TW561205B - Meltblown process with mechanical attenuation - Google Patents

Abstract

Cellulose containing dope is extruded through orifices and into a stream of gas moving in a direction generally parallel to the direction that the filaments are formed with varying degrees of mechanical attenuation provided to the filaments using a take-up device, such as a winder.

Description

561205 A7

The title of this application is a meltblown method with a mechanical refinement process, which was filed on April 21, 2000, and benefits from the application date of the previous provisional application serial number 60 / 19M37. This application is also a continuous part, and its application was filed on the 23rd of the year, and the profit and profit of the previous joint trial declaration of serial number 4G9 / 768,741, which is also serial number 09/256 197, was in 1999 On February 24th, the continuation of the applications filed, and the current US Patent No. 6,2 丨 〇, 8〇 丨 is also serial number 09/185, 4 23, and the application filed on November 3, 1998 is continuous. Part. The disclosures of these previous applications are incorporated herein by reference. Scope of the invention The present invention relates to a method for producing filaments, which uses a method for improving dissolution, and in particular to a method for producing filaments of lyocell fiber, which uses a mechanical type Improved meltblown method for refining the filaments® Background of the Invention Over the past decade, major cellulosic fiber producers have engaged in the development of methods for making shaped cellulosic materials, including filaments based on the Leocell fiber method Objects and fibers. A method for producing filaments of Leosai fiber is called a melt-blown method, which can be roughly described as a step in which a fluid spinning dope is extruded through a row of nozzle holes, and when an air stream or other gas is elongated and refined The hot filaments are formed into a plurality of filaments. The filaments can be collected as continuous filaments or discontinuous filaments. A method like this is described in International Publication No. WO98 / 0791 1, which is assigned to Weyerhaeuser, the assignee of the present invention. -4-This paper size is in accordance with Chinese National Standard (CNS) A4 (210 X 297 mm). The fiber produced by the existing meltblown method has the variability in diameter according to its length. Variability in the length and diameter of the object to the filament, and a non-smooth surface and a natural distribution flange. In addition, it has been observed that the filaments of Leosai fibers are made by a melt-blowing method, which shows that fibrosis is at the required low level. The characteristics of these Leosai fiber filaments produced by the conventional meltblown method make them less suitable for applications where such characteristics are desired; meanwhile, these characteristics make the meltblown Leosai fiber filaments less suitable. For other applications, such as where filament diameters are less variable, have less natural flanges and higher strength. Another method used to make filaments of vegetable orsay fiber is called the dry spray wetting and spinning method. Examples of dry spray wet methods are described in US Patent Nos. 4,246,221 and 4,416,698 issued to McCorsley III. The dry spray wet method includes a fluid spinning dope, which is extruded through a plurality of nozzle holes to form a continuous filament in an air gap. Usually the air in this gap is stagnant, but sometimes the air circulates in one direction, which is opposite to the direction of the filaments, in order to cool and stiffen the filaments. The formed continuous filaments are refined in the air gap by a mechanical tensioning device, such as a winding machine. A tensioning device has a speed which is greater than the speed at which the spinning dope is exposed from the nozzle holes. This speed difference causes the filament to be mechanically elongated, resulting in a decrease in the diameter of the filament and an increase in its strength. After the filaments have been treated with a non-solvent, the cellulose is then precipitated by a conveyor stringer or other stringer device to form continuous filaments. These filaments can gather into the drawstring for transportation and cleaning. The raw fiber can be obtained by cutting the string of the filament. Transforming ground ’The filamentary continuous structure can be twisted to form a filament. The paper is suitable for size @ K 标 半 (CNS) A4 size (210X297 mm) 561205 A7

Things of yarn. From the dry-jet wet method (dry-jet silk 11 ... Gongyi ™), Chengzhi Leosai Fiber System has a smooth surface, and along a stack, less in cross-section diameter. Variable characteristics. In addition, the dryness of the diameter between wet filaments is low. In addition, from dry two ;: Run < ... Sai fiber filaments, unless the filaments are post-treated to Tiller type = so: flange two will have very few flanges. It is believed that the sensitivity of fibrillation of Leosai fiber filaments is greater than that of dry spray ^ ", which is greater than that of Baizhi meltblown. The fibrillation sensitivity of the fiber made by the method. Therefore, when selling the "Leo Sai fiber filaments made by ..." method, or the foot Leo Sai fiber made by the silk like this Fibers can be more suitable for applications, such as where low natural flanges, smooth surfaces, low variability along a fiber cross-section, and low variability from fiber to fiber diameter are desired compared to conventional usage Leosai fiber fibers made by the meltblown method are still easier to fibrillate. When used in Leosai fiber fibers To increase and broaden, there will be a need for improved methods for producing Leosai fibers, which will be able to produce fibers with the required properties' without using those undesired properties to the existing methods of producing Leosai fibers, Introduction to the invention The present invention provides an improved method for producing filaments of Leosai fibers like this, which comprises extruding a spinning dope, passing through a plurality of orifices, and entering the air stream 'to form a substantially continuous elongate filament. Method. The air stream is refined and the extruded filaments are stabilized from time to time. In addition, according to the present invention, the filaments use a winding -6-

This paper size applies to China National Standard (CNS) A4 (210 X 297 mm) 561205 A7

