WO2012002729A2

WO2012002729A2 - Dope for spinning lyocell, method for preparing a lyocell filament fiber using same, and method for preparing a lyocell staple fiber using same

Info

Publication number: WO2012002729A2
Application number: PCT/KR2011/004752
Authority: WO
Inventors: 김우철; 이상목; 정종철; 진상우
Original assignee: 코오롱인더스트리 주식회사
Priority date: 2010-06-30
Filing date: 2011-06-29
Publication date: 2012-01-05
Also published as: EP2589689A2; US20130101843A1; CN103025931B; WO2012002729A3; EP2589689B1; EP2589689A4; CN103025931A

Abstract

The present invention relates to a dope for spinning lyocell, comprising cotton linter pulp and an aqueous solution of N-methylmorpholine-N-oxide (NMMO), to a method for preparing a lyocell filament fiber using the dope, to a lyocell filament fiber prepared by means of the method, to a method for preparing a lyocell staple fiber using the dope, and to a lyocell staple fiber prepared by means of the method. The fiber of the present invention has a low degree of orientation and a low degree of fibrillation and exhibits high elongation even without additional processes, and therefore can be used as fibers for high-quality clothing.

Description

【Specification】

[Name of invention]

Lyocell spinning dope, lyocell filament fiber manufacturing method using the same and lyocell staple fiber manufacturing method using the same

Technical Field

The present invention relates to a lyocell spinning dope, a method for producing lyocell filament fibers using the dope, and a method for producing lyocell staple fibers using the dope. More specifically, a lyocell spinning dope which can provide a lyocell fiber that can be applied as a high-grade garment fiber by showing high elongation with low orientation and fibrillation degree without additional processing, and manufacturing lyocell filament fiber using the dope. The method and the manufacturing method of the lyocell staple fiber using the said dope.

Background Art

Fiber refers to a natural or artificial linear object that is pliable and thin in shape and has a large ratio of length to thickness. These fibers are divided into long fibers, brisket fibers and short fibers in terms of their shape, and are divided into natural fibers and artificial fibers in terms of raw materials.

In the past, fiber has been closely related to human life, and natural fibers such as cotton, hemp, wool and silk fibers have been used as the main raw material for the coating. With the development of science and technology after the Industrial Revolution, textiles have expanded their use not only for coating materials but also for industrial purposes, and the field of artificial textiles has emerged as a new textile material to meet the demand for rapidly increasing fibers with the development of culture and population growth. Pioneered.

The regenerated fibers in these artificial fibers not only have excellent touch and fit, but also have a much faster moisture absorption and discharge capacity than cotton, and thus have been widely used as raw materials for coating. In particular, among such recycled fibers, rayon fibers have excellent gloss and color development and can realize a touch equivalent to that of natural fibers, and have been widely used in the past because they are recognized as harmless materials to the human body. However, these rayon fibers shrink and wrinkle well It has the characteristics of the material that occurs, the manufacturing process is complicated, and many chemicals are used in the process of melting wood pulp, causing environmental problems in the operation or environmental pollution in the process of wastewater treatment.

Accordingly, research on fibers that are harmless to the environment and the human body and which have physical properties superior to those of other fibers has been conducted. Recently, lyocell fibers manufactured from natural pulp and amine oxide hydrates have been introduced. These lyocell fibers have superior tensile properties and tactile properties compared to conventional recycled fibers, and do not generate any contaminants in the production process, and the amine oxide solvents used are recyclable and biodegradable when disposed. As an eco-friendly fiber, it is used in various fields. However, lyocell fibers have excessive fibrils formed on the surface due to high orientation and weak bonding force between fibrils, and thus, the surface texture of the fibers and the quality of the final product are deteriorated. In addition, the removal of fibrils from lyocells requires additional steps such as acidic sallase treatment, which complicates the manufacturing process, increases production costs, and reduces fabric weight and fiber properties during fibril removal. There was also a problem.

Accordingly, there is a demand for the development of a method capable of providing high-quality fibers having low orientation and fibrillation degree by a simple process without adding a step for removing fibrils while maintaining the characteristics of eco-friendly lyocell fibers.

