure change width is large, it is necessary to further increase the number of mixing stages or the number of solvent addition stages.

Generally, the pressure fluctuation width immediately after the final stage of mixing and immediately after the compression chamber is preferably 5 / cm ¹ 'G or less, more preferably 3 kg / erf · G or less.

: J Noru

A filter may be provided in the final stage of mixing and immediately before the pressure chamber. <There are various types of filters, but a filter having a large filtration area and a small pressure loss is preferable. In general, a pre-type or disk-type surface filtration method may be used.

In addition, the distribution system, including the mixed area, shall have a structure in which no ban part occurs as much as possible. If there is a blind spot that causes stagnation, a degraded bolimer will occur, and this degraded material will fall off and plug the orifice hole. This has very undesirable consequences.

In addition, make sure that there is no narrow gap in the flange and detection end, including the extruder system. If a polymer solution enters this area, stress corrosion will occur and a crack will form, from which polymer solution may erupt. In order to prevent this corrosion, a material having high corrosion resistance may be used.

Pulling it to the brass spinning section. This part is Wheels · Consists of a decompression chamber and a spout orifice. The shape, dimensions, and the like of this part are the same as those of a conventionally known technique. However, the dimension of the orifice will be determined in consideration of the pressure in the polymer melting zone and the pressure in the compression chamber.

Pressure and temperature ultimately affect the spinning state and the physical properties of the obtained fiber. The pressure and temperature of this part of the decompression chamber flash spinning section is 40 kg Ζ αι! · G 1 50 kg cr crf · G and 1 501 in the case of high-density polyethylene. 90 c. The optimum value of the temperature ♦ pressure varies depending on the operating conditions, and is particularly affected by the molecular weight of the polymer. Basically, in some sense, a disadvantage of phase separation occurs. Therefore, the conditions of the decompression chamber are determined in consideration of the operating conditions and the state of phase separation.

FIG. 5 to FIG. 10 show an embodiment of an apparatus for carrying out the method for producing a reticulated fiber of the present invention.

FIG. 5 shows a flow chart of a typical process of the present invention, and FIG. 6 shows the inside of a screw extruder used for this. That is, as shown in FIG. 5, the manufacturing apparatus is provided with an extruder 4 barrel 5, a solvent pump 6, and a spinning device 7. The melt is melted by the extruder 4 and sent to the melt zone where the melted polymer in the renole 5 is closed. Solvent is pumped from a separate solvent pump 6 through a polymer check valve (not shown) into the poly-dissolution zone. The rotating screw in the barrel 5 mixes and dissolves the solvent and the poly to form a uniform poly solution, which is sent to the spinning device 7. The spinning device 7 comprises a decompression orifice, a decompression chamber and a spinning orifice, and a heating device. At this point, the polymer solution is spun into a low-pressure region through the spout orifice, forming a continuous mesh fabric.

The extruder barrel 5 has a screw 1i in the barrel as shown in Fig. 6, and this screw is provided with a lined section 12, a compression section 13 and a weighing section 14, 15, It consists of 16. 'Looking closer at this metering section, metering section 14 is filled with molten polymer coming from compression section 3 and cannot flow back to hopper port 1 if melted . In addition, the measuring section 1554 has a larger depth than the front section 16 and the rear section 14, so that a minimum pressure portion is formed in the measuring section. For this reason, the solvent from the solvent inlet 18 is easily injected into the extractor barrel. The molten polymer coming from the front of the metering section 14 and the solvent coming from the inlet 18 are mixed by the screw rotating at the rear section 16 of the metering. The solution flows out of the opening 20 as a solution. The metering units 14, 15, 16 are optimized by the polymer flow rate and the solvent flow rate.

FIG. 8 shows another preferred embodiment of the extruder.

Fig. 7 shows the structure of the extruder used to carry out the present invention and the special mixing structure (mixing mixer) of the screw and the co-wheel. The polymer is supplied from 17 and is melted by the screw 21 by the face rolling of the driving system 19 and extruded forward (to the right in the figure). On the other hand, the solvent is added from the solvent inlet 18 installed in the barrel 5, and the two are mixed by the mixing structure (dalmage type) 22 to reach the outlet opening 20 of the mixture. Fig. 8 is a structural diagram with mixed structures (Dalmage type and Pin type) 22 'and 22 "having different shapes from Fig. 7.

In the present invention, the mixture coming out of the outlet opening 20 is directly guided to the spinning device, or after that, a solvent is further added and a mixing operation is performed, and then the mixture is guided to the spinning device. To obtain a reticulated fiber. .

The diameter of the screw of the extruder is selected according to the production amount of the mesh fiber to be produced, and the diameter of the same structure is the same as the diameter of the screw of the extruder. Or different. In each case, the length of the structure is arbitrarily determined depending on the required mixing degree and the volume of the hole-up in consideration of the residence time. <FIGS. 9 and 10 show the present invention. 4 is a schematic flow chart showing a further preferred embodiment (equipment) of the present invention, wherein reference numeral 4 denotes an extruder 5, a barrel 8, a special mixing section 8 coaxially with the extruder 5, and a solvent bottle 6. 9 shows a mixing section composed of a static mixing element, and FIG. 9 shows an example of multi-stage mixing, that is, the polymer was mixed and melted in a special mixing section denoted by reference numeral 8. Thereafter, the mixture is further mixed and dissolved in the static mixing section 9.

Figure 10 shows the process flow sheet in which the solvent is added in multiple stages and mixed and dissolved each time. That is, the solvent is added to the first-stage mixing section 8 from the first-stage solvent pump 6, mixed and dissolved, and further added and mixed and dissolved in the second-stage mixing section 9 from the second-stage pump 6. To obtain a polymer solution of the same polymer concentration. As described above, according to the present invention belonging to the class ^ _, since the stirring mechanism for dissolving the polymer can be reliably closed,

'' Δ polymer can be dissolved in a short time to dissolve the polymer in a short time because the mixing effect is large, and the mixing effect is large, and the polymer is dissolved using the thermal power and chemical characteristics of the solution. Since high molecular weight and narrow molecular weight distribution of the polymer can be dissolved uniformly, and the flashing force can be extremely increased by spinning under high pressure, A high-density polyethylene-based three-dimensional network fiber with a long-period scattering intensity ratio of 40 or less is generated, and a three-dimensional network fiber with a long period of 150 A or more and 200 mm or less is obtained. -In addition, a three-dimensional network fiber having a specific surface area of 30 nf ng or more is produced. (I)-Next, a method for producing a three-dimensional silk fiber using the high pressure differential activation method, which belongs to the above-mentioned classification 1: in the method for producing a three-dimensional reticulated fiber of the present invention, will be described. '

According to the production method of the present invention belonging to the category, as described above, a high-pressure uniform solution comprising a high-density polyethylene-based polymer and chlorofluorocarbon is composed of a decompression orifice, a decompression chamber, and a spinning nozzle. In the method of extending the spinning device and flashing to a low pressure range to obtain a high-density polyethylene-based polymer network weave, a high pressure difference is generated before and after the high pressure orifice. And activates the body.

The production method of the present invention, which belongs to a further class, differs from the conventionally known method of spinning by setting the conditions of the pressure chamber so that the polymer liquid belongs to the two liquid phase region. Spinning from one liquid phase region As a result, there is a clear advantage that the pressure in the decompression chamber during spinning can be increased.

Therefore, according to the present invention, it is possible to obtain a higher solvent flashing force than conventionally known techniques, and it is possible to obtain a high-strength fiber that is stretched and oriented more highly. . Further, since the pressure in the decompression chamber can be increased, it is possible to obtain high-strength steel by spinning at a relatively low temperature at which the decomposition of the polymer solvent does not occur. Means both one-phase solution and two-phase solution.

The high pressure difference referred to in the present invention means that, for example, an orifice is provided at an inlet of a decompression chamber and a pressure difference is generated by this orifice ', which is not implemented by a conventional method. A high pressure difference. For example, it means a pressure difference of at least 80 _kg / oi G or more.

Activation means that when a phase separates from one liquid phase to two liquid phases, the liquid undergoes kinetic fluctuations so that phase separation occurs easily. For example, it means that fluctuation such as density occurs. Whether it is activated or not can be determined by measuring light transmission through a pressure vessel with an optical window and a container. That is, when a high pressure difference is generated in the one liquid phase solution, the transmitted light is not transmitted at all. After a while, a clear solution is obtained. This temporary fluctuation means activation of the liquid.

In the present invention, it was not previously expected that a highly fibrous, high-strength reticulated fiber could be obtained by spinning from the one-liquid phase region, which has not been conventionally recommended. is there. In the present invention, this was made possible only by applying activation to a liquid, and in the present invention, this activation was achieved by generating a high pressure difference in the liquid. .

This pressure difference must be high enough to activate the liquid, and is arbitrarily selected according to the polymer used, the concentration, and the like. For example, it is preferably at least 30 kg / erf G. In the present invention, a large pressure difference is suddenly generated in the 滹 pressure orifice, causing some structural change in the solution, leading to a ^ pressure chamber, and discharging the solution at a higher pressure than the spinning nozzle. This 丄 0 structural change is caused by thermodynamic fluctuation due to high pressure difference. This thermodynamic fluctuation generally means, for example,

* Re, it is.

"The phase diagram showing the boundary condition h of one liquid phase and two liquid phases of the polymer solvent referred to in the present invention is obtained by measuring the phase equilibrium of the polymer solution.

These can be determined by the usual method of observing the cloud point. That is, using a high-temperature and high-pressure vessel having an optical window, the change in transmitted light in the case of one liquid phase and in the case of two liquid phases is observed with a visible light or a single laser beam, and the boundary (cloud point) Obtained by finding conditions.

20 These cloud points are due to the type of polymer (molecular weight, molecular weight distribution and molecular weight), the type of solvent, the polymer concentration of the solution Φ, the temperature, and the pressure. Then, in accordance with the usual method, it is determined by observing the occurrence of an equilibrium cloud point when a solution in which the type and the degree of the polymer solvent are determined is used. That is, the solution

The pressure is gradually changed while keeping 25 at a constant temperature. Also remove the solution Gradually change the temperature while maintaining a constant pressure. Alternatively, depending on the case, the temperature and the pressure may be simultaneously and slowly changed, or the like, and any method may be searched for.

The specific solution activation method in the present invention means a large pressure change, as shown in A _: -→ B of FIG. That is, A is the pressure of the solution and B is the pressure in the pressure chamber. And, as described above, the mesh steel obtained from such a large pressure difference is a non-conventional weaving fiber, and as shown in Fig. 1, point B is one liquid phase. The spinning method is preferred.

In the production method of the present invention, the amount of the polymer in the polymer solution is 4 to 25 wt%, and preferably 5 to 20 wt%.

Hereinafter, a spinning method belonging to Class 1 of the present invention will be specifically described. The batch type generally uses an autoclave equipped with a stirrer device. The autoclave is a stirrer for mixing and stirring the polymer solution, a resistance thermometer for detecting the temperature inside the autoclave, and a diaphragm type for detecting the pressure inside the autoclave. It has a pressure gauge. In general operation, a polymer is added into the autoclave, and the lid and the body, which form part of the autoclave, are connected by a mounting bolt. Next, the inside of the autoclave is evacuated through a valve to completely remove the air, and then the solvent is introduced from the valve and sealed.

The polymer and the solvent in the autoclave are ripened by the built-in heater provided on the entire surface of the autoclave while being stirred by the stirrer. The polymer can be dissolved in a solvent. In the process of dissolving this polymer in a solvent, What is important is that for a given polymer and solvent combination, the temperature and pressure conditions be such that the polymer solution can be maintained in a clear, homogeneous phase. This is equivalent to setting the stirring in the autoclave to one liquid phase condition in the Kanazu diagram.

According to the method belonging to the classification ^ _ of the present invention, in order to prevent the polymer and the solvent from aging, a flash which occurs adiabatically at a temperature of a preferable solution is higher than a temperature at which the polymer dissolves in the solvent. This is the temperature at which the amount of heat required to evaporate the existing solvent is needed. If the extrusion temperature is too high, the degradation of the polymer will be marked by radicals generated by the aging of the polymer and the thermal decomposition of the fermentation medium, and the degradation of the polymer will be significant. Causes deterioration and coloring.

The pressure of the solution in the autoclave can be arbitrarily selected as long as the pressure is higher than the above-mentioned boundary pressure for maintaining a clear homogeneous solution. The required pressure can be obtained by a mechanical pump or pressurization of an inert gas.However, the inside of the autoclave is completely filled with the solution, and the desired pressure is applied by utilizing the ripening of the solution. The method of obtaining is preferred. The pressure of the solution is measured by a diaphragm pressure gauge.

Next, by opening the release valve, the polymer solution consisting of a large phase passes through the autoclave and the vacuum chamber by the pressure in the autoclave, and then through the spinning nozzle. It is rapidly released under atmospheric pressure and flash spinning is performed. In patch operation such as autoclaving, the solution is In order to keep the internal pressure of the lave constant and to keep the flow rate of the solution through the spinning nozzle constant, a method of increasing the pressure using an inert gas pressure or a liquid pressure such as nitrogen may be used.

The polymer solution extruded from the discharge valve causes a pressure drop when passing through the decompression orifice, and the pressure in the decompression chamber measured by the diaphragm type pressure gauge and the pressure of the solution are increased. In the present invention, it is necessary that the difference between the pressure and the pressure is set to a high pressure difference sufficient to activate the liquid. For example, at least 80 kg Z cm ^; G or more is preferred.

Then, the temperature of the pressure chamber is maintained at the same level as the solution or slightly lowered.

The solution discharged from the spinning nozzle is highly fibrillated due to the flash of the solvent and solidification of the polymer, and is fully stretched. Give Ori,

The vacuum orifice, vacuum chamber and spinning nozzle used in these spinning processes may have any conventionally known shape and structure. That is, it is sufficient that the pressure difference of the low pressure orifice, which is a necessary condition for the present invention, is sufficient to activate the liquid. In addition, the depressurization orifice appropriately corresponds to the viscosity, flow rate, extrusion pressure, and spinning temperature of the solution so that the polymer liquid belongs to one liquid phase region in the phase diagram in the decompression chamber. The diameter and shape of the spinning nozzle are arbitrarily selected. The volume of the pressure chamber is selected so as to have a residence time for maintaining the activated state of the liquid, and is usually about 0.5 to 1 O c c, but is not particularly limited.

The spinning method of the present invention can be carried out in either a batch system or a continuous system. ' In particular, in a continuous method, if a method is used in which the entrance of the polymer dissolving area is sealed with a molten polymer using a screw extruder, it is easy to produce a high-pressure homogeneous solution. Multi-stage addition of solvent to the polymer * At least the first stage of mixing and dissolving, for the polymer that is illegally melt-filled by the screw extruder, This is performed in the area of the target mixing provided in the screw of the extruder. When the solvent addition, mixing, and dissolution in the second and subsequent steps are performed using a static mixing element, a more uniform solution is used. It is easy.