Thread machine 'or other M's tightening device for mechanical refinement. The mechanical winding machine or other tightening device applies an external force to the filament in parallel with the length of the filament. This force is in addition to the force exerted by airflow or gravity. The Leosai fiber filaments produced by the method carried out according to the present invention, and the Leovi fiber cut from the filaments like this show the desired quality, low sensitivity, such as fibrillation, and smooth The surface, the diameter of the cut along the filament, or the length of the fiber and the low variability from fiber to fiber, and extremely: > natural flange. In addition, the filaments and fibers retain strength characteristics that make them suitable for many applications, such as where Leosai fiber filaments and fibers are currently used and planned. A further advantage of the present invention is the rotation speed of the filaments of the Leosai fiber, which is higher than the speed at which the filaments are rotated by ordinary dry wetting or melt-blown methods. Higher spinning speed will increase productivity by increasing spinning dope output. If the output of the spinning dope is not increased, the fiber diameter can be reduced. The size of the extruded filaments, which are refined by the gas, and the size of the filaments, which are mechanically refined according to the present invention, can vary. For example, in one embodiment, it is preferred that it provides most of the gas refinement with a small amount of mechanical refinement. In other cases, it is preferred that a small amount of refinement is caused by the introduction of extruded filaments into the gas stream, and most refinements are provided mechanically. Combination cellulose filaments including cellulose and other polymers, and filaments including a mixture of cellulose and other materials can also be formed by combining cellulose with other polymers using one of the methods practiced in the present invention. Produced from spinning dope. Brief description of the diagram This paper size applies to China National Standard (CNS) A4 (210 X 297 mm)

Order

Line 561205 A7

The previous content and the present invention are also understood in detail by referring to the following, among which: Many of the accompanying advantages are made clear-it is easy to understand, and a detailed description with accompanying drawings will give you a better picture. The block diagram of the silk wire is more than the block diagram of the M wire; FIG. 2 illustrates an embodiment of a method for forming a wire like the present invention; only FIG. 3 is an extrusion head which is beneficial to meltblown as shown in FIG. 2 Cross-sectional view of the device; Figure 4 is a method of performing a fibrillation of Leosai fiber by one thousand times as one of the methods performed after the fibrillation test described in Example 1 according to an embodiment of the present invention. Photomicrographs; $% Figure 5 is a scanning electron micrograph of a commercially available Tencel® Leocell fiber, 1000 times magnified after being subjected to the same fibrillation effect as a bucket filament; and, Figure 6 is for In the example iiMBA, the average fiber diameter of filaments, and the method of plotting the coefficient of variation "Sentence diagram graphical element symbol description 200 supply line 204 extrusion head 206 gas supply line 208 potential filament 210 spray line 212 spray line 214 regeneration liquid Paper size applies Chinese national standard (CNS) A4 specifications (210X297 public love)

Binding

Line 561205

215 Regenerated filament 216 Pick-up roller 218 Winded filament 220 Solvent dripping liquid 222 Container 300 Extrusion head 332 Spinning dope supply conduit 334 Groove 336 Capillary 338 Conversion zone 340 Nozzle 342 Air chamber 344 Incision 346 Internal conduit 348 Detailed description of the preferred embodiment with half pieces Although the preferred embodiment of the present invention has been illustrated and described, it will be understood that various changes can be made without departing from the spirit and scope of the present invention. For example, in the preferred embodiment, the 2 gas system is described as a gas; however, it must be understood that other gases can have equivalent functions. A plurality of nozzle holes as required in the present invention are described in the following text of a dissolution nozzle. It must be understood that the use of a melt-head description is exemplary and other types of devices including a plurality of orifices suitable for extruding a spinning dope into the filaments will be beneficial to the present invention. The following description of an embodiment of the present invention refers to the production of Leosai fiber. The paper size applies the Chinese National Standard (CNS) A4 (210 X 297 mm).

Binding

Line 561205

[Explanation of the Invention] However, it is necessary to understand the method described below, and other combinations can be used to order only, and its dagger-type fibers, such as fiber combinations, are formed from cellulose and other polymer mixed spinning dope. Using the fibers of the method implemented in the present invention, the spinning dope is decomposed cellulose, preferably in the form of wood pulp in amine oxide, and is preferably a non-solvent for cellulose, such as third grade water Formed by amine N_ oxide: The wood pulp can be any of many commercially available decomposable or non-decomposable grade pulps derived from sources such as Aweyerhaeusa, International Paper Products, Sappi Saiceor vulcanized pulp, and Kraft pulp pre-hydrolyzed by International Paper Products. In addition, the wood pulp can be a highly hemicellulose, low-polymerization pulp, which is described in US Patent Application Serial Nos. 09 / 256,197 and 09 / 185,432 and International Bulletin No. These documents are incorporated herein by reference. Representative examples of amine oxide solvents in the examples that are beneficial to the present invention are described in US Patent No. 5,409,532. The preferred amine oxide solvent is N-methylmorphine-N-oxide (NMM0). Representative examples of solvents useful in the embodiments of the present invention include dimethylene (DMSO), dimethylacetamidine Derivatives of amines (DMAC), dimethylamidamine (0% [), and caprolactam. The pulp is subjected to any known method such as those set forth in U.S. Patents Nos. 5,534,113, 5,330,567, and 4,246,221, Decomposed in amine oxides. Figure 1 shows a block diagram of the preferred method for the use of Leocell fiber filaments made from cellulose spinning dope. If necessary, cellulose in the form of wood pulp is decomposed in amine oxides. -Before the water mixture, such as through the physical destruction of a paper shredder, to form a spinning dope. The pulp can be obtained by any conventional method, such as -10- This paper size applies the Chinese National Standard (CNS) A4 (210 x 297 mm) (Centi) Thread 561205 A7 B7 5. Description of the invention (8) US Patent No. 4,246,221 taught by McCorsley, decomposed in a monoamine solvent. For example, the pulp can be soaked in about 40% NMMO and 60% water insoluble In the mixture, the proportion of pulp wetted in NMM0 can be about 1: 5 .1 weight ratio. The mixture can be mixed in a two-arm S-shaped mixer at a temperature of about 120 ° C under vacuum for about 1.3 hours until sufficient water is distilled off based on NMMO to about 12% ~ 14% in order to make a fiber Vegetarian solution. Alternatively, NMMO with the appropriate water content can be used initially to avoid the need for a vacuum steamer. This is a convenient way to prepare a spinning dope in the laboratory, during which a concentration of about 40% to 60% is commercially available NMMO can be mixed with the experimental reagent NMMO with only 3% water to produce a cellulose solvent with 7% to 15% water. The moisture normally present in the pulp must be calculated to adjust for the required moisture present in the solvent. References can be found in the Journal of Polymer Science, 18th Edition of Polymer Physics: 1137-1144 (1980), articles by authors Chanzy, H., and A. Peguy, and by British Polymer Journal, page 174 (December 1980) By authors Navard, P., and JM Haudin, based on an article prepared by a laboratory for cellulose spinning dope in NMMO aqueous solvent. As in the embodiment of the present invention, the spinning dope is processed through a melt nozzle, and the spinning dope is extruded through a plurality of nozzle holes into a chaotic air flow, and the air stream moves substantially parallel to the direction in which the spinning dope leaves the nozzle hole. Instead of entering directly into an air gap, such as where there is no air flow or as in the case of a dry wetting method, as opposed to where the spinning dope leaves the air flow in the direction of the nozzle. Parallel air flow The point at which the spinning dope leaves the orifice describes the downstream air flow. As described in more detail below, according to the special structure of the melter head, the air leaving the melter head does not need to advance in the direction of the filaments; however, the distance from the spinning dope leaves the sprayer -11-This paper size applies the Chinese national standard (CNS ) A4 size (210X 297mm)