[Content of invention]

[Problem to solve]

The present invention is to provide a lyocell spinning dope to provide a lyocell fiber exhibiting high elongation with a low degree of orientation and fibrillation without additional processing to be applicable to high-grade clothing fibers.

In addition, the present invention is to provide a method for producing a lyocell filament fiber using the lyocell spinning dope. The present invention also relates to lyocell filament fibers prepared from the lyocel spinning dope.

In addition, the present invention provides a method for producing a lyocell staple fiber that exhibits high elongation and excellent strength with low degree of orientation and fibrillation without additional processing, and is suitably applied as a high-grade garment fibers.

In addition, the present invention is to provide a lyo-seal staple fiber produced by the above production method and exhibiting excellent properties that can be suitably applied as a high-grade garment fibers.

[Measures of problem]

The present invention provides a lyocell spinning dope comprising cotton 1 inter pulp, water and N-methylmorpholine-N-oxide (NMMO).

The present invention also comprises the steps of discharging the spinning dope from the spinneret; Passing the discharged dope through a male bath and turning it into a filament; Washing the filament having passed through the arch bath; And it provides a method for producing a lyocel filament fiber comprising the step of drying the washed filament.

The present invention also provides a lyocell filament fiber prepared from the spinning dope.

In addition, the present invention comprises the steps of discharging a spinning dope comprising a cotton linter pulp and an aqueous solution of N-methylmorpholine-N-oxide (NMMO) from the spinneret; Passing the discharged dope through a bath to form a filament; Washing the filament having passed through the arch bath; Drying the washed filaments; Imparting crimp to the dried filament; And it provides a method for producing a lyocell staple fiber comprising the step of cutting the filament imparted with the crimp. The present invention also provides a lyocell staple fiber produced by the manufacturing method. Hereinafter, a lyocell spinning dope, a lyocell filament fiber manufacturing method, a lyocell filament fiber, a lyocell staple fiber manufacturing method, and a lyocell staple fiber according to a specific embodiment of the present invention will be described in detail. According to one embodiment of the invention, there is provided a lyocell spinning dope comprising a cotton 1 inter film, water and N-methylmorpholine-N-oxide (NMM0). Can be.

The present inventors have been researching to solve the biggest problem of lyocell fibers, the high degree of orientation and excessive fibrils formed on the surface of the fiber, and a specific manufacturing method which describes the lyocell spinning dope including a cotton linter filler When applied to, experiments confirmed that lyocell fibers with low degree of orientation and fibrillation can be provided and completed the invention. By using the lyocell spinning dope, since the amount or fibrillation degree of fibrils formed on the surface of the lyocell fiber is very small, not only the surface texture of the fiber and the quality of the final product can be improved. By eliminating additional subsequent steps, the manufacturing process can be simplified and production costs can be reduced. In addition, the lyocell fiber obtained by using the lyocell spinning dope can have a low initial modulus, and can be applied to high-quality clothing fibers such as lining of clothes and innerwear.

In general, cotton that has a long length of fiber separated primarily from seeds is called lint, and cotton that has a second length separated by fiber is called linter. Such linters typically have a fiber length of 3 to 5 mm 3 and can be obtained from annual cotton, which is advantageous in terms of supply and demand of raw materials.

In addition, as will be described later, the cotton linter pulp may contain alpha-cellulose in a high content, for example, it may include 99% by weight or more of alpha-cellulose, and thus exhibit a low degree of fibrillation. It can be used as the fabric of high quality clothing products by containing small amount of impurities. The lyocell spinning dope may comprise a cotton linter filter 6 to 16 weight ¾>. If the content of the cotton linter filter is less than 6% by weight can not implement the fiber properties, if it exceeds 16% by weight it may be difficult to dissolve in the aqueous phase.

In addition, the lyocell spinning dope may contain 84 to 94% by weight of an aqueous solution of N-methylmorpholine-N-oxide as a solvent component. When the content of the N-methylmorpholine-N-oxide aqueous solution is less than 84% by weight is not preferable because the melt viscosity is greatly increased, if the weight exceeds 94weight ¾> spinning spinning viscosity is significantly lowered to produce a uniform fiber in the spinning step It can be difficult to do.