As described above, the present invention, which belongs to the category, is characterized in that a high force difference is generated in a polymer solution, instantaneous thermodynamic fluctuations are generated, and the spinning is performed in an activated manner. In addition, since the fiber is spun from the liquid area, there is no upper limit to the force in the “pressure chamber”, high pressure conditions can be taken, and flash flushing is large. A highly fibrillated three-dimensional network fiber having an intensity ratio, a long period of 150 mm or more and 200 A or less, and a specific surface area of 30 or more is produced.

FIG. 4 shows a phase diagram of high-density polyethylene and fluoro-1i measured in the example of the present invention, and illustrates the polymer concentrations of 12 wt% and 15 wt%. .

This is achieved by using a device that has a pair of optical windows at the bottom of the side surface of the autoclave body, is connected to the bottom valve, and has a low pressure / region pressure mechanism. Measured by changing the pressure of the liquid at a speed of less than ^ 5 kg Z ai G per minute and observing a point through the optical window Next, a new high-strength nonwoven fabric (H) composed of a three-dimensional network fiber will be described.

In other words, the nonwoven fabrics belonging to the category I are composed of high-density polyethylen-based fluffy three-dimensional mesh fibers deposited in random directions and firmly and firmly bonded to each other. And an inner layer that is weaker than the surface layer and is thermally bonded to the film-like fiber layer, and has an inner layer having a specific surface area of 5 rrf / 'g. It is a continuous mesh fabric with high tensile strength and high tear strength, and more preferably, the nonwoven fabric has a tear strength of X (kg / 50 g). Method), the tensile strength is defined as Y (kg 3 cm 50 g / m), and the strength of each of the non-woven fabrics is proportional to the standard basis weight of 50 g / m ^2. ¾ 0.4,

.And '

2 0 X “28 ≤ ≤ ≤ 30;;

The ignorance belonging to the classification _L will be described in detail below.

As described above, in this nonwoven fabric, a high-density polystyrene-based three-dimensional continuous mesh fabric is randomly arranged and deposited. — That is, the flash-spun three-dimensional network substantially free of ends is spread, and the fiber elements are arranged so as to be substantially uniform in all directions, and are deposited and accumulated. Has become a texture.

In order to maintain the form as a paper-like nonwoven fabric or to exert mechanical strength, the textile is heat-bonded in the surface layer. This surface layer has a firm bond and does not fluff even if the surface is strongly rubbed with a finger. And this firmly bonded layer Both sides of the front and back sides, or any one side are formed.

The heat bonding strength of the inner layer of the nonwoven fabric is different from the heat bonding strength of the surface layer. That is, the inner layer is a film-iron layer in which the degree of aged adhesion is more gradual than that of the intermediate layer, and thus the inner layer fiber form is left in a large amount. As a result, the D surface layer and the inner layer are independent and form a nonwoven fabric structure.

The cross section of such a nonwoven fabric itself is known, and is disclosed in the above-mentioned U.S. Pat. No. 5,532,589.

However, non-woven fabrics belonging to Class J1 are conventionally known; they are characterized by having a higher specific surface area in each layer than a paper-like three-dimensional network fibrous non-woven fabric. It has physical properties.

The inner film-like fiber layer in the present invention refers to a layer that is partially film-shaped and partially fiber-shaped, and is a layer that is forcibly connected to another layer. In the above, when one part of the fiber-like material exposed by the separation is grasped and it is difficult to make the fiber, the independent three-dimensional net-shaped steel fiber having a length of 10 to several tens απ or more It is a layer that has not been able to find a fiber as a continuum and has undergone sufficient bonding to be cut in the middle.

Non-woven fabrics belonging to the category are characterized in that the specific surface area of this inner layer exceeds 5 tn ² / g. That is, it is a non-woven fabric having a high specific surface area, which is unprecedented as a layer constituting a three-dimensional net-like nonwoven fabric such as paper, and excellent in opacity and covering power.

That is, if the three-dimensional network fiber has a large specific surface area, irregular reflection of light occurs, and opacity * covering power and whiteness increase. The specific surface area of the inner layer is determined by mechanically peeling off the surface layer and the inner layer, and without peeling off the film-like or textile-like material straddling between the layers at the time of separation, using a cutter or the like. It can be obtained by cutting into layers and measuring the specific surface of each layer. In the present invention, the measurement of this area was carried out by the BET method of nitrogen adsorption, and was measured by using a soromatic 1800 manufactured by Carlo Elba.

In this nonwoven fabric, the specific surface area of the nonwoven fabric measured without obstructing the inner layer / surface layer of the nonwoven fabric is 5 / g or more.

This nonwoven fabric has an unprecedentedly high mechanical strength, despite having a high specific surface area as described above. In the nonwoven fabric of the three-dimensional network fabric, a large specific surface area means that the bonding between the fabrics is insufficient and mechanical strength cannot be expected, but in the present invention, both are achieved simultaneously. The surprising effect is obtained. That is, the relationship between the tensile strength and the tear strength, which represents the mechanical strength of the nonwoven fabric, has never been better. Between the tensile strength Y (kg 3 cm width 50 gnf) and the tear strength X (kg / 50 g / m) by Elmendorf, X ≥ 0.4

-20 X + 28 ≤ Y ≤ 30

Here, the strength of the nonwoven fabric is a value converted in proportion to the standard weight, and in the present invention, the standard weight is 50 g / rf. That is, the basis weight of the non-woven fabric belonging to the category I may be 15 to 200 g / m, but is preferably 20 to 120 g / rri, and the central basis weight is 50 g / m '. The strength was determined on the basis of 50 g according to.

FIG. 12 shows the relationship between the tensile strength and the tear strength. As shown in Fig. 12, the range of the strength of the non-woven fabric belonging to the classification is X = 0.4 ゝ Y = 30 and Y =-20 X + 28, and within the area encompassed by X = 0. is there.

The patches described in the above range are data shown in Examples described later, and the same marks are used for nonwoven fabrics using the same filament. Let's do a lot.

-On the other hand, the dotted line in the scope of the present invention indicates data using the fabric described in the comparative example.

Since nonwoven fabrics usually have directionality, the vertical and horizontal directions, and, if necessary, the oblique direction are measured when determining their physical properties. Non-woven fabrics belonging to the JL category are arranged in such a way that each fiber element of the mesh fabric is arranged almost uniformly in all directions as in the previous arrest. Can be measured and the average can be found. And, the physical ratio of vertical / horizontal is included in the range of 1.3Ζ1 to 1 ゾ 3 for non-woven fabric belonging to classification ϋ.

In addition, the directionality of the fiber in the nonwoven fabric can be relatively easily obtained from the transmittance of the Mic polarization in each direction, and by using this method, it belongs to the classification of the present invention. The effect on the direction of the nonwoven fabric can be confirmed. The directionality required from the Mike mouthwave and the mechanical strength, especially the tensile strength, almost match.

The directionality of the nonwoven fabric due to the microwave is measured using, for example, “Microwave Molecular Orientation Meter” OA-200 U manufactured by Shinzaki Paper. -' In the present invention, the tensile strength of the nonwoven fabric is measured according to J IS- 1068 and converted to a standard basis weight of 50 g Z rrf and Y (kg / 3 cm width 50 g / m). And The elemendorf tear strength of the nonwoven fabric was measured in accordance with JIS-L-1085, and converted to the standard basis weight as X (kg / 50 g / m). Various known methods can be sought for the method of thermally bonding the flash spinning and textile sheets. High-density polyethylene adheres at a temperature close to the melting point of the crystal in order to achieve strength as a nonwoven fabric, maintain its shape, and fuzz the surface. Therefore, in order to obtain a mature bonded nonwoven fabric, it is necessary that the mature bond between the fibers is strong, that shrinkage does not easily occur during the mature bond, and that the fiber has a high strength at the high temperature near the bonding temperature. According to the present invention, the above-described three-dimensional network fiber is used as a woven fiber.

As described above, heat bonding is performed by using the net-like textile according to the present invention, which is made of extremely fine fibrils, has a unique structure for a long period, and has excellent high-temperature characteristics. Thus, a nonwoven fabric belonging to the above is obtained, and the nonwoven fabric has a high destructive strength.

Numerous studies have been conducted on three-dimensional reticulated nonwoven fabrics, including the aforementioned US Pat. No. 3,169,899 and Japanese Examined Patent Publication No. 43-21112, and some of them have already been used as products. Du Pont: Tyvek®). However, those having good mechanical properties as shown in the present invention are not known.

The non-woven fabric of the present invention belonging to the above-mentioned category II is also characterized by being opaque. That is, the conventional heat bonding method However, because of the large specific surface area of the reticulated fiber, it reflects light irregularly and has excellent opacity. " Furthermore, since the mechanical strength is high and the high-temperature properties are good, the fiber is not easily damaged by the mature bonding, and the mechanical strength is developed even if the bonding degree is not increased. And opacity

It is unreserved.

The opacity of this non-fiber fabric is different from that of covering materials such as packaging materials, envelopes, and clothing.

This is a very important property. As a method that matches the observation results with the naked eye, a method of measuring the amount of transmitted light by a He-Ne laser is recommended. This measurement was output in a dark room.5 Beam diameter 2.5

The laser light was applied to a non-woven fabric, the amount of light transmitted through the non-woven fabric was measured with a laser parmeter, and this position was continuously shifted and averaged. ·,, Naturally, the amount of transmitted light varies depending on the basis weight of the non-woven cloth, and if the basis weight increases, the amount of light decreases. In the case of the non-woven cloth of the present invention, the basis weight is 25 g Z m and the light quantity is 25 W or less, and at 40 g /

20 W or less, 5 Q g / m ^{2 for} 1.8 W or less, S 0 g Z m for 16 'W or less Is shown. In addition, 22 20 μW or less at 25 / ', 16 βW or less at 40 g / m, 14 4 at 50 g Zm

It is preferable that the weight is less than 12: 丄 W at 60 g of below W W. In addition, other useful physical properties can be imparted to the nonwoven fabric of the present invention to which the classification belongs, while maintaining the above-described mechanical strength and opacity.

25 If it is clear, these physical properties depend on the type of bonding method used. It is possible to give a variety to the people. That is, the nonwoven fabric of the present invention can employ various conventionally known methods in the heat bonding step. Usually, the nonwoven fabric has a large bonding area in order to increase the mechanical strength of the nonwoven fabric. A possible thermal bonding method is adopted. In these heat bonding methods, a flat roll method using a flat roll, a shallow emboss roll of 100 pcs / cnf or more, or a mouthless press method using a sandblast roll is used. It is possible to adopt the rule of force rendering and the method of full calendar rendering. The bonding surface of the nonwoven fabric of the present invention belonging to the category #L obtained from these has a smooth appearance.

as a ί dimensions given can Ru other physical properties, 1 000 ira H ₂ 0 or more 5000 thigh H ₂ 0 following of water pressure and ^{i ~ 1 0 4 · sec /} 5 0. £ range of guard rail Hee Le Toru of I feel better.

The water pressure resistance was measured according to JIS L 1092, and the Gurley-hill i3 temper was measured using a B-type Gurley-type densometer.

The nonwoven fabric of the present invention belonging to the class J1 is a non-adhesive sheet in which the fiber elements are arranged in a random direction by spreading the three-dimensional netted fabric as it is, as described above. It is heat bonded. As a process for obtaining the non-adhesive sheet, any conventionally known process may be selected.

The dissolution process for obtaining the fibers constituting the nonwoven fabric of the present invention is not particularly limited, and a conventionally known dissolution process can be used. This fiber is composed of high-density polyethylene with a high molecular weight and a narrow molecular weight distribution. The raw polymer is dissolved in a solvent in a short time and spun to prevent deterioration of the polymer. To do And melting at high pressure from the spinning machine is required. Spindle assembly for obtaining this textile is not limited as long as it can take the above-mentioned spinning mechanism. That is, the orifice for decompression, the m-chamber nozzle, and the like for activating the homogeneous solution may be arbitrarily used.

As a method of expanding the three-dimensional network fiber into a non-adhesive nonwoven sheet, any known method and apparatus may be used. Basically, it consists of a collision device that spreads the reticulated steel that is spun-a device that determines the direction of travel of the fiber that has spread by collision, a device that gives charge to the spread fiber, and a device that receives and deposits the fiber. ing. That is, a number of methods such as [63, 899, Special Publication No. 44-218Π, and l) SP3 _: 456, 156, and improvements thereof are known, and these methods can be used. , Especially restricted Ά, o

Next, a high-strength nonwoven fabric () having an unfused portion made of a three-dimensional mesh fabric will be described.

In other words, nonwoven fabrics belonging to the classification are made of high-density polyethylene-based fibrous three-dimensional netted fibers, arranged in random directions, deposited in an S-shape, and partially unfused independent A nonwoven fabric including a layer made of mesh-shaped steel fibers, wherein the independent mesh fibers have a long-period scattering intensity ratio of 40 or less. In other words, nonwoven fabrics belonging to the class are composed of high-density polyethylene-based three-dimensional network-connected fibers, which are randomly arranged and deposited. That is, the flash-spun three-dimensional net-like fiber substantially free of ends is unrolled and each steel element is expanded. The layers are arranged so as to be substantially uniform in all directions, and the series is deposited in layers to form a non-woven fabric.

The nonwoven fabric has a partially unfused, or at least part of, a loosely bonded layer in at least a part of the many fiber layers constituting the nonwoven fabric. That is, the above-mentioned layer is provided on the surface of the nonwoven fabric or on the inner layer portion, and an independent net-like fiber can be taken out from this layer. The independent net-like fabric referred to here is, for example, a bundle of steel-like materials generated on the end face when the layers are separated, and separated from other materials by careful pulling. A net-like fiber that can be pulled continuously. Therefore, in this layer, it is not firmly adhered to the film, is not adhered at all, or is loosely adhered '. Therefore, unlike this non-woven fabric belonging to the category i, the woven fabric has a freedom of movement of the reticulated fabric formed in the non-woven fabric, and as a result, flexibility is provided.

Such an independent reticulated fiber retains the fiber form and is a continuous fiber of 20 以上 or more, and X-ray small-angle scattering can be measured in line.

Then, the characteristics of the fine structure of the mesh fiber constituting the nonwoven fabric of the present invention appear. That is, it is characterized in that the long-period scattering intensity due to small-angle X-ray scattering is 40 or less. This indicates that the characteristics of the mesh fabric used to produce the nonwoven fabric of the present invention are manifested as they are. In other parts, the long-period scattering intensity ratio of the part that retains the fiber shape even when the fiber is subjected to a strong thermal bonding process is almost the same as that immediately after spinning. It does not change. On the other hand, the independent reticulated filament in the nonwoven fabric which has undergone the mature bonding treatment tends to increase in long cycle, and is preferably 150 A or more.

Non-woven fabrics belonging to the above-mentioned category are made of fibrous fibers which are extremely gross, similar to non-woven fabrics which belong to the above-mentioned category. It is a mature glued apricot, and is highly opaque to soldiers because of its high mechanical strength and high temperature characteristics near the melting point.

The nonwoven fabric of the present invention belonging to the category ^ includes a layer capable of taking out an independent reticulated fiber form, and the other layers are more firmly adhered to the film even if they are similar layers. May be. That is, any conventionally known method for deeply bonding the sheet may be employed, such as pressing between rolls, force-rendering, and embossing.