Binding

Line 561205

Description of the invention At some point downstream of the mouth, as in the present invention, the air begins to flow in the direction of a parallel filament. The high-speed air elongates or elongates the filament. This air refinement is different from the mechanical refinement by providing a more variable tension, and provides a continuous tension due to the turbulence of the air flow. This non-mechanical elongation serves two purposes: it produces certain longitudinal molecular orientation dimensions, and it rapidly accelerates the filament as it leaves the nozzle orifice, thereby reducing the final fiber diameter. This air flow is also believed to stabilize the underlying filaments as described in more detail below. According to the present invention, in addition to the refinement of the filaments provided by the muddy airflow, the additional refinement of the filaments is formed parallel to the length of the filaments by applying an external force to the filaments, and the like The external force is obtained by supplying in addition to the airflow or gravity. In a preferred embodiment, the external force like this is provided by a mechanical device, such as a thread tightening device, in the form of a winder or a thread roller. . This device provides a mechanical refinement, which complements and adds the refinement provided by the airflow. In a particular embodiment, the latent filaments can be regenerated before they are tightened by means of a device that provides mechanical refinement. The method practiced in the present invention produces approximately continuously elongated filaments which, once regenerated, are collected as approximately continuously elongated filaments. Continuously extending filaments like this is the opposite of previous meltblown methods, such as those described in International Publication No. W098 / 26122, which produces shorter, discontinuous rayon fibers. The spinning dope is transferred to a rotating device from 70 to a temperature of about 140 C via a pump or extruder at some high temperatures. The temperature of the spinning dope must not be too high, so that the solvent is rapidly decomposed, or too low, so that the spinning dope becomes brittle and cannot be rotated. Recycling solution solvents such as water, mono-water · -12- This paper size applies to China National Standard (CNS) A4 specifications (210X297 public love)

Order

Line 561205 V. Description of the invention (10 NMMO mixtures' low-fat alcohol, or these mixtures NMMO can then be restored from the regeneration tank so that the reused liquid is at a predetermined distance below the extrusion head. Used as a solvent. Better The regeneration solution is used as a fine droplet spray. Figure 2 is a detail of the preferred embodiment of the modified melt-blown method made according to the present invention. The spinning dope supply is guided through an extruder and a positive displacement pump. Not shown, also through line 200 to the extrusion head 204 with multiple orifices. Compressed gas or another gas system is supplied through line 206. Latent filaments 108 are directed from the orifices 340 in the z-direction (see Fig. 3) Extrusion. These spinning dope fine lines 208 are selected by high-speed gas traveling in the Z-direction, which direction is generated by air leaving the intermittent notches 344 (Fig. 3) in the extrusion head. This filament is' effectively elongated and lengthened when it is carried down by the airflow. A suitable point in its travel is now the potential filament line 2 0 8 passing through the opposing nozzle mist line 2 1 0, 2 12 And in contact with a water spray or other regenerating liquid 214. The regenerated filaments The 215 series is selected by a rotating picking roller 216, which will be used to mechanically refine the source of external force. When the selection roller begins to fill, a new wave wheel 2 16 series is introduced to lengthen and Collecting filaments without slowing down production is like using a new roll on a paper machine. The surface speed of roller 216 is faster than the linear speed of falling filaments 215 so that the filaments are mechanically pulled Long. The mechanical force applied to the filament through the thread-tightening device is related to the surface speed of the roller 216, the rate at which the filament is carried by the air flow, and the speed at which the spinning dope is discharged from the nozzle. A mobile porous belt can be used instead of the roller to collect and mechanically elongate the filament and guide it to any required downstream processing. For example, this paper-13- This paper size applies to Chinese national standards ( CNS) A4 specification (210 X 297 male 561205 A7 B7 5. Invention description (11) shows that the roller system operates above a minimum surface speed, and it assigns at least some mechanical refinement to the filament. The roller is Can operate at maximum speed and will be operated by many The element includes the maximum speed at which a continuous filament can be formed. At lower winder speeds, the diameter of the filament is greater than the filament formed when the roller is operated at a higher speed. Continuous filaments have been made using winding machine speeds in the range of about 200-1000 meters per minute. It must be understood that the present invention does not limit one particular type of thread tightening device, other types of thread tightening devices such as conveyors , Belts, rollers, and similar devices can provide satisfactory results. Regeneration solution containing diluted NMMO, or other solvent drops 220 leaving the gathering fiber, enter container 222. From there it is sent to a solvent recovery unit, during which the recovered NMMO can be concentrated and recycled into the process. Fig. 3 shows a cross-sectional view of the preferred extrusion head 300 which is advantageous in the preferred method. A manifold and a spinning dope supply pipe 332 extend longitudinally through the spray holes 340. Within the nozzle, a capillary tube and a plurality of capillary tubes 336 are lowered by the manifold. These reduce the diameter in the transition zone 338 so that it enters the extrusion orifice 340. The air chamber 342 extends longitudinally through the die hole. These are discharged through a cutout 344 positioned immediately adjacent the outlet end of the orifice. The cutouts or notches 344 are intermittently positioned along the length of the head end 300, and are concentrated on the spray hole 340. The width and length of the cutout 344 can vary depending on many factors, such as the volume required to flow through the cutout 334, and the rate at which gas must exit the cutout 334. In general, smaller slots will provide higher gas rates for a given pressure in compartment 342, and larger slots will provide lower gas rates at the same pressure in compartment 342. For the following orifice diameter, with a width of 0.01 inches and a length of 0.25 inches -14- This paper size applies to China National Standard (CNS) A4 (210 X 297 mm) 561205 A7