The weight ratio of N-methylmorpholine-N-oxide and water in the N-methylmorpholine-N-oxide aqueous solution may be 91: 9 to 83:17. When the weight ratio of the N-methylmorpholine-N-oxide and water is greater than 91: 9, the dissolution temperature is increased, so that decomposition of the cellulose may occur when dissolving salose, and when the weight ratio is less than 83:17, Dissolution performance of the cellulose may be difficult to dissolve.

The lyocell spinning dope is swelled with N-methylmorpholine-N-oxide (NMM0) and cotton lint filler in an N-methylmorpholine-N-oxide aqueous solution containing water in a weight ratio of 90:10 to 50:50. After the weight ratio of N-methylmorpholine-N-oxide (N 0): water is 93: 7 to 85:15, the final content of the film is 6 to 16 weight ¾ », more preferably 10 to 14 weight% It may be prepared according to a process of removing water if possible. On the other hand, according to another embodiment of the invention, the step of discharging the lyocell spinning dope from the spinneret; Passing the discharged dope through a bath to form a filament; Washing the filament having passed through the arch bath; And it may be provided a method for producing a lyocel filament fiber comprising the step of drying the washed filament.

The present inventors have found that when the lyocell spinning dope containing the cotton linter filler is applied to a specific manufacturing method, the highest problem of lyocell fibers is high. It was confirmed through experiments to solve the degree of orientation and excessive fibrils formed on the fiber surface, and to provide an environment-friendly lyocell fiber of excellent quality and completed the invention. According to the method for producing the lyocell filament fiber, since the lyocell fiber having a very small amount of fibril or fibrillation degree formed on the surface can be obtained, there is no need to install an additional process for removing fibrils. The process can be simplified and production costs can be reduced. In addition, according to the above manufacturing method, not only the surface texture of the fiber and the quality of the final product are excellent, but also the low initial elastic modulus can be obtained lyocell filament fiber that can be applied to high-quality medical materials such as lining of clothes, underwear, etc. .

Since the contents of the lyo-seal spinning dope have been described above, a detailed description thereof will be omitted.

The spinneret serves to discharge the fibrous filaments through the air contact to the vault liquid. Discharging the spinning dope from the spinneret may be performed ^at 80 to 130 ^° C.

In addition, after the spinning dope is discharged, the step of passing it through the air gap may be additionally performed. At this time, the air gap serves to pre-quench the liquid dope by supplying air to the dope discharged from the spinneret. At this time, since the stretching viscosity of the dope is higher than the general dope, the temperature of the supplied air (air) may be 5 to 30 ^° C, preferably 5 to 20 ^° C in order to proceed smooth spinning process.

In addition, the air volume of the air provided in the air gap may be 10 to 300 m ³ / hr, preferably 30 to 100 m ³ / hr. When the air volume of the air is too small, cutting by uneven stretching occurs, which is not preferable. When the air volume is excessively large, cutting by spin angle of the spinneret is not preferable.

The dope discharged from the spinneret and selectively passed through the air gap is submerged in a subculture bath to form a filament, wherein the temperature of the subculture bath may be 30 ^° C. or less. This means that the uneven temperature is below 30 ^° C It is not so high that it is necessary to maintain the proper high speed. Here, the male bath is not particularly limited because it can be prepared and used in a conventional composition in the art.

On the other hand, the method for producing a lyocell filament fiber may comprise the step of washing the filament passed through the arch bath, and the step of drying the washed filament.

In the step of washing the filament passed through the coagulation bath, in consideration of the ease of recovery and reuse of the solvent after washing, it can be used as a washing liquid of 0 to 100 ° C temperature, water can be used as the washing liquid If necessary, other additives may be further included.