I; By sroll: Partially matured adhesives, adhesives with a filter of the fiber force, adhesives in an oven or by forced hot air flow, etc. may be explored. Of course, various methods such as simultaneous processing on both sides, processing on only one side, and sequential processing on one side may be sought. Then, a nonwoven fabric which has been subjected to a treatment such as a kneading process or the like after the mature bonding and a portion of the layers of the silkworm filial layer may be difficult to be softened.

On the other hand, the nonwoven fabric may be a non-adhesive state or a state of being compacted by pressure without performing any heat treatment contributing to adhesion to the sheet-like material. In addition, nonwoven fabrics in which fibers are entangled with a needle punch or water punch or the like, and nonwoven fabrics in which mature bonding is used in combination are also included.

Next, a non-woven fabric made of three-dimensional mesh fiber with excellent uniformity (H) It will be described.

As described above, the nonwoven fabric according to the present invention belonging to the category is a nonwoven fabric in which spread three-dimensional mesh fibers are deposited in random directions, and is a bundle present in the mesh fabric constituting the nonwoven fabric. If the shape is a bundle having a density of 40 denier or less, or a bundle having a density of 40 denier mm or more, the width is 5 ™ or less and the length is It must be a bundle of 30 or less.

The present inventors have found that when the opened three-dimensional mesh fabric constituting the nonwoven fabric does not have a specific opening defect portion, the nonwoven fabric becomes a very uniform nonwoven fabric in terms of appearance and weight distribution, A non-woven fabric belonging to the classification ox by Kakimoto Kamoto of the keen study was obtained.

This specific unwoven area is defined as a three-dimensional net-woven fiber that has been unwound after flash spinning, which has been condensed during the sheeting process and has a width of 40 denier-mm. It is a bundle that has been bundled to a fiber density or higher and has a width of 5 mm or more and a length of 30 nm or more. The bundle portion means a bundle formed by fibrils of the entire three-dimensional network fiber and a bundle formed by consolidating a part of the fibrils of the three-dimensional network fiber. The fiber density was determined by taking continuous fibers having a length of 2 on or more for about 100 cm in length, measuring the spread width every 2 cm, and dividing the weave degree by the spread width.

Such a nonwoven fabric made of an opened three-dimensional net-like fiber having no specific opening defect portion is a sheet width variation rate of the sheet expressing the macroscopic uniformity of the nonwoven fabric ( R) is 0.3 or less, and a laser spot expressing microscopic uniformity of the nonwoven fabric. It is more preferable that the transmission light quantity change rate of the incident light is 0.5 or less. Dropping such conditions can provide a very uniform illusion. The bulk variation rate (R) and the transmitted light quantity variation rate are defined as follows.

Weight per unit change = R Z

The basis weight Xi was measured with a 1 cm II X 5 cm long sample, and the average value was obtained.

X-. ∑ X i / α (η: 30 or more by Kiyoshi constant),

R = _{X ma} X - is calculated by using the X m _in. Percentage change in transmitted light = r χ / '(basis weight) / 50 Measure the transmitted light of laser-spot light (spot diameter: 2.5 ø ø) in the width direction of the sheet, and average it. = ∑ yi / n. (Where n is the number of measurements or more) and ry _max -y. -/ (Basis weight) / 50 is a coefficient for correcting the posterior sensitivity of the convergence portion of the reticulated fiber in the non-woven fabric, which changes depending on the difference in the average g per unit area. This correction is due to the fact that the amount of laser transmission changes with the square root of the rate of change in the weight of the nonwoven fabric as the basis weight increases.

Thus, the nonwoven fabric belonging to the classification JL according to the present invention is a macroscopically and microscopically uniform nonwoven fabric.

In other words, in this nonwoven fabric, the unwoven fabric constituting the nonwoven fabric does not form a bundle having a width of 50 mm or more and a length of 30 or more, which is focused to a fiber density of 40 denier dish width. However, such a nonwoven fabric having a high uniformity has not been known so far, and the nonwoven fabric according to the present invention employs the nonwoven fabric according to the flash spinning method, which is the first to achieve the uniformity. A three-dimensional reticulated fabric is obtained.

Further, in the uniform nonwoven fabric of the present invention, the opened high-density polyethylene-based three-dimensional network fiber constituted by the nonwoven fabric has a long-period scattering intensity ratio of 40 or less and a long-period of 150 A or more. As described above in detail, a nonwoven fabric with high strength, high thermal nucleus properties, high opacity, and high covering power, which has never been seen before, is excellent in uniformity.

The nonwoven fabric belonging to the classification day obtained in this way can be applied to applications such as filter fields using the high degree of uniformity.

Next, a method (2) for producing a nonwoven fabric having excellent uniformity belonging to the classification and description will be described.

'' The manufacturing method belonging to the classification _L includes: a rotatable disk portion; a cylindrical portion extending vertically from the center of the disk portion and having a circular outer surface having a diameter smaller than that of the disk portion; It comprises a scart portion that is inclined and disposed in a space between one surface and the circular outer surface of the cylindrical portion, and the force seat portion has a direction substantially parallel to the eclipse line of the cylindrical portion. A plurality of oscillating surfaces for oscillating unopened three-dimensional net-like iron fibers flying in the direction, and a oscillating direction of the three-dimensional net-like fiber arranged alternately with the oscillating surface and oscillated by the oscillating surface. This is a method for manufacturing a nonwoven reticulated fiber nonwoven fabric using diffusion and oscillating rotational dispersion of three-dimensional reticulated iron constituted by a cushioning surface that alleviates a sudden change in the oscillating surface. The inclination angle between the center of the disk and the upper surface of the disk is the angle between the center of the collision surface and the upper surface of the disk. The angle of inclination is approximately equal to the angle of inclination ^ and the cushioning surface is near the cylindrical part The feature is to use the diffusion / oscillating rotation dispersion of three-dimensional mesh dog fabric, which has a fan-shaped shape whose width near the disk is wider than the width of the disk.

The range in which the inclination angle is substantially equal to the inclination angle means rr = β ± ή.

Hereinafter, the present production method will be described based on an example of a strenuous method for producing a nonwoven fabric of the present invention belonging to Class I.

Originally, three-dimensional meshed steel by the flash spinning method, unlike the normal spanbond method consisting of individual spun fibers, the steel fibers connected in a mesh pattern were opened and dispersed. It is difficult to obtain a uniform dispute because it must be done.

The present inventors have developed a high-speed photographing device tf '(a stobovision ionizer manufactured by Sugawara Laboratories) to elucidate the cause of the non-uniformity existing in this nonwoven fabric. · Using 1), the state of the three-dimensional network of the dispersal part was tracked by a 130,000 abstract photo. The preferred open IS dispersion technology is a high-speed rotation.This method is based on the high-speed production of non-woven fabrics because the method of colliding undistributed three-dimensional mesh fibers against the dispersion plate and dispersing the open fabric is left behind. The method was used.

As a result of the above observation, the largest cause of uneven opening of the synthetic fibers in the non-woven sheet by the flash spinning method is the most unusual reason. Since the three-dimensional filamentary fiber made by the flash spinning method has a continuous three-dimensional net-like structure, it can be easily opened with a slight tension acting on the textile even after it has been opened. It has the property of being focused on a bundle of several millimeters wide. In other words, according to the knowledge of the present inventors, it is clear that When the protruded and widened three-dimensional mesh fabric travels in the space region between the rotation dispersion plate and the hub area, tension is generated in the fabric due to viscous resistance with the surrounding air. This tension has the effect of reducing the width of the expanded three-dimensional braided mesh. In addition, the three-dimensional mesh fiber impinged on the rotating dispersing plate, when traveling in the spatial region between the rotating dispersing plate and the web collecting surface, changes the swing direction of the three-dimensional mesh fiber. When the water occurs in the space above the collecting surface, the forward speed toward the Ura collecting surface is reduced, and it falls as if it were floating in space. In this state, it was confirmed that the three-dimensional mesh fabric had a small opening width, was easily affected by external factors, for example, the surrounding airflow, and was easily converged into a bundle. .

When the tube including such a bundle portion is made non-woven by appropriate thermal bonding, it has an uneven appearance in which a portion having a high fiber density and a portion having a low fiber density are mixed, and The spots are extremely large.

In view of the foregoing, the present inventors have conducted intensive studies in order to obtain uniformity-added ignorance, and have arrived at a manufacturing method belonging to the above-described configuration classification.

In addition, it is preferable to use a diffusing and oscillating dispersion plate in which the oscillating surface constituting the scart portion is substantially flat, and the collision surface is a substantially convex curved surface, and more preferably. The distance between the bottom of the rotating dispersion plate and the open surface of the opened three-dimensional mesh fiber is set to be equal to or less than the distance between the bottom of the rotating dispersion plate and the point where the swing direction of the three-dimensional mesh fiber changes. Combine things.

The three-dimensional net shape. It refers to the point at which a two-dimensional network fiber that is reciprocated in a direction substantially orthogonal to the axis of the cylindrical portion of the rotation dispersing plate is turned by a change in the direction of movement.

The O distance between the lowermost part of the rotating dispersion plate and the collecting surface of the three-dimensional net-like fiber is determined by the amount of solution discharged per spindle of the spinning nozzle and the positional relationship between the spinning nozzle and the rotating dispersion plate. It should be less than the distance between the bottom of the tillage dispersion plate and the swing change point of the net-like debris. Good. Confirmation of距難of this' is, ^ serial high-speed image capturing device by 1 Z 3 X 10 ⁵ Extract of the moment de be done by observing with a photograph - kill.

The rotating dispersion plate according to the present invention is such that the three-dimensional net-like fiber is guided on the surface of the ura while maintaining the shape of the three-dimensional steel fiber which has been sufficiently widened and opened. The high-speed fluid and the three-dimensional mesh fiber that have been ejected from the nozzle are widened and opened by a fan having the same width regardless of whether they collide with the swinging part or the buffer part in the skirt. The falling speed in the direction is almost constant, and the widened open-woven three-dimensional reticulated steel is guided on the surface of the ura without generating tension to converge it. Of course, the fluid ejected from the nozzle scatters in the atmosphere when it collides with the rotating dispersion plate, but most of the fluid conceals leading the three-dimensional mesh fabric to the collection surface.

In the case of using the rotating dispersion plate according to the present invention, regardless of the dispersion conditions, the width of the unwoven woven fabric constituting the nonwoven fabric converged to a fiber density of 40 denier m or more is 5 or more. To obtain a non-woven fabric having a length of 30 mm or more and containing no bundle. Further, the distance between the rotational dispersion plate according to the present invention and the rotational dispersion 扳 the bottom and the opened three-dimensional net-like weir surface is increased by the rotational dispersion 勛 the oscillation of the bottom part and the three-dimensional net-like fabric. The three-dimensional mesh fiber constituting the nonwoven fabric obtained by combining the setting with the distance not more than the distance between the direction changing point does not include the above-mentioned bundled capital, and the width is not limited. It was almost constant over the entire area of the fabric.

These nonwoven fabrics were extremely uniform in that the basis weight variation in the width direction was 0.3 or less and the variation in the amount of transmitted laser light in the '† i direction' was 0.5 or less. .

Such a uniform nonwoven fabric is not limited in terms of basis weight in terms of the production principle, but is usually useful having an average basis weight of 5 to 500 g Zm ² (preferably 15 to 300 g). Such a uniform non-woven fabric can be used to expand the range of use as a non-woven fabric of a flash-spun reticulated fiber which has excellent characteristics as a special fiber. Something is immeasurable. A preferred example of the production of the non-woven fabric comprising the three-dimensional mesh fiber of the present invention belonging to the category I will be described in detail with reference to the accompanying drawings.

In FIGS. 13, 14 (a) and 14 (b), reference numeral 32 denotes a cylindrical projection, which is a part of the three-dimensional reticulated fiber colliding with the skirt part 33 and the high-speed airflow. It serves to prevent blow-up.

Reference numeral 3 denotes a disk, which controls the traveling direction of the three-dimensional net-shaped beam deflected by the skirt portion 33. The skirt portion 33 swings the widened open weave three-dimensional net-like fiber for widening and weaving the three-dimensional net-like fibre.

The swinging surface 3 4 and the cushioning surface 3 5 are alternately arranged in the scar section 33. In general, 2 to 5 rocking surfaces 34 are arranged.

It is preferable that the oscillating surface S 4 is formed substantially in a flat shape, and the collision surface 35 is formed substantially in a convex curved shape. The oscillating surface 34 is substantially flat if the intersection line 37 between the oscillating surface 34 and the disk surface is almost straight as shown in Fig. 14 (a). means. As long as the three-dimensional mesh key is smoothly swung, the intersection line 37 'may be a curved surface having an extremely gentle curvature, that is, a concave surface or a convex surface. The contact surface between the oscillating surface 34 and the cushioning surface 35 is designed so that the shape of the cushioning surface 35 that comes into contact with the disk has a fan shape whose width near the disk is wider than that near the cylinder. It is preferable that an end shape is formed.

A buffer surface 35 is substantially convex curved surface, the high seat Y ₂ of intersection of the cylindrical portion 3 2 represented by the 1 4 (b) Fig means that the conical curved surface is constant . Slow: Polyhedral surface consisting of a flat surface or several flat surfaces may be used as long as it can maintain the role of the opposing surface.

It is also possible that the connection between the rocking surface 34 and the cushioning surface 35 with the side surface of the cylindrical portion 32 and the connection with the upper surface of the disk portion 31 may be made smoothly with a curvature. Of course.

The inclination angle between the swing surface 34 of the skirt portion 33 and the surface of the circle Μ 31 shown in FIG. L4 (b) is the angle between the cushioning surface 3 δ and the surface of the circle 盩 31. It is important that a = β, preferably a = β, to achieve the enormousness of the present invention. If this relationship is satisfied, the contact surface 3 5 The width near the disc 31 is wider than the scorpion near the fan. As disclosed in SP3, 497, 918, the contact surface 35 has a wedge shape in which the width near the disk portion 31 is narrower than the width near the cylindrical portion 32. When taking, the swing part 34 4 Θ ί Θ ί ί 斜谖谖谖谖谖部部 3 5 5 5 5 5 5 5 ^ ^ ^ ^ 、、、、、、、 The structure is inevitably smaller than the inclination angle of 34. The effect of this rotating dispersion plate on the three-dimensional network is shown in Fig. I8.

The inclination angle is preferably in the range of 30 ° to 60 °, and is selected according to the relationship between the discharge flow rate and the desired tube width. When the angle of inclination is large, the momentum lost by collision with the three-dimensional mesh fiber and the high-speed fluid is reduced, so the three-dimensional mesh is large and the momentum that guides the fiber to the collection surface is large. It will be a web.

The shape of the oscillating surface 3 and the buffer surface 35 of the rotary dispersion plate, X shown in the first 1 4 (b) Fig.,, Y,, X z, in the length and the 1 4 (a) FIG Y ₂ If the distribution center angles r and 7? Of the indicated shaking surface 34 are determined, they are automatically determined. In addition, the relation between X ′, Y «and Χ ₂ , Υ ₂ is determined by the relationship between the inclination angle“ and ^.