^ Slot has been found suitable. The internal conduit 346 supplies heat to the electric heating element or steam / oil. The gas supply of the compartment 342 is usually supplied in advance, but it can also be used to control the temperature within the wiper head itself. As described above, the spinning dope is extruded into a flowing air stream, and the air stream travels in a direction substantially parallel to the direction in which the spinning dope is extruded through the orifice 34. The gas leaving the cutout 344 is joined to a predetermined angle to form a single jet which flows along the axis to distinguish the angle formed by the two opposing air streams. In the illustrated embodiment of FIG. 3, the jets exiting the cutout 344 are joined at an included angle of 60 and merge to form a single jet that flows parallel to the extrusion direction of the spinning dope through the cutout 340. Therefore, the average air direction is provided in a direction which is substantially parallel to the direction in which the spinning dope is extruded from the slot 34 and the direction in which the latent filaments travel. Although FIG. 3 illustrates a preferred embodiment of an extrusion head useful as the present invention, it must be understood that other types of extrusion heads are useful as the present invention. For example, U.S. Patent No. 4,380,570 and U.S. Patent No. 5,476,616 are examples of useful extrusion heads. Another suitable extrusion head is the content of gb 2337957A awarded to Law. The capillaries and orifices in the orifices of the extrusion head in Figure 3 can be made in metal unit blocks by any suitable method, such as drilling and electrical discharge machining. Alternatively, since the nozzle hole has a relatively large diameter, the nozzle hole can be processed into a combination mold with matching halves 348, 348 '' (Fig. 3). This shows its effective advantages in terms of processing costs and cleaning. The diameter of the rotating nozzle can be in the range of 300-600 microns, preferably about 400-500 microns, and has a length / diameter ratio in the range of about 2.5-10. It is most hoped that -15- this paper size applies the Chinese National Standard (CNS) A4 specification (210X 297 mm) 561205 A7 ----- ~ _____ V. Description of the invention (13) ^ --- --- with a nozzle Capillary lead with larger diameter. The capillary is suitable for about 12 to 2.5 times the diameter of the orifice and has a length / diameter ratio of about 10-25. The larger nozzle diameter used in this preferred device and method is powerful, one of which is a large output per unit time, for example, the output is equal to or exceeds about 1 gram per minute per nozzle. Furthermore, large-diameter nozzles are almost not like small-sized nozzles, and it is easy to feel the small foreign matter in the spinning dope, or the clogging of non-decomposed substances. If clogging must occur, large nozzles are easier to clean, and because of the low pressure required, the structure of the extrusion head is relatively low. The operating temperature and temperature distribution chart along the nozzle hole and the capillary tube preferably conform to about 70. 〇 to 14〇 It to avoid the rapid deterioration of the spinning dope or solvent. It has been shown that being close to the outlet of the rotary nozzle is advantageous for having a rising temperature. At only one of the possible high temperatures, up to about 14 ° C, during which NMMO starts to decompose quickly, with many advantages. Among these advantages, the 'output rate is roughly increased due to the decrease in viscosity due to the higher spinning dope temperature. Through the orifice temperature Distribution, because the time maintained at or near this temperature is very small, the decomposition temperature can safely reach the exit point. The temperature of the air leaving the melt nozzle can be in the range of 40 ° C-140 ° C, preferably about 70 ° C. The minimum speed of the air stream is preferably greater than the speed at which the spinning dope leaves the orifice, so that at least some refinement of the formed filaments is generated by the air stream. The maximum speed of the gas will depend on the required final speed. In some cases Maximum speed, artificial (discontinuous) fibers will be formed, which is in contrast to continuous filaments that are easy to produce at low airflow speeds. The gas speed can be adjusted in relation to the surface speed of the roller and spinning dope flow rate to suit the airflow distribution The amount of non-mechanical elongation is compared to the mechanical elongation assigned by the tightening device. For example, at the entrance to the 0.25 inch long and 0.010 inch wide slot 344, ranging from about 0.06 to about ι 9 per square -16- This paper scales applicable Chinese National Standard (CNS) Α4 Specifications (210 X 297 mm) 561205 A7 B7