The drying of the washed filaments may be performed at 80 to 200 ^° C., preferably at 100 to 150 ^° C., to impart a tension of 0.1 to 2 g / d, preferably 0.2 to 0.5 g / d, to the filament. It may include a step. The drying step may be carried out in a drying process of one step, it may also be carried out in a multi-stage drying process to vary the drying process conditions by dividing the interval. Specific drying conditions of each step in the multi-stage drying process can be arbitrarily selected as needed within the tension and temperature range, in addition to the above conditions, can be used in the technical field to which the present invention belongs. Meanwhile, FIG. 1 briefly illustrates an example of a spinning apparatus that can be used for producing lyocell filament fibers. Referring to the configuration of Figure 1, the general type of lyocell multifilament manufacturing apparatus is a gear pump for supplying the spinning stock solution at a constant pressure, spinning the spinning stock solution supplied from the extruder in the form of fibers A spinneret 12 to be provided, a first bather 14 for laying down the uneven fiber 13 discharged from the spinneret, and a second bather 15 if necessary. The filament having passed through the above baths 14 and 15 removes the solvent and the like contained in the spinning dope and the like by water in the washing device 17 by the driving of the traction roller 16. Subsequently, the filament passed through the washing apparatus may be dried in the drying apparatus 18 and then wound to obtain a final lyocel filament. However, these radiators are lyocell filaments It is only one example that can be used for the production of the fibers, and the manufacturing method and manufacturing apparatus applicable to the present invention are not limited to the above description and FIG. 1. On the other hand, according to another embodiment of the invention, there may be provided a lyocell filament fiber prepared from the lyocell spinning dope.

As described above, it has been found through experiments that lyocell spinning dope containing cotton linter pulp can be applied to a specific manufacturing method to provide lyocell fibers with a low degree of orientation and fibrillation.

The lyocell fibers obtained by applying the lyocel spinning dope to a specific manufacturing method have a very small amount of fibrils formed on the surface or a degree of fibrillation. As described above, not only the surface texture of the fiber and the quality of the final product are excellent, but also the low initial elastic modulus can be easily applied to high quality garment fibers such as lining of clothes and innerwear.

Accordingly, the lyocell filament fibers may have a degree of fibrillation of at least one grade. The degree of fibrillation refers to the degree of fibril generation on the surface of the filament. Specifically, the fibrillation is generated by rubbing the fibers with each other for a predetermined time with respect to the fiber in the state of being dipped in water, and the fibrillation It may mean a value measured from an image obtained by observing under a microscope. This 'fibrillation degree' can be represented by the following general formula (1), the lower the number of fibrils generated has a higher degree of fibrillation degree.

[Formula 1]

Fibrillation degree (grade) = number of fibrils / filament unit length (0.1 隱)

Rating 0 = Fibril 0

1 rating = number of fibrils <10

2 ratings = number of fibrils <20

3 ratings = number of fibrils <50

4 ratings = number of fibrils <100 pieces

5 ratings = number of fibrils> 100 pieces In the degree of pebble (grade), the 0 grade is the highest grade. As shown in Experimental Example 1 to be described later, the lyocel filament fibers may have an initial modulus of 150 to 230 g / d. In addition, the lariocell filament fibers may have a strength of 4 to 8 g / d. The initial modulus and strength may be measured after drying the lyocell filament fibers prepared from the lyocell spinning dope in an oven at 105 ^° C for 2 hours.

The lyocell filament fibers can be easily applied to high-quality garment fibers, such as clothes lining and innerwear, while exhibiting a low initial modulus while having a suitable strength for garments. According to another embodiment of the invention, a spinneret comprising a cotton linter pipe and a spinning dope comprising an aqueous solution of N-methylmorpholine-N-oxide (NMM0) Ejecting from the; Passing the discharged dope through a bath to form a filament; Washing the filament having passed through the coagulation bath; Drying the washed filaments; Imparting crimp to the dried filament; And cutting the crimped filaments.

As described above, the results of the inventors of the present invention, according to the specific manufacturing method using a lyocell spinning dope containing a cotton linter filter, it can be confirmed that lyocell fibers with a low degree of orientation and fibrillation can be produced without additional processing It became. That is, when the lyocell spinning dope containing the cotton linter pulp is used, the amount of fibrils formed on the surface of the lyocell fibers or the degree of fibrillation is very small, so that the surface texture of the fibers and the final product Not only can the quality be improved, but further omissions such as acid sallase treatment can be omitted to simplify the manufacturing process and reduce the production cost. And obtained using the said lyocell spinning dope Lyo Sal fibers can have high strength and elongation, and can be applied to high-quality garment fibers such as lining of clothes and undergarments.

In addition, according to the above-described manufacturing method, it is possible to manufacture a lyo-seal staple fiber, which is an optimized form that can be applied as a high-grade garment fiber among lyo-seal fibers through a relatively simplified manufacturing process.