As shown in Fig. I5, the unspread three-dimensional reticulated fiber 26 ejected from the nozzle 24 together with the high-speed fluid is a rotating dispersion plate provided near the tip of the nozzle 24. The cloth is widened and collides with the scat part 33 to change the traveling direction of the three-dimensional net-like fiber. The three-dimensional reticulated weave oscillating surface 34 and the contact surface 35 constituting the skirt portion 33 are arranged so as to be inclined with respect to the axis of the nozzle 25. Further, as shown in FIG. 15, the corona discharge device 27 and the like arranged downstream of the rotating dispersion plate immediately after being ejected from the rotating dispersion plate on the widened and opened three-dimensional mesh fiber. It is preferable to apply the tertiary layer, since the silk-like fiber can be uniformly opened and a more uniform non-woven web can be obtained. Since the degree of widening and weaving of the original reticulated fiber is temporally uniform, the state of dispersion by static electricity obtained by the corner discharge device S can be made extremely uniform. Since the three-dimensional network steel can be stably deposited on the surface of the ura collection surface, the turbulence of the web due to the air current on the ura collection surface is suppressed, and the uniformity of the nonwoven web is further improved. be able to.

Figures 16 (a) to 16 (d) 、 are the high-speed rotating books. The rotating dispersion plate according to the present invention is installed at a distance where the swing change point of the mesh fabric is on the ft collecting surface. 5 is a schematic view of the state of action on a three-dimensional reticulated fiber observed by the high-speed imaging apparatus described above.

Rotational dispersion 、 was performed at a speed of 10 to 3000 rpm using a Z axis shown in Fig. 15 as the axis of rotation using a 200 W servomotor. The actual HI number of the three-dimensional silk fiber was 300 to 900. Speed.

FIG. 16 (a) shows a state in which the three-dimensional netted fabric colliding with the central portion of the oscillating surface 34 is falling almost in the vertical direction while widening on the rotational dispersion. Fig. 16 (b) shows the three-dimensional network that swelled about 50 'from the figure in Fig. 16 (a) and collides with the swinging surface of the rotation dispersion plate. Indicates a state in which the width is widened and falls diagonally to the left on the surface. Fig. 16 (c) is from Fig. 16 (b). Furthermore, the three-dimensional mesh fiber that has been rotated about 10 ° and colliding with the buffer surface 35 O of the rotating dispersion plate 30 is falling almost vertically while widening on the rotating dispersion plate. Is shown. Fig. 16 (d) shows that the three-dimensional mesh fiber rotated about 10 ° more than Fig. 16 (c) and collided with the left end of the oscillating surface 34 of the rotating dispersion plate was rotated and dispersed. This shows a state in which it is expanding on the board and falling in the right-upward direction on the drawing. As shown in Fig. 16 (a) to Fig. 16 (d), the three-dimensional mesh fiber that collided with the rotating dispersion plate is widened in a fan-like shape, and the scat section starts from the fiber collision point 39. Intersection line between 3 3 and the upper surface of the disk portion 3 1 (intersection line 37 between the swinging surface 34 and the upper surface of the disk portion 31 or the cushioning surface 35 and the upper surface of the circular portion 3 1 In the direction perpendicular to the intersection line 38), the widening is maintained while maintaining the three-dimensional net-like fiber shape, and is guided along with the fluid onto the ura collection surface 3.6.

Figs. 16 (a), 16 (b) and L6 (d) show the falling state of the three-dimensional reticulated fiber after impact on the revolving surface 34 of the rotating dispersion plate. Comparing the figure with Fig. 16 (c), which shows the falling state of the three-dimensional net-like steel after the collision with the buffer surface 35, the widening open state of the three-dimensional net-like fiber is shown on the Ura converging surface 36. It is confirmed that they are almost the same until they are derived. In addition, there is no unevenness of spreading, no partial focusing of three-dimensional net-like steel fibers, and no buckling in the air. In other words, even during the high-speed rotation of the rotation dispersion, the width of the three-dimensional mesh fiber is increased without changing the position of the collision point, and the traveling three-dimensional mesh fiber is uniformly collected on the collecting surface. Leading to.

FIGS. 18 (a) to 18 (d) show wedge-shaped cushioning surfaces disclosed in FIGS. 3 and 4 of US Pat. No. 3,497,918. 16 (a) to 16 (d) are schematic views showing the effect of the rotating dispersion plate on the three-dimensional network fiber by the same method as in FIGS. 16 (a) to 16 (d).

The stationary positions of the rotational dispersion plates in FIGS. 18 (a) to I8 (d) correspond to FIGS. 16 (a) to 16 (d) _; {l, respectively.

Compared with the widened open steel width H 1 of the three-dimensional mesh fiber that collided with the rocking surface 34 shown in FIGS. 18 (a), 18 (b), and 18 (d), 8 (c) It was confirmed that the width H2 of the three-dimensional mesh fiber colliding with the buffer surface 35 shown in the figure was about 1.5 to 2 mm, and the openability was improved. It is uneven.

As observed, as the width of the three-dimensional network fiber widens, the tension generated in the falling traveling three-dimensional network fiber changes pulsatingly during rotation of the rotating and dispersing plate. As shown in Fig. 8 (a), Fig.-18 (b) and Fig. 18 (d), it is confirmed that the widened three-dimensional network induces the @@ and the partial convergence of the key fiber. Is done.

Fig. 17 (a) II to Fig. 17 (d) show that the rotation dispersion plate according to the present invention was placed at a distance where the swaying change point of the three-dimensional Aboshi steel was above the Ura junction. Fig. 16 (a) to 16 (d) are schematic diagrams showing the effects on the three-dimensional silk-like steel in the same case as those shown in Figs. 16 (a) to 16 (d).

The stationary positions of the rotational dispersion plates in FIGS. 17 (a) to 17 (d) correspond to FIGS. I6 (a) to 16 (d), respectively.

As shown in Fig. 17 (a) to Fig. 17 (d), when the swing change point © of the three-dimensional reticulated steel occurs above the trapping surface, the drop after the swing change point The width H 3 of the widened weave of the three-dimensional reticulated fabric is larger than the width H 2 of the three-dimensional reticulated weave above the point of oscillation This was confirmed.

In addition, the three-dimensional reticulated fiber falling after the swing change point is in a floating state with a slow falling speed as shown in the region in the figure. This O floating three-dimensional network襪維is, external factors, for example, outside of the influence the susceptibility rather維密degree 4 0 denier / ^/ «Ri by width is small but produces a © part focused slight tendency of the airflow is there.

Hereinafter, the present invention will be described in more detail with reference to various experimental examples of the present invention.

11 Example 1

Flash spinning of high-density polyethylene was carried out using the flow sheet shown in Fig. 1Q.

The shape of the extruder and the mechanical mixing device attached to the screw are schematically shown in FIG.

When the dimensions of each part are shown, the screw size is 35 ø in diameter, and the length of the lined part / depth = 3 15 no 5 Compressed part length / depth = 3 15 «/ 5-→ 1.6 mm. The length / depth of the measuring section is 245 / 1.6. The shape of the damaging part is a multi-thread screw made of steel, the length is 210 mm, the diameter is about 50 ø, the screw used is 16 threads, it has a semicircular groove, the groove depth 3 _; 6 (maximum), the twist angle is .35 ° right. Furthermore, the shape of the pin mixing section is a multi-row array of cylindrical pins, the pin arrangement is 8 × 17 rows, the size is 285, and the diameter is about 50 °. In this pin mixing section, pins of the same shape are also planted in the same row of 8 i7 rows on the barrel side, as in the case of planting the pins on the axis coaxial with the screw. When the key rotates, the movable pin on the same axis as the screw moves between the fixed pins. The polymer and solvent are mixed. The gap between the barrel and the movable pin shaft is 5-1

Five

86. In addition, they have a static mixing section indicated by reference numeral 9 in FIG. 10. The static mixing element used is a mixer SMX type (nominal diameter 15 ™) manufactured by Sulzer. For example, metal pieces are welded in parallel, and they are connected at an angle of 90 °. This was used in 50 stages.

Each mixing unit is provided with a solvent injection port, each of which is connected to a double plunger pump. A spinning device indicated by reference numeral 7 in FIG. 10 was attached to the end of the extruding / dissolving device.糸 The yarn device is equipped with a filter for filtration and a 0.6-5 L decompression filter.

10 reefs, about 2 cc pressure chamber, 0.55, 0, 55 L holes and it

It was a combination of yarn yarns with 3 mm 3 L of tunnel flares. *.

The polymer was supplied and high-density polyethylene (ΜI = 0.31 M „/ Ma = 4.8, density 0.960 g / cii) was supplied from the extruder's * paper; Then, supply the same amount of Fluor--11 from the two metering pumps, and set the poly concentration to 12.0 wt% at a polymer flow rate of 8.8 kg / Hr. The pressure was 350 kg / (^, indicating that the pressure was llOK Z crf at room temperature 19 and therefore the pressure difference before and after the pressure relief was 240 kg Z crf. The conditions were in the liquid phase region, and as a result, a three-dimensional net-like fabric of pure white, which was more highly spun than the spinning nozzle, was discharged.

This fiber has a density of 112 d, a specific surface area of 48 niZg, and a long period due to small-angle X-ray scattering. The scattering intensity ratio was 6. The initial modulus was 40.3 g / d and the breaking strength was 9.5 gd in the tensile test with 4 burns of Z cm.

In addition, the elongation rate at 130 in TMA is 1.5%, and the dynamic viscoelastic modulus in 、, イ is 1 O: ¹ . a dynZcrf temperature 123 ° C, the crystal fraction diverging of tan ^5: starting temperature of Tsu der Te 127.

The orientation angle by X-ray diffraction is 16 °, and the orientation coefficient F by infrared absorption dichroism at a wave number of 201 cm- ¹ . ² ° showed a value of 0.50. Microwave birefringence was 0.149.

In this case, iI was 0.35 Mw / Mn = 4.6.

Example 2

77.7 g of high-density polyethylene (Mί = 0.3i Mw / Μ „= 4.3 density 0.960 g / cm ³ ) was added to an experimental high-pressure autoclave with a volume of about 500 cc. Add 570 g of Fluorine-11, and heat under pressure while stirring to dissolve to create a solution with a polymer concentration of 12 wt%. After adjusting the temperature of the solution to 185 and stopping stirring, immediately apply back pressure to keep the inside of the autoclave at 295 kg / cni G. Open the bottom valve that connects the spout assembly. At this time, the tip assembly was equipped with a 0.4 ø5 ™ L decompression orifice, a decompression chamber of about 2 cc, and The spinning nozzle had a hole of 0.5 mm ø 0.5 L and a 3 ma 3 3 mm L of tunnel flares.

During spinning, the pressure in the decompression chamber was 105 kg Z Cm ² and the temperature was 185 ° _C.

Highly fibrillated continuous three-dimensional net Fushiori I was obtained.

This fiber had an intensity of 85 d and a specific surface area of 40 crf Zg. The long period due to small-angle X-ray scattering was 168 A, and the scattering intensity ratio due to long period was 7.2. .

In the tensile test at αιι, the initial modulus was 367 g i and the shear strength was ί] .0 g d.

In this experiment, the phase diagram of the used high-density polyethylene and a 12 wt% solution of Fluorine-11 is shown in Fig. 1, where point A is inside the autoclave and point A is inside the pressure chamber. Indicated by B, due to high pressure differential-spinning from liquid phase region. -Comparison Kiyoshi 1

Using the same raw material as in Experimental Example 2, flash spinning was performed from a solution having the same polymer concentration of 12. In this spin-assembly 'J-, a decompression chamber and a spinning nozzle were used in Experimental Example 2. The same as above, but a 0.5 mm ø, 5 thigh L pressure orifice was used, and the solution temperature was the same as 185, but the pressure inside the autoclave was 120 kg. / an

At this time, the temperature in the decompression chamber was -184 ° C, and the pressure was 70 / G.

Although a silk-like fiber having an iron degree of 77 d was obtained, the fibril was thicker than the experimental example, and the specific surface area was 20 nf / g.

Further, the number of twists was 4 times, and the tensile modulus was 18 g nod and the elongation at break was 4.3 g / d in a tensile test with Z cni.

In this example, the positions on the phase diagram in the autoclave and the pressure chamber are-the points indicated by points C and D in Fig. 1, respectively. You.

Experiment ί Row 3

Using the dissolving apparatus of Experimental Example 1, the high-density polystyrene was changed to -Vi ί = 0.73, Μ „Μ„ = 3.0, and the density was 0.962 g /. % Of a fluoro-11 solution was prepared and spun. However, at this time, the decompression orifice is 0.6 raø, 5 ™ L, the spinning nozzle is 0.5 mφ, and the hole of 0.5 L is 4 ø, 4 mL. A spinner assembly consisting of a Tunnel Flare was used.

At a polymer flow rate of 7.4 kg / hr, from the solution pressure of 270 kg / cni G to the decompression chamber pressure of 98 kg / cni G (temperature 186'c), the knowledge discharged from the spinning nozzle Was a pure white continuous three-dimensional reticulated weave with a weave of 106 d. The conditions in the decompression chamber are within one liquid phase region.

This fiber has a specific surface area of 38 frf no g: and has an initial modulus of 33 g / (1, breaking strength 7.9 The values of g and d are shown.

The small-angle X-ray scattering of this fiber showed that the long period was 175 A and the long period scattering intensity ratio was 15.0.

TA 130. elongation at c 1. Ri 5% der, Bruno, 'Lee Bro emissions dynamic modulus 1 0 ^1. The temperature at which dyn / cm 'was reached was 120, and the crystal dispersion starting temperature of tan 5 was 124 ° C.

The orientation angle of this fiber by X-ray diffraction is 20 °, and the orientation coefficient F in the infrared. ² ° was 0.53, indicating high orientation.

In this case, the Ml of the fiber was 0.93 and _Mw / M „= 6.3. Experiment 4

A homogeneous solution having a polymer concentration of 9.2 wt% was prepared by circling the same apparatus and the same solvent as in Experimental Example 1, and a 0.55 mm and δ mmL dependent pressure orifice was prepared. Flash spinning was carried out using a mouth assembly consisting of a spinning nozzle having a hole of 55 mΦ, 0.55 L and a 3 ML. 3 thigh L tunnel tunnel.

At 7.5 kg / Hr, the solution showed a temperature of 131 ° C and a pressure of '325 kg./oi G, and in a pressurized chamber, the temperature changed to 191 and the pressure changed to 110 ° o4 G, and then spun. The mixture was discharged from the nozzle into the atmospheric pressure to obtain a pure white continuous three-dimensional reticulated fiber with a filth of 101 d.

With this knowledge, the specific surface area was 4 JL m / g.

The long period due to small-angle X-ray scattering was 162 A, and the scattering intensity ratio due to the long-term period was 8.4. '

Go to the tensile test with the number of repetitions of 4 at Z: cm. The initial modulus was 38.5 g / d and the breaking strength was 9.3 g Zd.