A square inch of air pressure provides a gas velocity just above zero (0) until the speed of sound. As a specific example, when the slot 344 is 0.25 inches long and 0.01 inches wide, the gas in the chamber 342 between about 0.4 pounds per square inch provides a gas rate of about 175 meters per second at the exit of the slot 344. When the stagnant air mixes into the parties and the stagnant air enters the dilated jets produced by these jets of mobile air, the mobile air dramatically slows its rate of exiting the slot 344. As in the present invention, the deceleration of the air must not be so great that the air velocity is lower than the speed at which the filaments are squeezed out of the orifice. The change in the humidity of the gas can affect the properties of the fiber. For example, a gas with a high humidity is more likely to produce a fiber with a smaller diameter than a fiber made with air with a low humidity. It has been observed that the mechanical refinement applied by the thread tightening device has the advantage of providing minimal airflow, which is not sufficient to impart any non-mechanical (such as gas) refinement ', but is sufficiently stable for filaments to be wound around The length of the thread machine. As mentioned above, in the general dry spray wet method, no airflow or a reverse airflow is provided in the air, and it is believed that the lack of airflow in this air gap, which is parallel to the direction of the spinning dope leaving the nozzle, will be the opposite Ground influences the dry spray wet method which can control the foot scale. For example, it is believed that in the general dry jet wetting method, providing a small amount of airflow in the direction of the spinning dope leaving the die hole (for example, insufficient to refine the filament) will stabilize the filament formed by lateral movement Objects that would otherwise cause the immediate filaments to become fused together. In addition, due to the elasticity of the lateral filaments, the direction of the parallel spinning dope leaving the die hole can avoid the rebound of the potential filaments, which can cause the formation of a loop due to their elasticity. Provides an additional benefit of airflow in the direction of the parallel spinning dope exiting the die hole • 17- This paper size is applicable to China National Standard (CNS) Α4 specification (21〇 × 297 mm)

Binding

Thread 561205 A7 B7 V. Description of the invention (15) Regarding the ability of the wire to guide the wire to the thread tightening device after the wire was originally formed by the die hole. Leosai fiber filaments having the following properties have been produced according to the method of the present invention:: about 6 to 17 CV% diameter variability between fibers: about 丨 0 to 22 CV% fibrillation index: about 0 to 1 Fineness: Dry toughness: Wet toughness: Dry lengthening: Wet lengthening: Circuit toughness: Dry modulus: Wet modulus: Bundle strength: Variability along the fiber diameter of about 2.2 to 0.5 d number about 33 to 42 cN / Number about 22 to 28 cN / Number about 11% to 14% About 12% to 15% About 13 to 18 cN / Number about 670 to 780 cN / Number about 170 to 190 cN / Number about 33 to 47 cN / number. Good surface dyeability. The texture of the smooth surface fabric can be changed according to the elongation scale. The method as practiced in the present invention is believed to provide the only opportunity to use the properties of Leocell fiber produced by such a method. After adjusting the orifice diameter, the spinning dope viscosity, extrusion rate, gas velocity, and thread tightening device speed are less than once Neil's Leosai fiber filaments can be produced as in the present invention. Specific examples of the properties of the filaments of the Leosai fiber produced by the method of the present invention are described below. -18-