Therefore, by the above-described manufacturing method, it is possible to easily manufacture a lyo-seal staple fiber having a shape that is simplified and has excellent physical properties according to low degree of orientation and fibrillation degree, and is suitably applied as a high-quality garment fiber. .

The spinning dope used in the method for producing the lyocell staple fiber is as described above.

In the method for producing a lyocel staple fiber, the step of discharging the spinning dope comprising the cotton linter pulp and N- methylmorpholine-N-oxide aqueous solution from the spinneret; Passing the discharged dope through a bath to form a filament; Washing the filament having passed through the unacquaintance bath; And specific details about the step of drying the washed filament, it can be applied in the same manner as described above in the 'method of producing a lyo-seul filament fiber'.

After the filament is dried, a crimp is applied to the filament. This crimping step can be carried out in conventional crimping devices which have been applied to the production of various synthetic staple fibers. And, in this crimping step, in order to finally produce a lyocell staple fiber having excellent physical properties, the filament may be given a crimp of 8 to 20 / inch, preferably 10 to 16 / inch. . After imparting crimp in such a range, the lyocell staple fiber is manufactured through a subsequent cutting process, thereby exhibiting excellent touch and physical properties, thereby obtaining a fiber that can be more preferably applied as a high-quality garment fiber.

After imparting crimp to the filaments, these filaments may be cut to produce lyocel staple fibers. At this time, the lyocell In order to enable the staple fiber to be preferably used as a high-quality garment fiber or the like, in the cutting step, the filament may be cut to a length of 20 to 200 mm 3, preferably 30 to 130 mm. Accordingly, a lyocell staple fiber having a length corresponding to this can be produced, and such lyocell staple fiber can have an optimized form as a fiber for high-quality clothing.

On the other hand, Fig. 2 briefly illustrates an example of a spinning apparatus that can be used for producing lyocell staple fibers. Referring to the configuration of FIG. 2, in the lyocell staple manufacturing apparatus, the cotton linter filter is pulverized and stored, and the filter is dissolved in a concentrated solvent, that is, an aqueous N-methylmorpholine-N-oxide solution, and a spinning stock solution, In other words, it forms a spinning dope. Since the method of forming the spinning dope has already been described above, further detailed description thereof will be omitted.

In addition, the manufacturing apparatus is provided with a spinneret to spin the spinning stock solution in the form of fibers, and has a bathing bath for uncoiling the uneven fiber discharged from the spinneret. The filament having passed through the arch bath removes the solvent and the like contained in the spinning dope and the like by water in the washing apparatus by driving the traction lor. Subsequently, the filament passed through the water washing device may be imparted with an emulsion, dried in a drying device, and then crimped in a crimp device, cut into a predetermined length, and finally made into a lyocel staple fiber.

The above-mentioned spinning apparatus of FIG. 2 is just one example that can be used for the production of lyocell staple fibers, and the manufacturing method and manufacturing apparatus applicable to the present invention are not limited to the above description and FIG. 2. On the other hand, according to another embodiment of the invention, there is provided a lyocel staple fiber produced by the above-described manufacturing method. These staple fibers have a length of 20 to 200 mm can be suitably applied as a high-end garment fibers. In addition, since the amount of fibrils formed on the surface or the degree of fibrillation of the lyocell staple fiber obtained by applying to the above-described manufacturing method is very small, for example, the degree of fibrillation may be 1 grade or more. Therefore, the staple fibers not only have excellent surface feel and quality of the final product, but also have high strength and elongation, and thus can be suitably applied to high-quality garment fibers such as linings and undergarments of clothes. The definition of 'degree of view' is as described above.

As shown in the experimental example to be described later, the lyocell staple fiber may have a breaking elongation of 3 to 8g / d strength and 9.5 to. These strengths and elongations were pre-dried to a final moisture level and shortly after the filament specimens were made into staple fibers for 2 hours or less at 110 ^° C for 2 hours, and then left at the standard condition of KSK 0901 (fiber test room standard) for more than 24 hours. After reaching the water equilibrium state, it may be measured at a tensile speed of 300m / min using an instru- ment's slow elongation type tensile tester.