Further, 13 (in Tc 'extension ratio of 1, 5%, temperature dynamic elastic modulus at by Bro emissions is ¹ 0 1. Η / αί is 122' at T eight C. Tan [delta] of the crystal dispersion Starting temperature is 126

X-ray diffraction shows an orientation angle of 13 'and an orientation coefficient F ° of 0.43 due to infrared absorption dichroism at wavenumber 2017 OR-.

The number of microwaves is 0.147.

This O維was _{MI = 0.34. "/ M Λ} = 4. 8.

Experimental example 5

Using the same dissolution apparatus and spinning assembly as in Experimental Example 1, the high-density polyethylene was converted to MI = 0.78. M _w / _n = 8.0, The solution was changed to 0.962 g / crf, and a 12.4 wt% solution of Fluorine-11 was prepared and spun.

At a flow rate of 9.7 kg / Hr, the solution pressure is reduced from 210 kg / oi G to 210 kg / oi G. The room pressure is changed to 33 kg Zen! G (decompression room temperature 190) and discharged from the spinning nozzle. A series of three-dimensional networks of d.

This fiber had a specific surface area of 33 m / _g .

The long period of X-ray small angle scattering was 173, and the ratio of the scattering intensity due to the long period was 19.2.

In the tensile test with four burns, the initial modulus was 23.6 g / d, the breaking strength was 7.4 gd, and the elongation at 130'c in the TMA measurement was 1.7%, dynamic in neutron "C: elastic modulus is 10 '. The temperature to become dyn's cn! Is 116, and the crystal dispersion starting temperature of tan (? Is as high as 124'c Has characteristics.

The crystal orientation angle by X-ray diffraction is 27 °, and the infrared orientation coefficient F ^ at a wave number of 20ί7 cm- '. Is 0.51. Microwave birefringence showed a value of 0.133.

In addition, this spun fiber was measured as _Mw / „= 6.0 at Ml = 0.94.

Compare f column 2

Using the dissolving apparatus of Experimental Example 1, fluorocarbon with high density polyethylene (Ml = 5.0, „/ M„ = 7.0, density 0.969 g / c) was used. % Solution was prepared and spun. At this time, Use a 7 ™ 5 mm L thread weft nozzle with a 0.7-ma 0.7-mL hole and a 4 4 4 L sponge assembly with a 4 mm tunnel hole. Was.

At a polymer flow rate of 8.8 kg ZHr, the solution pressure of 130 kg / dG dropped to a decompression chamber pressure of 53 kg / G (temperature of 173 ° C) .From the spinning nozzle, a continuous three-dimensional with a weave of 157 d was obtained. Reticulated. Weave was obtained. The conditions of the pressure chamber were stirring in the two liquid phase region.

This textile has a specific surface area of 18 m ² / g, an initial modulus of 10.8 g d in a tensile test of 4 times of burning '· / on, and a shear strength of 3.8 g d It was only. .

In the measurement of small-angle X-ray scattering, the long period was 133 A and the scattering intensity ratio was 52.4.

The elongation at 130 by TMA was' 3.6%, and the crystal dispersion starting temperature of tan δ in Viselon at 113 c was inferior in thermal properties.

Next, this steel was stretched about twice while twisting 4 cm on a hot plate ripened to 120 V.

In the tensile test, this hot-stretched fiber had an initial modulus of 19.2 g Zd and a breaking strength of 10.1 g Zd, but the yarn became transparent and the specific surface area decreased to 9.1 of / g. .

The long-period in X-ray small-angle scattering was shifted to 235, and the scattering intensity ratio was increased to 90.

Experimental example 6.

According to the flow chart shown in FIG. 5, a method using the extruder screw 2 shown in FIG. 6 (hereinafter referred to as method A) and FIG. Was A flash-spun at law using an extruder scan click Li Interview first and special mixing structure shown in (called hereinafter A ₂ method).

The extruder shown in FIG. 5 has a barrel diameter of 35 ø, and the screw used for the method is described using the reference numeral in FIG. 1 6 «™ (9 peaks), groove depth about 5 Compressed section length of code 1 3 245 7 peaks), code 1 40 front quantification section length 1 40 (4 peaks), groove depth 1.6 The length of the solvent addition section of symbol 15 is 0 ram (two peaks), the groove depth 3 The length of the rear measurement section (mixing / melting part) of symbol 16 is 140 ™ (four threads) ) The groove depth is 1.6. A screen 'device was attached to the tip of this extruder, and a spinning device was attached via piping. The orifice diameter of the decompression chamber of the spinning device is 0.5 ø, the volume of the decompression chamber is about 2 cc, and the diameter of the spinning orifice is 0.5. ―

The co-feeding of the solvent in the extruder was performed through an inlet 18 using a double-junction pump.

Main: NetBackup Lee emissions de click scan (- [mu] I) is 5.0 (weight average molecular weight of about 9 X 1 0 ⁴⁾ dense potentiation Re ethylene les down the (manufactured by Asahi Kasei Corporation Sa integrators click J one 240) The spinning was carried out using a polymer solution having a polymer concentration of 11-11% by weight of fluorocarbon. That is, the extruder was operated at a barrel temperature of 230, a screw rotation speed of 50 rpni, a polymer flow of 77 gZ, and a solvent flow of 623 g. . The heating temperature of the piping and the spinning device after the tip of the extruder was 175, and the heating temperature of the solvent was 100 ° C. At this time, the liquid temperature immediately before spinning was 175'c, and the pressure in the compression chamber was about 40 NOG. The spinning state is extremely stable, and the pressure fluctuation in the decompression chamber is 45 kg / cm ♦ G ₀

The pressure at the tip of the extruder was about 200 kg / cii-G, but no leakage occurred from anywhere. In addition, although a hollow metal 0 ring was used for the seal of the flange portion, no leakage of the solution occurred. -.

If the discharge volume is further increased and brought up to the polymer flow rate of llOg Z and the solvent flow rate of 890 g Z, the pressure fluctuation width of the pressure chamber becomes extremely large, and the value also becomes 1 (3 kg / cii Beyond G, practically stable spinning became difficult.

Then went the spinning of the A _z method. The shape of the special mechanical mixing section used is shown modelly in FIG. · If the dimensions of each part are shown, the screw size is as follows: feed part length / depth = 315 no 5 thigh, compression part length Z depth = 315 no 5 → 1. & 丽/ Depth-245 m / 1.6 thighs. The shape of the dal image is a multi-threaded screw structure, the length is 210 »m, the diameter is about 50 thighs, the screw used is 16 threads, it has a semicircular shape, and the groove depth is 3 6 mm (max), right torsion angle

35 degrees. Furthermore, the shape of the pin mixing section is a multi-row structure of P3 cylindrical pins, with a length of 285 plates, a diameter of about 50 dragons, and 8 pins and 17 rows if the pins are arranged. In the pin mixing section, pins of the same shape are planted on the barrel side in the same eighteen and seventeen rows, as in the case of planting the pins on the shaft on the same section as the screw. When the is rotated, the movable pin on the same surface as the screw moves between the fixed pins, and the polymer and the tether are mixed. Roh barrel and between clearance of the movable pin eclipse is a ί books'. _0.

Flash spinning was performed under exactly the same method and conditions as the t method. ^ Spinning was extremely stable even when the discharge amount was 1000 g, that is, the polymer flow rate was llO g Z, and the solvent flow rate was 890 g / min. At this time, the pressure in the decompression chamber was 55 kg / crf-G, and the fluctuation range of the pressure was 4 to 5 kgcm · G.

The pressure at the tip of the extruder was about 250 kg / crf'G, and there was no leakage of the agent from anywhere.

Experimental example 7

Flash spinning using the method shown in Fig. 9 (hereinafter referred to as method B)

9

Five

Was done. That is, through the pipe to the next the A ₂ Method of scan click Li Yu over press extruder described in Example 6, was placed a mixed system consisting of the static mixed-element corresponding to the code 9 of FIG. 9. The static mixing element used was a mixer SMX type manufactured by Sulzer (nominal diameter 15 dragon ø), in which the metal strips were welded in a cross-girder shape, and they were shifted 90 °. Are linked. This was used in 50 stages.

Is a spinning method, main Le preparative Lee emissions de click scan is 1.2 (weight average molecular weight of about 14 ^104), high density poly ethylene les emissions (manufactured by Asahi Kasei Corporation Sante click B - 161) and off A polymer solution consisting of lon-111 was used. The temperature of the screw extruder is 230, the temperature of the special mixing section of the A3 method is 200 ° c. The temperature of the piping and static mixing section is 175, and the polymer concentration is 11 weight. %. Spinning at a flow rate of 77 g / min, a flow rate of 623 g / min, and a total discharge of 700 g / min, the liquid temperature immediately before spinning is 175, and the pressure in the decompression chamber is 70 kg / d. -G. The spinning state was extremely stable, and the pressure variation in the decompression chamber was also 2 to 3 kg / cm ² · G. Experiment M8-Flash spinning was performed by the method shown in Fig. 1 (hereinafter referred to as Method C). That is, according to the method described in Experimental Example 7, a solvent injection port was provided between the tip of the extruder section and the static mixing section 9 and connected to a double blower pump. Therefore, the polymer melted by the extruder reaches the polymer dissolution zone. A solvent is added to this region from a pranjar pump, and the polymer and the solvent are mixed in the special mixing section 8 to dissolve the polymer. Further, the mixed solution reaches the static mixing zone from the extruder tip. During this time, a solvent is further added. This polymer / solvent mixture leads to a static mixture, which is discharged from the outlet as a completely uniform polymer solution for mixing-dissolution.

-High index polystyrene (Suntec S-160 manufactured by Asahi Kasei Corporation) with a melt index of 0.78 (weight average molecular weight of about 16 x 10 ⁴ ) The spinning was carried out using a polymer solution having a polymer concentration of 1 and a solid density of 1. The spinning section was performed at an extruder temperature of 270, a special mixing section temperature of 200, and a static mixing section temperature of 175. The pressure was set to 5 ^s C. The pressure chamber nozzle was 0.5 mm, the decompression chamber volume was 2 cc, and the spinning nozzle was 0.5 mø. The mixture was mixed and dissolved at a static mixing unit pressure of 200 _kff / oi · G. The liquid temperature immediately before spinning was 1 to 5. (: The pressure in the pressure chamber was extremely stable at 80 kg / αί * G. The pressure fluctuation in the pressure chamber was 2-3 / era ·.

What is the polymer flow rate at this time? At 7 minutes, the solvent flow rate was 623 g Z minute, and the solvent was added directly to the first stage special mixing section. The addition amount in the previous step was 77 g, and the remaining solvent flow rate of 546 g / min was added immediately before the static mixing section in the second stage. Therefore, the first stage has a polymer concentration of 50 wt% and the second stage has a concentration of 11 ^ t%.

Experiment 9

Using the AAB and C methods described in Experimental Examples 6 to 8, using high-density polyethylene having different melt indexes and fluorocarbon F-11, respectively. Going green yarn

The dissolved state of the polymer corresponds to the pressure change immediately before spinning, especially the pressure change in the decompression chamber. 'In other words, the more the polymer was incompletely dissolved, the greater the pressure fluctuation in the decompression chamber, and finally the spinning became impossible. Even if spinning was possible, undissolved polymer would be ejected if the pressure variation was large, and the fibers were crumpled and the strength was too low to use.

Each method was compared using the pressure fluctuation range representing this dissolution state, and is shown in Table 1. All polymers were high-density polyethylene (made by Asahi Kasei Corporation). The solvent used was Fluorine-11. The polymer concentration was 11% by weight, and the total discharge rate was 1000 g / min. The spinning conditions and apparatus used in Experimental Examples 6 to 8 were used. As is evident from Table 1, it is clearly shown that the more preferred spinning method is from A, method to _Az method, and further to B method, C method.

Incidentally, prototype poly Ma in this experiment - using (. Asahi Kasei Corporation, M l = 0 31, weight average molecular weight of about 21 X 1 0 ^4), examples were spun by Method C The conditions are as follows.

That is, the temperature of the extruder screw section was 300: the temperature of the special mixing section connected at the same speed was 200, and the temperature of the piping and the static mixing section was 170. The pressure in the polymer zone is t-, 250 / d-G in the special mixing section, and 20 (Hg / crf'G) in the static mixing section. For control, a gear pump with an extrusion volume of 35 per one-side transfer is installed at the end of the special mixing section.

S This part matured at 200'c. The pressure in the pressure chamber is

The liquid temperature in the decompression chamber was 110 g / ci'G.

Further, in any of the spinning examples, no leakage occurred from the flange portion or the like. In addition, a small amount of polymer was slowly and positively leaked from the rotating shaft of the gear pump for lubrication. Ε¾β width and weft t ^ J in Table 1 (early 1ii, kg / cdG)

Polymer one Polymer ^ 1 lal¾ 1 case lo-

-By the process shown in Fig. 10, a mesh-like steel made of high-density polyethylene was obtained.

The melt index (VII) is 0.35 (weight-average molecular weight, about 21 x 10 high-density polystyrene (Santech HD: B87 manufactured by Asahi Kasei Corporation) The chips of 1) are continuously melt-extruded by an extruder, while Fluorine-11 is added as a solvent by a fixed-quantity pump, and the mixture is extruded and mixed in a special mixing section. The structure of the extruder and the mixing section used at this time are as shown in Fig. 8, and the screw has a screw section, a dam section, and a pin section. Each length was 700 dragons, 210 mm x 250 dragons, and the corresponding barrels were 35 thighs, 50 丽 ø, 50 ø, and 'Solvent inlet was provided in the barrel in front of the dalmage.

Disk Po Li mer supply amount of Li-menu rotation number 4 6 r _P m is 7 4 g Z min, the amount of solvent is injected into the mixer unit was 240 g / min.

This mixture was introduced into the static mixing section together with 360 g / min of the solvent to be added to obtain a solution having a predetermined polymer concentration. At this time, as a static mixing element, a mixer S MX type manufactured by Sulza

(Nominal diameter 15 nm) with 50 steps was used.

When spinning this liquid, a 0.5 mra ø (Shino D = 10) low pressure orifice, ^ 2 cc low pressure chamber, 0.5 mm ø (L / D = 1) The spinning assembly made of the No. 1 yarn nozzle was used. The discharge state was extremely stable. Experimental Example 1 In FIG. 11, under the cow, only the mixer of the same forceps as the extrusion screw of the present invention was replaced with a conventionally known independent screw mixer. The process of π was carried out.

Using the extruder of 35, the molten poly was introduced into the screw mixer, while the solvent was entirely introduced into the screw mixer. This screw mixer is a mixed arresting mixer with two inlets, with a projection on the 35 mm ø barrel side and a notch in the screw hole. Was.

The same static mixer and spinning device as in Experimental Example 10 were used, but in this example, leakage occurred from the round part of the screw mixer, and spinning was impossible. '

Lonely test example 1 1

Fill an autoclave with an internal volume of about 50 Gcc. Add 7.7 g of high-density polyethylene (Sun HD HD B871, Ml: 0.35, manufactured by Asahi Kasei Kogyo Co., Ltd.), and evacuate the air. 1 g of glycerol was added (polymer concentration was 12 w-1%). In this solvent, 2,6-di-t-butyl para-cresol- was dissolved in advance as a ripening stabilizer in a concentration of 0.2 wt% with respect to the polymer.