561205 A7 B7 V. Description of the invention (16) Comparative example 1 Dry spray wet method This comparative example shows the use of a dry spray wet method without the production of air-refined Leosai fiber. The spinning dope is prepared from an acid-treated pulp, which is described in International Publication No. W099 / 47733, which has a hemicellulose content of 13.5%, and an average degree of fiber polymerization of about 600. The treated pulp was dissolved in NMMO to provide a fiber concentration of about 12 weight percent, and was rotated into filaments by a dry spray wet process as described in U.S. Patent No. 5,417,909. The dry jet wetting spin program is directed by the Thuringisches Institute of Textile and Plastic Research. German (TITK) V., Breitscheidstr 97, D-07407 Rudolstadt, and a stagnant air gap, or an air flowing air gap, is transverse to the direction of travel of the filament. This procedure produces filaments cut into rayon. The fiber properties prepared by the dry spray wet method are summarized in Table 1 below DJW-TITK. Comparative example 2 Meltblown method without mechanical thinning process This comparative example illustrates the production of Leosai fiber filaments using a meltblown method without a mechanical thinning process. A spinning dope was prepared from an acid-treated pulp described in International Publication W099 / 47743, Example 10, which has a hemicellulose content of 13.5% and an average degree of polymerization of about 600. This acid-treated pulp was dissolved in NMM0. Nine grams of dry acid-treated pulp was dissolved in a mixture of 0.025 grams of gallic acid propylene, 61.7 grams of 97% NMMO, and 21.3 grams of 50% NMMO to produce a cellulose concentration of about 9.8%. The mold box containing the mixture is immersed in an oil tank at about 120 ° C, and a stirrer is inserted. -19- This paper size applies to China National Standard (CNS) A4 specifications (210X 297 mm) 561205 A7 ___________B7 V. Invention Explanation (17) Among them, the stirring system is continued for 0.5 hours until the pulp 1 is dissolved. The resulting spinning dope was maintained at about 120 t and supplied to a single nozzle experimental solvent nozzle. The diameter of the nozzle hole in the nozzle part is 483 microns and its length is about 2.4 mm, and the length / diameter ratio is 5 cm. A removable coaxial capillary system directly positioned above the orifice is 685 microns in diameter and 80 mm in length, and a length / diameter ratio. The angle between the transition area between the 1 ^ through hole and the capillary is about 1 18 °. The air feed holes are parallel to the cut grooves of the open spray holes positioned at equal distances from each other. The air gap width is 250 micrometers and the full width at the nozzle end is 1.78 mm. 2The angle between the gas cutting groove and the center line of the capillary tube and the nozzle is 30. The spinning dope is fed to the extrusion head through a screw driving forward displacement piston pump. The air velocity was measured at 3660 per minute / meter using a hot-wire device. The air is heated to 60-7 0 C at the discharge point in the electric heating extrusion member. In the temperature range of the capillary without the spinning dope, the temperature ranges from about 8 ° C to about 140 ° C at the inlet end just before the outlet of the nozzle member. It is impossible to measure the spinning of the capillary and the nozzle under operating conditions. Stock solution temperature. The output system is greater than about 1 gram of spinning stock solution per minute. A fine water spray system guides the descending fiber 200 mm below the extrusion head, and the fiber system is tightly threaded on a roller, and the descending The linear speed of the fiber is about 1/4 of the surface speed operation. The properties of the collected fiber are summarized under the item MB in Table 1 below. '' The following examples 1-3 illustrate and describe the method used to produce the Lean + Lean Orsay fiber yarn according to the present invention. The embodiment of the object method, and it is intended for illustration purposes, and is not intended to limit the scope of the present invention. ^ This paper size applies the Chinese National Standard (CNS) A4 specification (210 X 297 mm) -20- 561205 A7 B7 V. Description of the Invention (1S) Example 1 The spinning dope used to make the Leosai fiber filaments is made from kraft pulp dissolved in N-methylmorphine N-oxide. The pulp has an average degree of polymerization of about 600, which Measured by ASTM D 1795-62, and a hemicellulose capacity of about 13%, measured by Weyerhaeuser's Dionex sugar analysis method. The spinning dope is at a rate of 0.625 grams per minute per hole. 20 micron-diameter nozzles are extruded by melt-blown die holes. The holes have a length / diameter ratio of 5. The die holes are maintained at a temperature range from 100 to 130 ° C. The spinning dope is Squeeze into a 12.7 cm long air gap before condensing with a low spray of water. Air is supplied to the head end at temperatures greater than 90 ° C and 20 pounds per square inch. The air cap (shown in Figure 3) The air pressure in chamber 342) is about 0.4 pounds per square inch and flows at a rate of about 18 SCFM. This provides an air velocity of about 175 meters per second from the outlet to the air slot. In this example, the slot system 0.25 inches long and 0.010 inches wide. Downstream of the air gap, the formed filaments are tightened by a winding machine operating at a speed of 500 meters per minute, which is greater than the linearity of the filaments in the air gap. Speed. Water is used to precipitate cellulose from the filaments formed. The water is passed through the winding machine before The mist was used to spray the silk. Four different samples were made using the method described above. The samples were labeled MBA-1 to MBA-4. The collected silk was washed and dried, and It was then subjected to the following procedures to evaluate its fineness (using the TITK test according to DIN EN ISO 1973), dry toughness (using the TITK test according to DIN EN ISO 5079), dry extension (using the TITK test according to DIN EN ISO 5079), wet toughness Degree (using DIN EN ISO 5079 -21-this paper size applies to Chinese National Standard (CNS) A4 size (210 x 297 mm) 561205 A7 _ ___B7_ 5. TITK test of invention description (19)), wet extension (using DIN IEN ISO 5079 TITK test), relative wet toughness (for example, wet / dry toughness), circuit toughness (using TITK test according to DIN DIN 53 843 T2), dry modulus (using TITK according to DIN ENE ISO 5079 Test), wet modulus (using the TITK test of DIN EN ISO 5079), diameter variability CV% (microfiber measurement of 200 fibers versus fiber CV%, and 200 readings from a bundle of strength (by Texas Tech University, International Strong Stanlow fiber in textile center Measured by a force tester), and fibrillation characteristics (individual fibers are placed in a 25 ml test tube with 10 ml of water, and shaken at a low amplitude of about 200 cycles per minute for 24 hours), which is estimated at 0 To the scale of 10, and 0 is low or no fibrillation, as illustrated in Figure 4, and 10 series plateau fibrillation, as illustrated in Figure 5. The above-mentioned "TITK" abbreviation is equivalent to the German company, Thuringisches Institute of Textiles and Plastics Research, which implements the test described. The characteristics of the filaments MBA-1 to MBA-4 are summarized in Table 1. The fibrillation index is determined by viewing SEM photographs of about 100 fiber segments and about 10 microns in length. If 0 to 1 fibrils / fragments are observed, the fiber line is determined to be 0. If each segment contains 5-6 fibrils or the segment becomes a fragment as shown in Fig. 5, a measurement value of 10 is assigned. Table 1 Samples DJW- Newcell ® Filament MBA-1 MBA-2 MBA-3 MBA-4 4 DJW- TITK DJW- TENCEL MB Pulp — Kraft Paper Kraft Paper Kraft Paper Kraft Paper-Kraft Paper Fineness (Number D) 09-3.03 1 .72 1.74 2.15 2. 17 1 .77 1 .70 1 .21 Dry toughness (cN / number) 30-42 37.7 34.7 34.6 33 .3 35.9 44.2 27 .7 Wetness (cN / number) 20- 27 25.5 24.5 26.1 22.7 27.8 32.4 18.2 -22- This paper size applies to China National Standard (CNS) A4 specification (21〇 × 297 mm) 561205 A7 B7 V. Description of the invention (20) Relative toughness (%) — 68 71 75 68 77 73 66 Dry extension (%) 6-10 12.3 12. 1 13.4 11.1 13.0 13 .8 11 .4 Wet extension (%) 8-13 13 .0 13.4 14.6 12.0 14.0 14.5 14.9 Circuit toughness (cN / Number) 18-29 17.8 17.6 13.9 13.4 9.6 10.5 9. 1 Dry modulus (Cn / number) 752 672 701 777 519 829 666 Wet modulus (cN / number) 188 180 181 170 176 212 123 Diameter variability CV% (in fiber) 21.58 10. 12 11.01 13 .88 7.3 5.2 29.5 Diameter variability CV% (along fiber) 7.5 6.9 8.3 7.8 6.1 5.2 13.2 Beam strength (cN / number) 44.0 0 45.23 46.07 33.77 Bundle lengthening (%) — 10.33 10.08 10.33 7.83 One-to-one fibrillation index (estimated by fibril in SEM) 1 0 0 0.5 10 10 0 Mean diameter (micron) — 12.4 13.1 14.2 13.40 13 .5 13 .5 11 .2