Such lyocell staple fibers can be easily applied to high-quality garment fibers such as lining of clothes, innerwear, etc., as they exhibit proper elongation and excellent strength for garments.

【Effects of the Invention】

According to the present invention, a lyocell spinning dope which can provide a lyocell fiber that can be applied as a high-grade garment fiber by showing high elongation with low orientation and fibrillation degree without an additional process, the lyocell filament fiber using the dope A manufacturing method and a lyocell filament fiber obtained therefrom and a method for producing a lyocell staple fiber using the dope and a lyocell staple fiber obtained therefrom may be provided.

[Brief Description of Drawings]

1 is a simplified illustration of an example of a spinning apparatus that can be used to make lyocell filament fibers.

2 briefly illustrates an example of a spinning apparatus that may be used to make lyocell filament fibers. [Specific contents for implementation of the invention]

The invention is explained in more detail in the following examples. However, the following examples are merely to illustrate the invention, but the content of the present invention is not limited by the following examples.

Example 1 Preparation of Lyocell Filament Fibers from Cotton 1 Inter Pils

A cotton linter pulp with a degree of polymerization (DP) 1200 (provided by Mint) was placed in a mill equipped with a 100 mesh filter to produce pulp powder having a diameter of 1700 or less.

The pulp powder was swollen in 50 wt% NMM0 aqueous solution. At this time, the content of pulp in the NMM0 aqueous solution was 6 weight ¾, and an antioxidant was added so as to be 0. 2 weight ¾ to the cotton linter filter.

The swelled peel slurry was injected at a rate of 16 kg / hour with a rotary valve pump to a kneader maintained at an internal temperature of 90 ^° C. and maintained at an absolute pressure of 50 mmHg. The spinning dope was discharged through the discharge screw after completely dissolving the pulp while removing the excess water to the aqueous solution.

The spinning dope was adjusted to have a final filament total fineness of 1,650 deniers and spun using a nozzle having 1000 nozzles and a nozzle cross section of 0.47 mirf. At this time, an air gap of 30 mm was placed between the nozzle and the male bath, and the air gap was supplied to the dope discharged at a flow rate of 30 mVhr at 15 ^° C.

The multifilament unfolded in the uneven bath through the air gap is

After washing with water in a five-stage washing equipment, an undried multifilament yarn having a water content of 170% was dried in a three-stage drying to obtain a lyocell multifilament yarn. At this time, the drying between the first and second stage The tension was 0.2 g / d, the tension between the 2nd and 3rd stages was adjusted to 0.5 g / d, and the temperature of each drying was sequentially adjusted to 100 ^° C, 130 ^° C, and 150 ^° C. The filament number of the lyocell filament yarn manufactured by the above method was 1000, and the average fineness was 1.5 d. Example 2 Preparation of Lyosal Filament Fibers from Cotton 1 Inter Pils

A lyocell multifilament yarn was obtained in the same manner as in Example 1, except that cotton linter pulp having a degree of polymerization (DP) 800 was used. Example 3 Preparation of Staple Fibers from Cotton 1 Inter Pulp A cotton 1 inter filter (provided by Mint) with a degree of polymerization (DP) 1200 was placed in a grinder equipped with a 100 mesh filter and had a diameter of 1700 /. Pulp powder of im or less was prepared.

The peel powder was swollen in a 50 weight ¾> NMM0 aqueous solution. At this time, the content of pulp in the NMM0 aqueous solution was 6% by weight, and an antioxidant was added so as to be 0.01 weight ¾> with respect to the cotton linter filter.

50% by weight of NMM0 aqueous solution was 89 weight ¾ NMM0 while the swollen puff slurry was maintained at an internal temperature of 90 ^° C. and injected at a rate of 16 kg / hour with a rotary valve pump to a kneader maintained at an absolute pressure of 50 mmHg. The spinning dope was discharged through the discharging screw after completely dissolving the felt while removing excess water to make an aqueous solution.