At this time, the decompression chamber volume is ¾2 cc, the decompression pressure is 0.75 Φ (L / D = 6), and the spinning nozzle is 0.75 ø (lead hole inlet angle is 60 ° LZD = 1.3), a circular assembly of circular nozzle was used.

Heat with stirring · Dissolve by pressurization, and in the autoclave Stirring was stopped when the solution temperature was 16 1 ° C. Immediately, the bottom valve was opened and French spinning was performed while the inside of the autoclave was pressurized to 300 ^ / crf G with a liquid intensifier. A highly white fibrous filament of 0 g / d was obtained.

The pressure in the decompression chamber during this fiber spinning was 110 kg / cifi G, and the pressure loss at the decompression orifice, that is, the pressure difference before and after the decompression orifice was 190. / cn! —

In addition, when the phase diagram of one liquid phase and two liquid phases of this system was determined using a pressure vessel with an optical window, the condition of the decompression chamber was clearly in the one liquid phase region. = Also, the state of activation was observed. For this purpose, using the same apparatus as that used to obtain the phase diagram, the change in the amount of light, that is, the pressure difference observed before and after the orifice in the pressure chamber orifice, was measured. As a result, it was confirmed that when a pressure difference was generated at a pressure difference of 190 _kg Z ai G, the liquid temporarily became completely dark-field. That is, it was found that the liquid was activated by the pressure difference. It was also confirmed that these decompression chamber conditions were one liquid phase conditions.

MM 1 2

The same equipment and polymer / solvent as in Experimental Example 11 were used, but in this case, the orifice in front of the decompression chamber was 0.5 (L / D = 10) spinning nozzle. 0.5 round ø (lead hole angle 60 °, L / D = 2) circular nozzle was used. In the same operation as in Experimental Example 11 (except that no mature stabilizer was used in this experimental kiln), the liquid temperature in the autoclave was 160 ° (:, the pressure was 240 kg G, and the pressure was 240 kg. Performs lash spinning to produce high-density polyethylene pure white highly fibrous A rilled reticulated filament was obtained. At this time, the pressure in the decompression chamber is 90 kgV ai G, the pressure difference before and after the depressurization orifice is 190 kg cii G, and the filament intensity is 202 d The strength was 3.6 g / d. Also activates liquid! It was measured by the same method as T-kiyoshi 11 and it was confirmed that it was activated. And it was also confirmed that these decompression chamber conditions belonged to one liquid phase.

Compare M 4

The same apparatus and polymer solvent as in Experimental Example 12 were used, but in this case, the low-pressure orifice was 1.5 mm (J / D = 3.3). ·

In addition, flash spinning was performed with the autoclave pressure set at 150 kg / erf G, and the pressure in the decompression chamber at this time was 9 Q kg / αίG similar to that in Experimental Example 12. However, the obtained yarn has a stickiness in which the difficulty between the two is not sufficient: a weaving degree of 275 (1, a very weak yarn having a strength of 1.5 g / d. The state of activation was measured in the same manner as in Experimental Example 12, but it was found that no liquid activation occurred.

Experiment Kiyoshi 1 3

The same apparatus and polymer / solvent as in Experimental Example 1.2 were used, but in this case, it was surrounded by a 0.5 hole (lead hole angle was 60 °, L = D 2). In addition, a spinning nozzle was used in which the Danube flare with a cut head was integrated.

Assuming that the liquid temperature in the autoclave is 161 and the pressure is 280¾0 ^ 0, and the spinning is performed, the pressure in the decompression chamber becomes 90 kg ノ αίG. A pure white filament of d was obtained. This The filament was a reticulated filament consisting of very fine fibrils with a narrow thread width and seemingly insufficient fibrillation. Activation of the liquid was also observed, confirming that the decompression chamber conditions belonged to one liquid phase.

Example ί 4

Using the same device as in Example 11, the decompression pressure was 0.45! It was performed using a circular Bruno nozzle of ^{6 0 1, L / "D} = 2); L, Roh D = 1 1), spinning Bruno Zunore 0 45 positions ų (rie de hole angle or..

In this case, different brands of high-density polyethylene (Santech HD-B161, Asahi Kasei Kogyo Co., Ltd., Ή = 1.2) were used at a polymer concentration of 14. By the same operation, the liquid is discharged at a liquid temperature of 180 and a pressure of 250 kg crf G, and is a highly powerful pure white fibrillated to a temperature of 120 d and a strength of 4.6 g no d. Of this product. At this time, the pressure in the decompression chamber was 80 kg / G. In addition, the pressure in the pressure chamber was a one-liquid phase condition, and activation occurred under this condition.

Lonely example 1 5

As shown in J. SP.3, 456, 156, the textile obtained in Experimental Kiyoshi 4 was transferred to a net using a dispersing device S having a rotating deflector and a corona discharge device. Collected on a conveyor. At this time, the three-dimensional reticulated ίyawei discharged from the spinneret was deposited on the net conveyor in a width m of 30 to 60 mm while continuously oscillating from side to side. . The non-adhesive tape was pressed between the entire surface pressure roll (at a temperature of 135) and the rubber port with a linear pressure of 13 kg / cm, once for each of the front and back sides for 10 m / min. The non-woven fabric thus obtained had a specific surface of 8.6 nf / g and 6.0 m / g, respectively, when the inner layer and the surface layer had difficulty. The specific surface area measured as a whole non-woven fabric without separating the layers was 6.4 rr? / G.

This nonwoven fabric, basis weight 4 0 g / tensile strength nf the vertical Z ® co is _{13.3 / 14.2 (k ff Z 3} cm width), e Leme down Dorf tear strength 1.02Z 1.02 (kg), the reference basis weight 5 this The converted value was a high-strength nonwoven fabric with a tensile strength of 17.3 to 0.7 (kgZ3 oii width) in vertical / horizontal and an elementary tear strength of 1.28Z1.28 (kg).

In addition, the amount of laser transmission of this ignorant cloth was 13.7, indicating that it had sufficient opacity.

The nonwoven fabric had a bacterial water of 3600 mH ₂ O and a Gurley HI air permeability of 900,5 ec 50 mi.

Also, the MI and molecular weight distribution of the nonwoven fabric are different from those of the textile.

'■ ^ ΛΡtsu:

Experimental Example 16-: L9

Non-bonded solids obtained by the same method as in Experiment No. 15 were bonded under various conditions using the same press. The bonding was performed once for each of the front and back sides, and the results are shown in Table 2. No. 2

^ Experimental example 1 6 Experimental example 1 7 Example 1 8 Example 1 9 Attaching nonwoven fabric (g / m) 3 9 G 0

Roll temperature (in) 137 135

I'J linear pressure (kgZcm) 1 3 1 0

^ Adhesion speed (m / min) 10 4 10

Inner layer 8.0 7.2 '8.9 7.2 Relative surface area

Eclectic layer 5.2 4.3 6 '1 5.1 (m ² / g)

Whole nonwoven fabric 6.0 5.4 7.2 5.6 Tensile strength Vertical / Horizontal (kg / S cm) 18.4 / 19.5 14.0 / 14.2 25.4 / 24.5 8.4 / 7.7

23.6 / 25.0 17.1 / 17.3

(kg / 3 cm / 50 £ / rn) 21.2 / 20.4 16.8 / 15.4 Tear strength-Degree-

Elmendorf (kg) 0.35 / 0.44 1.00 / 0.83 1.06 / 1.07 0.61 / 0.54 Commutative bow Crack strength ——Da 7a- — 0.45 / 0.57 1.22 / 1.01 0.88 / 0.89 1.22 / 1.08 _K ^ _Z .. . £. JIL). 111 4

Laser-transmitted light M (<"W) 19.8 11.9-62 1- 10.5 15.3 Water pressure (dish ii ₂₀ ) 4, 100 3,000 3,500

Garley Hill air permeability (s c / 50m «) 3,000 250 2,000

2 li 1 11 1 3 5! 3 o Experimental Examples 20-23

In the same manner as in Experimental Example 15, the textile obtained in Experimental Example 5 was collected on a net conveyer while being spread 30 to 65 ™ and swung right and left. M-bonding was performed using the σ-rules used in Experimental Examples 15 to 19. One treatment of each of the front and back was performed to obtain the results for the third wheat.

What

. ¾ Kenrei 2 0 ¾ Kenrei 2 1 'Kenrei ^<} 2' Contact ¹ ¾ Example 2 3 I; woven with Ώ (g / in) 4 0 4 0 4 2 G 0

135 135

—Round pressure (kg / cm) 1 3 2 0 2 1 3 Contact speed (mZ) 1 0 1 0 5 1 0 Inner layer 7.2 5.7 7.4 Ratio surface area

Eclectic layer 5.3 5.0 4.G 5.0 (rrf / g)

Whole non-woven fabric 6.1 5.2 5.3 5.8 1 ¾ Strength テ / ((kg 3 cm) 12.3 / 11.8 13.8 / 14.2 0.81 / 9.0 21.4 / 21.8 ^ Tensile strength — 7

(kg / 3 cm / 50fi / m) 15.4 / 14.7 17.3 / 17.7 9.6, 10.7 17.8 / 18.2 ':! Strength 1 ΓΓ

Elemendorf (kg) 0,55 / 0.66 0.50 / 0..52 0.77 / 0.80 0.68 / 0.66 Exchange strength Tear strength

Ereme .. —Dore 0.69 / 0.

? — (Kg, / 50 M .m). 82 0.62 / 0.65 0.92 / 0.95 0.57 / 0.55 Laser light M (w) 15.1 18.8 13.3 11.7 ft Water pressure 1 0) 2,400 2,800 2,100 2,600 sc / 50 » _; i) 800'950 5 8 540

Experimental Examples 24-27

The steel obtained in Experimental Example 3 was collected as a non-adhesive web on a net conveyor in the same manner as in Experimental Example 15 and then both sides were bonded together with a mouth. The results are shown in Table 4.

荬镜 Example 2 8

In the same manner as in Experimental Example 15, non-adhesive non-woven webs were obtained from the three-dimensional steel tube obtained in Experimental Example 1. This non-adhesive nonwoven web was treated on both sides with a vinyl toka render. The ripened drum at 136 was treated at a high speed of 35 m / min to obtain a nonwoven fabric whose surface was ripely bonded. .

The specific surface area of the inner layer portion of this ignorant cloth was 5.2 rrf Z g. In addition, this non-woven cloth has a laser transmission of 8 μW at 60 g Z trf and a Gare Hill air permeability of 44 s ec. It is a non-woven city and can be used for envelopes, labels, breathable wrapping materials, and various other paper-based uses. The physical properties of this non-woven fabric are 50 g / nf The tensile strength was reduced to IT 、ヱ IT IT IT IT IT IT IT IT IT IT IT IT IT IT IT IT IT IT IT IT IT IT IT IT IT IT IT IT IT IT. Photo 19 (b) is a photomicrograph of a cross section obtained in the same manner as in the case of T y v-ek @C in Comparative Example 5 described below. The three-dimensional silky fissures are more densely packed, despite the similar weight per unit compared to the comparative example. The fibers of the textile are fine. The shows. Four %

Comparative Kiyoshi 4-Non-adhesive web was obtained using the textile of Comparative Example 2 in the same manner as in Experimental Example 15 and subjected to the same thermal bonding.

In the case where the surface fuzz is stopped and bonded so as to retain the tensile strength, the relationship between the tensile strength and the tear strength is the area indicated by the solid line in Fig. 12 and the specific surface area of the inner layer is 2.5 to 4.0. The value of m / g was shown. In addition, the opacity rating due to the amount of laser light transmitted was inferior. Comparative Example 5 '--DuPont Co., Ltd.

The Tyvek © paper-like type (10 type) was compared with the three-dimensional net-woven nonwoven fabric of the present invention.

'Weight (g / rrf) 4 4! 5 5 1 6 1: ratio i inner layer 2. 6 ¹ 2, i ¹ 9 Λ ¹

1

^-1 ° ' ^U i

B

1.5'1,5: 1.7:

(nf g): whole non-woven fabric 1. 8 1. 3 ¹ 1. 9; exchange tensile strength

Vertical / Horizontal 14.1 / 16.1 1.4.16.

(kg / 3 cm / .50 g / rn) \-

! Converted tear strength

Vertical; 0.43 / 0.54 0.33 / 0.32 0.33 / 0.52

ί (kg / 50 g / m),

Laser transmitted light 1 2 2 * <

<1 6

(βW) ^{1 8.} + 1

In each case, the specific surface area of the inner layer was less than 5 rrf / g, and the opacity and tensile / tear strength indicated by the amount of transmitted laser light were inferior to those of the fabric of the present invention.

Experimental Example 2 9

The fiber obtained in Experimental Example 4 is moved using a dispersing device having a rotating deflecting plate and a corona discharge device, as shown in Shi 'SP 3,456,156. I gathered on a conveyor. At this time, the three-dimensional reticulated fiber discharged from the spinning nozzle was deposited on the net conveyor while continuously oscillating from side to side with a width of 30 to 60 m.

This non-adhesive nonwoven fabric was partially adhered using an embossing roll and a rubber roll. In other words, each embossing roll is a square of 0.7 mx 0.7 «in the width and circumferential directions. The pitch of each was 1.25 ™ and the emboss depth was 0.3 us.

The embossing roll was heated to 132 ° C, and both sides of the front and back were treated by dip- ing with a rubber roll to obtain a patterned, non-adhesive non-woven cloth. Although this cloth was excellent in the friction resistance of the surface, the texture was a little hard, so it was kneaded by hand.

A cut was made in this unknowing cloth, and when it was forcibly torn, it was difficult to find a strongly heat-bonded surface layer and an inner layer consisting of a crepe that retained the form of a reticulated crepe. By grasping one end of the mesh fiber in the inner layer and carefully separating it from the other mesh fibers, a large number of continuous mesh fibers of about 30 to 100 cm were taken out. When the small-angle X-ray scattering was measured using these net fibers, the long-period scattering intensity ratio was 90. On the other hand, the long cycle increased slightly, showing a response of 181 people.

This insane cloth is extremely flexible, has excellent surface friction, and has no fuzz even when strongly rubbing the surface with a finger, and has a very high covering power, protective clothing, simple clothing, Desiccant-suitable as a breathable packaging material, such as a removable material, and other flexible packaging.

This nonwoven fabric had a weight of 5 Qg nf and an average amount of transmitted laser light of 14 W. The nonwoven fabric's vertical / horizontal properties, tensile strength is 9.5 Z 10.3 (kg / 3 cm width), single-toner tear strength is 1.9 2 2 * 0 (kg), and the cantilever is The flexibility by the method was 5.25 · 6.6 (). Example 30.

The non-adhesive non-woven fabric obtained in Experimental Example 29 was treated between the entire surface of the crimping hole and the rubber roll. In this case, only the surface was treated, and the roll temperature was set to 135 and the roll linear pressure was set to 10 kg / cm. The obtained non-woven fabric is a non-woven fabric that has one surface firmly and strongly bonded to the other surface and is not heat-bonded to the other surface and the inner layer. Out

In the measurement of small-angle X-ray scattering of this fiber, the long-period scattering intensity ratio was 8.5, and the long-period was 180 mm.