Order

The threads MB A—1 to MB A—4 have the same robustness as the commercial Leocell fiber filaments made by a dry spray wet process, which can be used by Newcell GmbH & Co. KG, Kasino Str., 19-21 D-42103, Wuppertal products such as Newcell® (DJW-Newcell®), but with higher dry length than commercial filaments like this. The filaments of Example 1 are also compared with Leosai fiber man-made. 23- This paper size applies the Chinese National Standard (CNS) A4 specification (210X 297 mm) 561205 A7 B7 21 Description of the invention (The fiber has a high loop strength, and the man-made The fiber was prepared from the same spinning dope using the TITK dry-jet wet method described in Comparative Example 1. The fiber of Example 1 also had a higher dry modulus than the Leosai fiber rayon, and the rayon was Prepared using the same spinning dope of the TITK dry-jet wet method of Comparative Example 1. In addition, using the above test, the fiber of Example 1 is less prone to fibrillation than the commercial Leocell fiber, and the fiber TENCEL ② (DJW-Tencel⑧) and DJW-TITK fibers are produced by the dry jet wetting method available to Accordis. Compared with melt-blown Leosai fiber without mechanical drawing (sample MB), this example ι (MBA-1 to MB A-4) fibers have higher dry and wet tenacity, and have lower diameter variability in and along the fiber. This example shows that Leosac fiber has Invention Fineness characteristics of 1 denier. Leosai fiber filaments with denier less than i can be adjusted, such as the viscosity of the spinning dope, the output of the spinning dope in the nozzle, and the winding speed. The above procedure is repeated with the spinning dope samples prepared as described above. The samples for MB A-5 to MBA-17 are stated in Table 2, except that the winding machine speed is set at 220 meters per minute, per minute. The spinning dope is rotated under the above conditions at 350 meters per minute, 400 meters per minute, or 600 meters per minute. The diameter and the coefficient of variability to the diameter are stated in Sample MBA-5 in Table 2 below. To MBA-17. For samples MBA-18 and MBA-19, the spinning dope output was reduced to 0.42 g per minute per hole and 0.25 g per minute per hole, and the winding machine speed was 800 meters per minute. For the samples MBA-18 and MBA-19, the diameter and diameter variability are stated in Table 2. The diameters and diameter variability of MBA-1 to MBA-4 fibers are described in Table 1. • 24- This paper size applies China National Standard (CNS) A4 (210 X 297 mm)

Order

Line 561205 A7 B7 V. Description of the invention (22) Table 2 Sample MBA-5 MBA-6 MBA-7 MBA-8 MBA-9 MBA-10 MB A-11 MBA-12 Average diameter (microns) 17.6 19.9 21 .5 16.5 16.3 21 .6 14.2 13.6 Diameter variability CV% (in fiber) 15 24 30 23 17 25 23 16 Diameter variability CV% (along fiber) Winding speed m / min 220 220 220 350 350 350 500 500 Output per gram 0.625 0.625 0.625 0.625 0.625 0.625 0.625 0.625 0.625 Sample MBA- 13 MBA- 14 MBA- 15 MBA- 16 MBA- 17 MBA-18 MBA-19 MBA-20 Average diameter (microns) 15.7 13.6 13.2 11.8 14.7 9.4 7.2 9.4 Variable diameter CV% (in fiber) 26 19 21 12 16 15 17 21 Variable diameter 4 CV% (along fiber) Winding speed m / min 500 500 500 600 400 800 800 900 Output Gram per hole 0.625 0.625 0.625 0.625 0.625 0.420 0.250 0.625 MB Synthetic filaments from A-5 to MBA-20 are compared with those made without mechanical elongation described in Comparative Example 1 above and Comparative Example 2 below Get The filaments of the melt-blown fiber have a relatively low diameter and low diameter variability-25- This paper size is in accordance with China National Standard (CNS) A4 (210 x 297 mm) 561205