The spinning dope was adjusted so that the final filament total fineness was 45,000 denier and spun using a nozzle having 30,000 nozzles and a nozzle diameter of 0.2 kPa. At this time, an air gap of 50 kPa was provided between the nozzle and the male bath, and the air gap was supplied to the dope discharged with the air volume of 1,500 m ³ / hr at 15 ^° C. The multifilament magnified in the unfold bath through the air ¾ is

After washing with water in an 8-stage washing machine, it was immersed in oil and then dried in a three-stage drying of an undried multifilament yarn with a water content of 250% to obtain a lyocell multifilament yarn. At this time, the drying was adjusted to 0.2 g / d for the tension between the first and second stages, and 0.5 g / d for the tension between the second and third stages, and the temperatures of each drying furnace were 130 ° C, 150 ° C, and Adjusted to 170 ° C.

The filament number of the lyocell filament yarn manufactured by the above method was 30,000, and the average fineness was 1.5 d. The dried filament bundles (tow) were given 13 / inch crimps in the crimp unit, and the crimped toes were completely dried at 120 ^° C in a tensionless dryer (latis dryer) and cut into 38 隱 for cotton swabs. To prepare staple fibers. Example 4 Preparation of Staple Fibers from Cotton 1 Inter Pulp

A lyocell staple fiber was obtained in the same manner as in Example 3 except for the use of a cotton linter filter with a degree of polymerization (DP) 800.

Comparative Example

Comparative Example 1: Preparation of lyocell filament fibers from softwood peel sheet Softwood peel sheet (V81, DP 1200 from buckeye) was put into a grinder equipped with a 100 mesh filter to prepare a peel powder having a diameter of 1700 or less.

The peel powder was swollen in 50 weight ¾ NMM0 aqueous solution. At this time, the content of the filler in the NMM0 aqueous solution was 6% by weight, and the antioxidant was added to 0.01% by weight relative to the cotton linter (cotton 1 inter).

50% by weight of NMM0 aqueous solution was 89 weights ¾, while the swollen peel slurry was injected at a rate of 16 kg / hour with a rotary valve pump to a kneader maintained at an internal temperature of 90 ^° C. and maintained at an absolute pressure of 50 mmHg. To be NMM0 aqueous solution After dissolving the excess water and completely dissolving the dope, the spinning dope was discharged through the discharge screw.

The spinning dope was adjusted to have a final filament total fineness of 45,000 denier and spun using a nozzle having a nozzle number of 30,000 and a nozzle diameter of 0.2 kPa. At this time, an air gap of 50 mm was placed between the nozzle and the male bath, and in the air gap, 15 ^° C. cooling air was supplied to the dope discharged at a flow rate of 1,500 m ³ / hr.

The multifilament solidified in the unsupervised bath after passing through the air gap was washed with water in an eight-stage washing equipment, and then immersed in oil and then dried in three stages of undried multifilament yarn having a water content of 250%. The constructed drying was dried at to obtain a lyocel multifilament yarn. At this time, the drying was adjusted to a tension between the first and second stages of 0.2 g / d, the tension between the second and third stages of 0.5 g / d, and the temperature of each drying furnace was sequentially 130 ° C, 150 ^° C, and Adjusted to 170 ^° C.

The filament number of the lyocell filament yarn manufactured by the above method was 30,000, and the average fineness was 1.5 d. The dried filament bundle (tow) was given 13 / inch crimp in the crimping device, and the crimped tow was completely dried at 120 ^° C in a tensionless dryer (latis dryer) and then cut into 38mm for cotton yarn to staple fibers. Was prepared. Comparative Example 2: Preparation of lyocell filament fibers from softwood pulp sheet A softwood filler sheet (V-60, DP 800, manufactured by Buckeye) was put into a grinder equipped with a 100 mesh filter and manufactured into a powder of filler having a diameter of 1700 zm or less. The lyocell filament fibers were manufactured in the same manner as in Comparative Example 1. Comparative Example 3: Preparation of Staple Fibers from Softwood Peel Sheets

Softwood peel sheets (V81, DP 1200 from buckeye) were put in a mill equipped with a 100 mesh filter to prepare pulp powder having a diameter of 1700 or less. The peel powder was swollen in a 50 weight ¾ NMM0 aqueous solution. At this time, the content of pulp in the NMM0 aqueous solution was 6% by weight, and an antioxidant was added to 0. 2% by weight based on the cotton linter (cotton 1 inter) filter.