This non-woven fabric can be used for applications that make use of the difference between the two surfaces. For example, an adsorbent or deodorant is added to the non-adhered surface to make it a filter for adsorption or a deodorant finoletter. Materials (files, woven fabrics, etc.) are bonded together and used as a composite material with high covering power and high tear strength.

This O nonwoven fabric has an average transmitted light amount of laser of 5'W at a basis weight of 50 g, and shows extremely high covering power. In addition, the physical properties of non-woven fabric vertical / horizontal are as follows: tensile strength is 11.2 11.8 (k / 3 cm width), and Elemendorf tear strength is 1.6-1.6. (kg) and extremely high value.

Example 3 1

The non-adhesive nonwoven fabric obtained in Experimental Example 29 was subjected to a double-sided treatment using a flute calender. The surface layer was heat-bonded by a high-speed treatment in which the contact with the drum heated for 1 second was performed for 1 second, and a non-woven fabric having a net-like weave shape in the inner layer ^ was obtained. o 5

The small-angle X-ray scattering of the fiber extracted from the inner layer of this nonwoven fabric has a long-period scattering intensity ratio of 7.0 and a long-period of 230 mm.

In addition, this nonwoven fabric has a basis weight of 40 g / π レーザー and a laser average transmitted light of 8 βW, has excellent covering power, is a bulky paper-like nonwoven fabric, and is used for envelopes, labels, and other various paper uses. Can be used for

The physical properties of this non-woven fabric are as follows: tensile strength is 10.8 12-0 (kg / 3 cm width) and Elmendorf tearing strength is high.

1

Four

/ 1.4 (kg).

Experiment 3 2

The steel obtained in Experimental Example 5 was collected as a non-adhesive non-woven fabric in the same manner as in Experimental Example 29, and then a soft non-iron cloth with an embossed pattern was formed.

Similarly, measurement of small-angle X-ray scattering of fibers taken from the inner layer has a long-period scattering intensity ratio of 20 and a long-period of 210 A. This nonwoven fabric has a weight of 50 g / rf and a laser average. The amount of transmitted light was 15'W. The physical properties of the nonwoven fabric length / width are tensile strength of 3-3Z 9.0 (1¾3 cm width), single tongue tear strength of 7 / 1.8 (kg), and The degree of flexibility 0 by the lever method was 5.h / 5.0 (cm).

Comparative Example 6

Using the steel obtained in Comparative Example 2, in the same manner as in Experimental Example 29, a non-adhesive nonwoven fabric was produced, and a flexible nonwoven fabric was produced in exactly the same manner.

5 Similarly, remove the mesh-shaped steel from the inner layer and remove Small angle scattering measurements were made. The long-period scattering intensity ratio is 6 Q and the long-period is 240 A /

This nonwoven fabric had a basis weight of 50 g / m ² and an average laser transmission light quantity of 20′W, which was inferior to that of Experimental Example 29.

In addition, the physical properties of inexperienced vertical / horizontal materials have a tensile strength of 6.5Z6.4.

(kg 3 cm width), and the single-toner tear strength was 0.8 / 0.8 (kg). The strength was inferior to that of Experimental Example 29.

Compare 17

Five

A commercially available nonwoven fabric of Tyvek® 1443 R manufactured by E. I. dn Pont was unraveled.

This non-woven fabric is a flexible non-woven fabric having an embossed pattern, and as shown in the present invention, retains the form of reticulated iron wire in the inner layer. When the small-angle scattering was measured, the long-period scattering intensity ratio was 50 and the long-period was 172 A.

Further, the basis weight of the nonwoven fabric was 44 g / m, the average amount of transmitted laser light was 22'W, and the nonwoven fabric was conspicuous and had poor covering power.

The physical properties of the nonwoven fabric's vertical / horizontal properties are 7.9 /

At 9.0 (/ 3 cm width), the single tongue tear strength was 1.4 / 1.6 (kg), and the flexibility by the cantilever method was 6.2 to 6.3 (cm).

Experimental example 3 3

Molelet index (MI) 0.71 in fluorocarbon solvent A solution with a concentration of 11 in which polyethylene resin is dissolved is passed through a 0.8 mm diameter and 5 mm long decompression orifice to form an 8 mm diameter and 40 plate long pressure chamber. After pressurizing with a nozzle, pass through a nozzle with a nozzle diameter of 0.90 mm and a length of 0.75 mm:

Table 5 shows the spinning conditions and yarn properties.

¾HL Ί; id J (in)

Spinning

Solution pressure; 300 (kg- / cmG)

, 杀

(Compressed room temperature; 191 C ° C)

; water

Pressure chamber pressure 8 0

; Case \

Polymer flow rate; • 18 (kg / H)

1 mu 顿. 270 (d)

1 item Tensile strength ® (/ d)

\! Specific surface area * ②. 4 9

* ① bow tension

Grasp: i 5 cm, Tensile speed 10 on min. Condition, 4 times Z cm twisted three-dimensional reticulated fabric test.

* ② Specific surface area

Amco: Measured using the company's product (Rikiroeruba, Sovitomatic 1800).

An example of the spun three-dimensional netted steel fiber and gas stream suitable for producing the nonwoven fabric of the present invention arranged perpendicular to the spinneret at a distance of 5 plates in the horizontal direction from the spinneret Was supplied to a rotary dispersion plate to produce a nonwoven web. The rotating dispersion plate has three swinging surfaces similar to those shown in Figs. 14 (a) and 14 (b). The dimensions of the rotating dispersion plate are as follows. It is right. Disk diameter D, 100> ™, rocking surface for镥成the circular cylindrical portion diameter D ₂ 4 0 scan mosquitoes over preparative portion the inclination angle of "= 4 5 (X, = 1 0 Y i = 1 0 Yuradomen Is the center angle _r = 106.2 around the disk rotation at the intersection where the moving surface contacts the side of the cylinder, and the center is the disk rotation の at the intersection where the rocking surface contacts the top of the disk = 75.7 ° The collision surface has an inclination angle of ^ = 45 ° (X2 = 1 3 «. Yz = 1 3«) and both ends are flat. A continuous convex curved surface

The rotating dispersion plate was rotated at an E number of revolutions of 1,000 rpm 2,000 rpm and 3000 rpm. · The corona discharge was applied to the three-dimensional reticulated fabric that had exited the rotating dispersion to cause the electric charging to increase. Corona discharge was performed by applying a negative DC high voltage of ¾20 kv to electrode needles arranged in a semicircle around a rotating disk with 11 mm pitch and 16 needles.

By setting the distance between the bottom of the rotating dispersing plate and the net conveyor to 200 ™ and rotating the rotating dispersing plate, the three-dimensional reticulated fiber can oscillate in a swing cycle three times the rotation speed. While being pendulum-moved, a uniform non-woven tube having a net conveyor vertical effective width of about 30 on was formed with the aid of a suction duct provided below the net conveyor.

The state of drop of the open fiber was observed using a high-speed imaging device. confirmed.

The speed of the net conveyer is different from that of the

It turned out in minutes. A three-dimensional net composed of 100 cm length of the obtained web was taken out and the opening width was examined. The average discernment width is about 90 mm, and the minimum width is about 70 «

(Fiber density 3.8-denier width) and the fiber density of the bundle in the mesh fiber 40 denier The following †

The formed non-woven web was subjected to mature pressing once between the front and back sides between a metal roll having a smooth surface 132) and rubber.

Weight change rate in the width direction of the non-woven fabric thus created

R and laser spot transmitted light fluctuation rate r / y

Are shown in Table 6.

* ® Percentage change in width direction

1 cm X 5 on each 1 αιι in width direction * ② Fluctuation rate of transmitted light of laser spot light

A laser beam with a power of 5 mW and a beam diameter of 2.5 sm H is irradiated on the non-bonded non-woven fabric by a He-e laser, and the amount of light transmitted through the non-woven fabric is detected by a laser power meter.連続 Measure continuously in the width direction of the cloth and 10 points in 5 cm length direction.

From Table 6, the change in the basis weight in the width direction representing macroscopic unevenness of the nonwoven fabric is within 30%, and the variation in the amount of laser-spot transmitted light in the widthwise direction that causes microscopic unevenness in the nonwoven fabric. The ratio was within 50%, and it was proved that the nonwoven fabric of the present invention was a highly uniform nonwoven fabric. After softening this nonwoven fabric, an independent three-dimensional mesh fiber was collected from the inner layer, and the small-angle X-ray scattering state was examined. The long-period scattering intensity ratio was .11 and the long-period was 1. 80 A.

Experimental example 3 4

The rotational dispersion was performed under the same conditions as in Experimental Example 33, except that the distance between the bottom and the net conveyor was changed to 320 dragons. The rotation speed of the rotation dispersing plate is 200 Γ ΟΙ ΟΙ, the net moving speed is 17 mZ, and the formed web has an effective width of 45 cm. The average basis weight is 39 g / m ^2. I did. The three-dimensional reticulated fabric composed of the web with a length of 100 cm was taken out and the width of iron opening was examined. As a result, the average opening width is about 75 dragons, the minimum opening width is 20 m (steel density is 13.5 denier Luno dragon), and the net fiber is 40 denier / width or more. There were no bundles converging to density.

The formed nonwoven web was subjected to hot pressing in the same manner as in Experimental Example 33. This was performed once for each of the front and back sides to obtain a nonwoven fabric. _

This non-woven fabric was a uniform non-woven fabric with a variation rate of 30% in the width direction and a variation rate of laser-spot transmitted light of 49%, which was sufficient for both macroscopic and microscopic spots.

Compare 1 3

Table 7 shows the uniformity of the obtained nonwoven fabric and the openability of the obtained nonwoven fabric under the same conditions as in Experimental Example 33, except that the rotating dispersion plate was changed to the one having the scar shape shown in Table 7. The rotation speed of the rotation dispersion plate was 3000 rpm, and the net movement speed was constant at 2 Om minutes. The formed web has an effective width of about 3 Qcm and an average batting of 48 g / m

^ ^, —.

As a result of taking out and examining a three-dimensional mesh fabric formed at a length of 100 cm of the tube, the flat steel width was about 70 ™ and the minimum fabric width was 5 cm (the fabric density was 54 denier. / Job) contained many bundles of 60 mm in length.

This web was made into a nonwoven fabric by hot pressing once on each of the front and back sides as in Experimental Example 33.

As is clear from Table 7, the nonwoven fabric which deviates from the nonwoven fabric of the present invention has a variation in the basis weight in the width direction expressing macroscopic spots of 30% or more, and transmission of laser spot light expressing microscopic spots. The rate of change in light quantity was more than 50%, which was an uneven ignorance.

"* Disc diameter D, = 100 Μ Φ '

Cylindrical part diameter C. 1: D ₂ — 50 Any ø, g-2, C-3 D 40 iaia

Experimental example 3 5

Table 8 shows the basis weight and openability of the nonwoven fabric obtained under the same conditions as in Experimental Example 33 except that the rotational dispersion was changed to the one with the scar part shape shown in Table 8. . The rotation speed of the rotation dispersion plate was set to SOOOrpm, and the net moving speed was set to 20 m / min.

The density of the fibers in most bundles of the three-dimensional net-woven fabric that forms the obtained web is 40 denier or less, and the density of steel mixed with a very small amount is 40 denier / m. The size of the binding part larger than the width was 5 or less in width and 30 or less in length.

This web was hot-pressed once on each of the front and back sides in the same manner as in Experimental Example 33 to obtain a non-woven fabric.

As shown in Table 8-Table, the obtained non-woven fabric had a sufficient degree of uniformity.

Photo 20 (a) is a photo taken from the top of the nonwoven fabric of E-2 in this experimental example, with light being irradiated from the bottom. Photo 20 (b) is a photograph of Tyvek® B of Comparative Example 5 taken in the same manner.

In the case of Experimental Example 35, the bundle was invisible and visually uniform. On the other hand, in the case of Comparative Example 5, a stripped portion was observed, indicating that the microscopic uniformity was poor.

3 6

To obtain a 100 cm wide non-woven fabric consisting of high-density polyethylene mesh fibers by the flash spinning method, four spinnerets are spaced apart in the width direction of the web 280 thighs, spaced in the length direction of the web The high-density polyethylene resin used was Melt Indene's (MΓ) 5 and was dissolved in Fluorine-11 solvent to form a 3 wL½ solution. This solution passed through a decompression orifice with a diameter of 0.60 and a length of 5. The diameter was 8 females.-After being pressed in a pressure chamber with a length of 40 mm, the nozzle diameter was 0.65 mm. 。 Flash spinning was performed by passing through a nozzle with a Φ of 0.65 ™ in length.

Table 9 shows the spinning conditions and yarn properties.

* 'Liquid temperature 1 181 (in)

Solution pressure 1 200 (kg- Z cm G

· 'I mut

Pressure chamber temperature 1 178 (r)

Article

Pressure chamber pressure 1 7 0 (kg--/ cm Li

; Gender

i Polymer flow rate 1 2 (kg / Η?

! 1 mud weave; 160 (d)

; Tensile strength; 4.7 (g d)

; Specific surface area; 35 (/ g) The three-dimensional mesh fibers spouted from each spinneret are supplied to the rotary dispersion plate according to the present invention, similar to Experimental Example 33, which is arranged at a distance of 1 ™ horizontally from the spinneret. Dress up

The distance between the bottom of the rotating dispersion plate and the net conveyor is set to 150 ™.

At.

Rotation dispersion plate of each綞2 0 00 while rp not if the pendulum luck勛in synchronous operation is to 4 0 00 c Bruno amount of rocking Sai cycle if three-dimensional network Wei Ri by the and this in _m 'nets co With the aid of the suction duct provided at the lower part of the conveyor, it was deposited on the moving conveyor and stacked sequentially.

-The fiber density of most bundles in the opened three-dimensional reticulated fiber constituting the obtained web is less than 40 denier Lunong width, and the fiber density mixed in a very small amount is 40 denier. The size of the bundles over the width of // was also less than 5 mm in width and less than 30 in length.

The formed web was subjected to a mature press between the entire surface pressing roll (temperature 130.c) and the rubber call once each on the front and back to make the fabric non-woven.

The nonwoven fabric obtained in this manner is an extremely uniform nonwoven fabric having an effective width of 100 cm and a weight variation of 19% in the width direction of 41 Zm and a laser-spot transmission light quantity variation of 40%. Met. Industrial applicability

The three-dimensional net-like fiber, the non-woven fabric made of the three-dimensional net-like fiber, and the method for producing them according to the present invention have excellent characteristics and applications, respectively, because they are configured as described above. 説明 The explanation will be given in the following order. -

J_ and ^ The novel three-dimensional network fiber of the present invention

① It is made up of extremely incredible IH fibrils.