Fig. 6 is a graph showing the average diameter and the average variability coefficient among the filaments of various winding machine speeds described in the application examples of MBA-1 to MBA-16. From this pattern, it is observed that as the winder speed increases, the dry fiber diameter and variability coefficient decrease. Comparative Example 3 In order to produce a silk material using a general melt-blowing method without a mechanical refinement process, except that the winding machine speed is 0 meters per minute, the procedure of Example 丨 uses a spinning dope as described in Example 1. Repeat. Under these conditions, the filaments formed had an average diameter of 26.1 microns and a coefficient of variability in 44% fibers. Example 2 The procedure of Example 1 was repeated using a different air pressure. The speed of the winding machine is 500 meters per minute. In this example, the air pressure supplied to the meltblown head is 1 pound per square inch, which results in a pressure of about 0 • 06 in the air cap (chamber 342 between FIG. 3). This low pressure provides a perceptible air flow in the air cap, which travels at a rate greater than the linear rate at which the filament exits the orifice. The air flow is observed to refine the extruded filaments. The average diameter of the filaments produced was 14 74 microns. The diameter of the filaments is from 64.12 to 7.10 microns. Comparative Example 4 Dry Spray Wet Method The procedure of Example 1 was repeated using a different air pressure and winding speed. In this example, the pressure of the gas supplied to the meltblown head is 0 pounds per square inch ' which results in no airflow in the 2 gas cap member. Under these conditions, the filaments-26- This paper size applies to the Chinese National Standard (CNS) A4 specification (21〇χ 297 mm) 561205 A7 ____ B7 V. Description of the invention (24) Can not be wound at 500 meters per minute Generated at linear speed. At an airless winder speed like this, the extrusion spinning dope system is considered to be broken. It is observed that the air flow is absent in the air gap. When the method is started, the frequency of the extruded filaments cannot find its path to the winding machine, which is greater than the starting method described in its comparative examples 1 and 2. The air flow is provided in the air gap. Example 3 A spinning dope used to make a silk fiber of vegetable orsay is prepared by dissolving in N-methylmorphine N-oxide with an average degree of polymerization of about 750 as measured by ASTM D1795-62, and One was made by Weyerhaeuser's dionex sugar analysis method, measuring about 13% hemicellulose content. The concentration of the cellulose in the spinning dope was about 12% by weight. The spinning dope was extruded at a rate of 0.625 grams per minute per hole by a melt-blown dye with 20 nozzles having 457 micrometer diameter orifices. The orifice has a 5 length / diameter ratio. The nozzle is maintained at a temperature of 100 ° C. To 130. The range of 匚. The spinning dope was squeezed into a 12.7 cm air gap before being condensed with a water spray. Air is supplied to the head end at a temperature greater than 90 ° F and a pressure of about 20 pounds per square inch. The air pressure in the air cap (intermediate chamber 342 of FIG. 3) is about 0.4 pounds per square inch, and flows at a rate of about 18 SCFM. This provides an air rate of about 175 meters per second from the exit to the air slot. Downstream of the air gap, the formed filaments were operated by a winding machine and were fastened at a surface speed of about 900 meters per minute. It is said that the fibrous material is used to deposit cellulose ^ This aqueous system is sprayed onto the fibrous material in preference to the use of the winding machine '. The collected filaments (MBA-20) were washed and dried, and then subjected to the above -27-

561205 A7B7 V. Description of the Invention (25) The test of Example 1 described above is used to evaluate its fineness, dry toughness ~, dry lengthening, wet toughness, wet lengthening, loop toughness, and fibrillation properties. The following values are observed as fineness (d number) 1.12 Dry toughness (cN / number) 42.10 Wet toughness (cN / number) 28.10 Dry extension (%) 10.60 Wet extension (%) 13.10 Circuit toughness (cN / Number) 16.40 Fibrillation Index 2.00 Average Diameter (micron) 9.40 Diameter Variability (CV%) 21.00 -28- This paper size applies to China National Standard (CNS) A4 (210 x 297 mm)

Claims (1)

561205 A8 B8 Y • A method for making Leosai fibers, comprising: making a spinning dope from cellulose; extruding the spinning dope through a plurality of orifices into a flowing air stream; applying a flowing air stream to the filament And applying an external force in a direction parallel to the length of the filament to stretch the filament, the external force does not belong to gas flow or gravity; and regenerate the filament. 2. The method according to item 1 of the scope of patent application, wherein the airflow flows substantially parallel to the direction in which the spinning dope is extruded through the nozzle hole. 3. The method as claimed in item 1 of the patent scope, wherein the external force is provided by a mechanical device. 4. The method according to item 3 of the patent application, wherein the mechanical device is a take-up roller. 5. According to the method of claim 4 in the scope of patent application, the thread tightening device is operated at a surface speed which is greater than the speed at which the filaments are carried by the airflow. 6. The method of claim 3, wherein the mechanical device is a multi-hole belt. 7. The method of claim 3, wherein the porous belt is operated at a surface speed that is greater than the speed at which the filaments are carried by the airflow. 8 · The method according to item 1 of the patent application scope, wherein the step of elongating the flowing air stream 'will reduce the diameter of the filament. 9 · The method of applying for the scope of the first item of the patent, including the step of applying an external force, -29- This paper size applies the Chinese National Standard (CNS) A4 specification (210 X 297 mm) ‘Install Line 561205 A B c D 6. Scope of patent application will reduce the diameter of the filament. 10. The method according to item 5 of the patent application range, wherein the surface velocity ranges from about 200 to about 1,000 per minute per meter. 11. The method of claim 7, wherein the surface velocity ranges from about 200 to about 1,000 per minute per meter. 12.-A type of Leosai fiber is made by the method of the scope of the patent application. 13. If the Leosite fiber of the scope of the patent application is 12, it has a denier of less than about denier. 14. The method according to item 丨 of the patent application, wherein the filaments are stretched to a substantially continuous stretched filament. 15. A melt-blowing method for forming a Leosay fiber, characterized by elongating the fiber by mechanical force in addition to being stretched or stabilized by a moving gas flow. 30- This paper size applies to China National Standard (CNS) A4 (210 X 297 mm)