② Excellent mechanical strength ':'

③ Excellent high temperature characteristics

Is mentioned. There is no conventional steel that satisfies all of these requirements, and these features are suitable for use as a nonwoven fabric. In addition, the present invention has an advantage as described above, though it is an as-spun iron fiber, so that it is industrially advantageously produced and used. Therefore, it is also expected to be applied to various industrial materials and textiles, which required the strength of fiber and required stretching in the past. '--Book; The continuous fiber nonwoven fabric of the yarn direct connection type using the three-dimensional mesh fiber of Akira is extremely useful, and it is likely that it will be a nonwoven fabric with unprecedented performance.

Due to its strength, whiteness, reticulated structure and high specific surface area, this fiber can be used for various purposes by making it into a nonwoven fabric or using it as a fiber.

D_ Shown in the present invention; using a screw extruder, employing a spinning method and a process of sealing with a molten polymer, whereby a very strong flash-spun high-strength net is obtained.抆 The production of iron and steel becomes possible.

In other words, spinning using a high molecular weight polymer becomes possible, and solution preparation at a high E becomes possible. Extremely significant effects are achieved, such as eliminating process troubles due to leakage from the roller section and stabilizing the spinning system pressure.

E_ Utilizing a high pressure difference using high-density polyethylene and trichlorofluorene according to the present invention, and using a flash spinning method in which a liquid in a decompression chamber belongs to a single-phase region As a result, it is possible to obtain a highly fibrous high-density polyethylene network having higher strength than before. In addition, since the discharge is at a higher pressure, the yarn speed is increased, and the industrial speed at the production speed is reduced.

--1

The size is also large. In addition, 2

Also, since high-strength fibers can be obtained by spinning at a low temperature, polymer degradation and solvent decomposition are suppressed, stabilizing products and reducing solvent recovery costs.

The three-dimensional reticulated fiber non-woven fabric as in the present invention has a large specific surface area and a large mechanical strength (tensile strength and tear strength) based on the mechanical properties and thermal adhesive properties of the fabric that composes it. It is a new nonwoven fabric having This makes it possible to develop unprecedented performance in terms of covering power, uniformity, and mechanical strength, and is preferably applied to a relatively low basis weight area (25 to 70 g / rrf).

Applications of the non-ferrous cloth of the present invention that belong to the classification include envelopes, book covers, wall coverings, house wraps, building materials such as under roof materials, sterile packaging materials, sanitary materials, and filtration performance. It can be used for filters, floppy disk drives, ventilated packaging materials, various bags, recording paper, dust-free paper, difficult paper, impregnated paper, various tapes, materials for FRP, etc.

G Including a layer of a partially unfused reticulated fiber of the present invention. The 12δ non-woven fabric is a non-woven fabric made of the three-dimensional reticulated fiber according to the present invention, and is a non-iron fabric having high opacity and high covering property, particularly excellent in mechanical strength and ripened mechanical properties.

-This non-woven cloth can be used for protective clothing, safety clothing, sterile clothing, non-dust clothing, moisture-permeable waterproof cloth, s water cloth, stamp cloth, bag, etc.

In addition, the uniform nonwoven fabric according to the present invention has high uniformity in grooving over the entire effective width and excellent uniformity in appearance. Therefore, this non-woven fabric is extremely useful as a non-woven fabric having a high degree of strength required from the end use of unknowing cloth and a non-woven fabric having high uniformity even with a low basis weight.

It is also possible to increase the homogeneity of the non-woven fabric, including layers of partially unfused independent mesh fibers, in which case the high performance is added to the uniformity. , And very useful waste. —.

は The method of manufacturing a mesh-like nonwoven fabric using the rotating dispersion plate according to the present invention can provide a web having uniform openness and excellent openability over the complete destruction of the required sheet width. Therefore, the method using the rotational dispersion plate according to the present invention can easily cope with a high degree of uniformity required for the final use of the nonwoven fabric and a low-weight nonwoven fabric of 30 gZ <f or less.

Claims

Scope of Claim 1. A fibrillated, high-density polystyrene three-dimensional network characterized by having a long-period scattering intensity ratio of 1.40 or less.

2. The fibrillated high-density polyethylene system according to claim 1, wherein the three-dimensional network has a long period of 150 A or more and 200 A or less. Three-dimensional reticulated fiber.

3. The fibrillated high-density fiber according to claim 1 or 2, wherein the three-dimensional network fiber has a specific surface area of 30 f / _g or more. A polystyrene-based three-dimensional network fiber.

4. In the method of manufacturing reticulated fibers by the flash spinning method, the polymer is continuously supplied to the polymer melting area while being melted using a heated screw extruder, and melted. A solvent is added to the molten polymer while the inlet of the region is continuously sealed with a molten polymer that is continuously lined, and the two are mixed and dissolved under high pressure to produce a polymer solution. Is a fibrillated, high-density, polystyrene-based three-dimensional network IS fiber obtained by continuously discharging a polymer solution from a nozzle provided in a low pressure region.

5. The fibrillated high-density polyethylene system according to claim 4, wherein the three-dimensional network fiber has a long-period scattering intensity ratio of 40 or less. Three-dimensional reticulated fiber.

6. The fibrillated high-density polyethylene system according to claim 5, wherein the three-dimensional network fiber has a long period of 150 A or more and 200 A or less. Three-dimensional reticulated fiber. 7. The fibrillated, high-density polyethylene tertiary according to claim 5 or 6, wherein the three-dimensional network fiber has a specific surface area of 30 rf / _g or more. Former reticulated fiber. 8. A high-pressure homogeneous solution consisting of high-density polyethylene polymer and trichlorofluor-5 methane is spun from a vacuum orifice, a royal family and a spinning nozzle. In a method of obtaining a high-density polyethylene-based polymer network by discharging to a low-pressure region through a discharge device, a high-pressure difference is generated before and after the decompression orifice to activate the liquid. A fibrillated, high-density, polystyrene 0-based three-dimensional reticulated fiber.

9. The method according to claim 8, wherein a liquid in a decompression chamber comprising a high-density polyethylene-based polymer and trichlorofluorene methane is obtained in a phase diagram and obtained in a liquid phase region. A three-dimensional weave of high-density polyethylene that has been brillated.

510. The fibrillated high-density poly according to claim 8 or 9, wherein the three-dimensional network fiber has a long-period scattering intensity ratio of 40 or less. Ethylene-based three-dimensional silk fiber.

11. The fibrillated, high-density, polyethylene-based three-dimensional network according to claim 10, wherein the three-dimensional network has a long period of not less than 200 A. Wei.

12. The fibrillated, high-density, polyethylene-based three-dimensional net according to claim 10, wherein the three-dimensional netted fabric has a specific surface area of 30 nf ng or more. Wei Fushiori.

13. The fibrillated fiber according to claim 11, wherein the three-dimensional mesh steel has a specific surface area of 30 rf Z g or more. 5. High-density polyethylene-based three-dimensional meshed steel.

1 4. While using a ripened screw extruder, the polymer is continuously fed to the polymer melting zone while being melted, and the inlet of the melting zone is fed continuously. Claim: The method is characterized in that δ; a solvent is added to the molten polymer while closing with the molten polymer, and the two are mixed and dissolved under high pressure to produce a uniform polymer solution. 3. The fibrillated, high-density, polystyrene-based three-dimensional reticulated fabric according to paragraph 8, paragraph 9, paragraph 9, paragraph 11, paragraph 12, or paragraph 13.

1 5. Heated screw — extruder

-!

Solvent is added to the molten polymer while the inlet of the melting zone is continuously closed by the molten polymer that is continuously flooded, and the solvent is added under high pressure. The fibrillated high-density polyethylene system according to claim i0, wherein the two are mixed and dissolved to produce a uniform polymer solution. Three-dimensional mesh

16 6. In the method of manufacturing a netted fiber by the flash spinning method, a ripened screw is continuously fed to a polymer melting zone while being melted using an extruder. A solvent is added to the molten polymer while closing the inlet of the melting zone with a continuously supplied molten polymer, and the two are mixed and dissolved under high pressure to produce a polymer solution. A continuous method for producing a high-density polyethylene-based three-dimensional net-like fabric, characterized in that a polymer solution is continuously discharged from a nozzle provided in a region to a low-pressure region.

17 7. In the polymer dissolution zone, at least mixing and dissolution of the extruder must be performed at least in the mechanical mixing area attached to the extruder. 17. The method for continuously producing a reticulated fiber according to claim 16, wherein the method is characterized in that:

18. Claim 16 characterized in that in the polymer dissolution zone, mixing and dissolution of the polymer and the solvent are performed in multiple stages.

5. A continuous manufacturing method for the mesh fabrics described in 5.

19. In the polymer dissolution zone, mixing the polymer with the solvent '. Continuously producing the steel found in claim 17 characterized in that the dissolution is performed in multiple stages. Method.

20. Claims characterized in that, in the polymer dissolution zone, the addition of a solvent, and the mixing and dissolution of a polymer and a solution are performed in multiple stages.

Item 18. The intermittent method for producing Abishi iron wire according to Item 18.

―, 21. In the polymer dissolution zone, add solvent and dissolve the polymer.

Claims characterized in that mixing and dissolving with the agent are carried out in multiple stages; the method for continuous production of a reticulated fiber according to claim 19;

5 22. In the melting zone, every time the solvent is added,

20. The method for continuously reading a net according to claim 20, wherein the method is characterized by mixing and dissolving with-and successively lowering the viscosity of the polymer.

23. In the polymer dissolution zone, each time a solvent is added, it is mixed with the polymer and dissolved to reduce the polymer concentration sequentially.

21. The method for producing a net-like filament according to claim 21.

24. In the polymer dissolution zone, at least the first stage of multi-stage addition, mixing, and dissolution of the solvent to the polymer is performed for the polymer that is continuously melt-fed by a screw extruder. The extruder 24. The method for continuously producing a net-like fabric according to claim 21 or 23, wherein the method is performed in a region of mechanical mixing attached to the screw of the present invention.

25. The method according to claim 24, wherein in the polymer-dissolution zone, the solvent addition, mixing, and dissolution after the second stage are performed by using a static mixing element. A continuous method of manufacturing meshed steel.

26. A high-pressure homogeneous solution consisting of a high-density polyethylene polymer and trichlorofluoromethane is spun from a decompression orifice, a decompression chamber and a spinning nozzle. In the method of discharging to the low pressure area through the dispensing device and obtaining a high-density polyethylene-based polymer reticulated fiber, a high pressure difference is generated before and after the decompression orifice, and the liquid is generated. A method for producing a high-density polyethylene-based three-dimensional net * -shaped fiber characterized by being activated. .

27. A high-density polyethylene, wherein the liquid in the decompression chamber comprising the system polymer and trichlorofluoromethane belongs to one liquid phase region in the phase diagram. 26. The method for producing a high-density polyethylene-based three-dimensional network fiber according to item 26. '

28. Using a heated screw extruder, the polymer is continuously supplied to the polymer melting zone while being melted, and the melting polymer is continuously fed through the melting zone inlet. 26. The method according to claim 26, wherein a solvent is added to the molten polymer while sealing the mixture, and the two are mixed and dissolved under high pressure to produce a uniform polymer solution. Or a method for producing a high-density polystyrene-based three-dimensional reticulated fiber according to Item 27.

29. In the polymer dissolution zone, too much solvent for the polymer At least the first stage of the 'mixing' dissolution was added to the screw of the extruder for the volumer continuously melted and supplied by the screw dispenser Claim 25. Claim 28 wherein the addition, mixing, and dissolution of the solvent after the second stage are performed in the area of mechanical mixing using a static mixing element. A method for producing an ethylene-based three-dimensional reticulated fiber.

30. High-density polyethylene-based fibrilized continuous tertiary ': original mesh fibers deposited in random directions and firmly and firmly bonded to each other; Tensile strength and tearing, characterized in that the specific surface area of the inner layer is more than 5 nf / g in the integrated paper-like non-woven fabric consisting of the inner layer which has been weakly bonded to the textile layer and the inner layer 10 High strength three-dimensional reticulated fiber non-woven fabric. ,

31. Let X (kg / 50 g Z — ヱ Remendolf method) be the tear strength of Yt, and Y (kg 3 cm 50 g /) be the tensile strength.

15 (Each strength is a value obtained by proportionally converting the basis weight of the nonwoven fabric to the standard basis weight of 50 g /), X ≥ 0.4, and

-2 0 X 2 8 ≤ Y≤ 3 0

31. The continuous mesh nonwoven fabric according to claim 30, wherein the nonwoven fabric is a nonwoven fabric.

32. High-density polystyrene fibrilized three-dimensional network 20-shaped keys are arranged in random directions, deposited in layers, and partially unfused independent A nonwoven fabric comprising a layer made of a reticulated woven fiber, wherein the independent woven fiber has a long-period scattering intensity ratio of 40 or less.

25 33. The independent Amibushi weave has a long period of 0 A or more The high-density polyethylene-based three-dimensional reticulated steel nonwoven fabric according to claim 32, characterized in that:

3 4. Clean up the non-woven fabric in which the opened high-density polystyrene-based three-dimensional network fibers are randomly deposited.

When the bundle existing in the 5-unit network is a bundle having a density of '40 denier / 舰 width or less, or a bundle having a density of 40 denier / 'mm or more. A uniform non-woven fabric characterized in that it is a bundle having a width of 5 rara or less and a length of 30 mm or less.

35. The uniform nonwoven fabric according to claim 34, wherein the opened high-density polystyrene-based three-dimensional network fiber has a long-period scattering intensity ratio of 40 or less.

36. The uniform nonwoven fabric according to claim 35, wherein the opened high-density polystyrene-based three-dimensional network fiber has a long period of 150'A or more. .

37. A rotatable disk portion, a cylindrical portion extending vertically from the center of the disk portion and having a circular outer surface with a diameter smaller than the disk portion, one surface of the disk portion and a circular outer surface of the cylindrical portion And a non-open weave three-dimensional reticulated fiber flying in a direction substantially parallel to the axis of the cylindrical portion. A plurality of oscillating surfaces to be oscillated, and a bump arranged alternately with the oscillating surfaces to relieve a sudden change in the oscillating direction of the three-dimensional reticulated fiber oscillated by the oscillating surfaces The method for producing a nonwoven fabric nonwoven fabric using a rotating and dispersing plate of a three-dimensional network fabric composed of

The center of the rocking surface that constitutes the skirt and the upper surface of the disk The angle of inclination is approximately equal to the angle of inclination ^ between the center of the cushioning surface and the upper surface of the disk, and the cushioning surface is fan-shaped, with the width near the disk being wider than the width near the cylinder. A uniform non-manufacturing method characterized by using diffusion and oscillating rotational dispersion of a three-dimensional network fiber.

• 38. Claims characterized in that the swing surface forming the scart portion is substantially flat and the collision surface is substantially convex curved surface using diffusion _ · swing dispersion. A method for producing a uniform cloth as described in paragraph 37.

39. The distance between the bottom of the rotating dispersion plate and the collecting surface of the opened three-dimensional mesh fiber is defined as the distance between the bottom of the rotating dispersion plate and the changing point of the swing direction of the three-dimensional mesh wire. The method for producing a uniform nonwoven fabric according to claim 37 or claim 38, wherein the method is set as follows.