The swelled peel slurry was maintained at an internal temperature of 90 ^° C. and injected at a rate of 16 kg / hour with a rotary valve pump at a kneader maintained at an absolute pressure of 50 mmHg. The spinning dope was discharged through the discharge screw after completely dissolving the pulp while removing the excess water to the aqueous solution.

The spinning dope was adjusted to have a final filament total fineness of 45,000 deniers, and spun using a nozzle having a number of 30,000 nozzles and a nozzle diameter of 0.2 mm 3. At this time, an air gap of 50 mm was placed between the nozzle and the male bath, and the air gap was supplied to the dope discharged with the air volume of 1,500 m ³ / hr at 15 ^° C.

The multifilament, which was uncoiled in the unsupervised bath through the air gap, was washed with water in an 8-stage washing equipment and then immersed in oil, and then composed of three stages of undried multifilament yarn having a water content of 250%. Drying was dried at to give a lyocell multifilament yarn. At this time, drying was adjusted to the tension between 1st and 2nd stage 0.2g / d, tension between 2nd and 3rd stage was 0.5g / d, and the temperature of each drying furnace was 130 ° C, 150 ° C, and 170 Adjusted to ° C.

The filament number of the lyocell filament yarn manufactured by the above method was 30,000, and the average fineness was 1.5 d. The dried filament bundle (tow) was given 13 / inch crimp in the crimping device, and the crimped toe was completely dried at 120 ^° C in a tensionless dryer (latis dryer) and then cut into 38 隱 for cotton swabs. Fibers were prepared. Comparative Example 4: Preparation of Staple Fibers from Softwood Sheets Softwood pulp sheets (V-60, buckeye Co., Ltd. DP 800) were put into a mill equipped with a 100 mesh filter to prepare pulp powder having a diameter of 1700 or less, and staple fibers were prepared in the same manner as in Comparative Example 3. Experimental Example

Experimental Example 1 Measurement of Tensile Strength and Initial Elastic Modulus of Lyocell Filament Fiber According to the American Society for Testing and Materials (ASTM) D-885, a universal testing machine (Model 5566, Instron) was used in the above Examples and Comparative Examples. The strength and elongation of lyocell filament fibers were measured at room temperature. For this measurement, the lyocel filament fibers obtained in Examples 1 and 2 and Comparative Examples 1 and 2 were dried in an oven at 105 ^° C. for 2 hours.

Specific measurement conditions are as follows, and the measurement results are expressed as the average value of 10 replicates.

(1) tensile strength

1) Crosshead Speed: 300 画 / min

2) Experimental error: 士 1 MPa

(2) Initial modulus

1) Head Speed: 300mm / min

2) Grip Distance: 250 隱

3) 25 ^° C. and 60 RH% Atmosphere Experimental Example 2: Measurement of lyocell staple fiber tensile strength and elongation at break First, final cutting was performed in each of Examples 3 to 4 and Comparative Examples 3 to 4 to measure tensile strength and elongation at break. Immediately before the filament bundle was extracted with the specimen. The length of these specimens was adjusted to 250 mm 3.

After pre-drying each specimen to below process moisture content for 2 hours under 1KTC temperature, it is allowed to stand at least 24 hours in the standard condition of KSK 090K fiber test room) to reach equilibrium, and then The tensile strength and the elongation at break were measured at a tensile speed of 300 m / min using a tensile tester. Experimental Example 3 Measurement of Alpha-Cellulose Content of Raw Material Filter

The pulverulent powder in the examples and comparative examples was immersed in a 17.5% NaOH solution at 2 () ° C. for 20 minutes, and then the weight of the undissolved material was measured by drying. At this time, the material that does not dissolve is alpha cellulose, the content was calculated according to the following general formula (2).

[Formula 2]

Alphacellulose content of raw pulp (¾>) = W / S X 100

[W = dry fiber weight (g), S = dry weight of Pulp sample (g)] Experimental Example 4: Fibrillation degree measurement

A lyocell obtained in the above examples and comparative examples using a device that injects and seals the filament O.lg cut to 5 mm and pure water 1ml into a cylindrical cylinder having a diameter of 10 mm long and 30 mm long and then reciprocates 10 times per second. The degree of fibrillation of the filament fibers was measured. Specific measurement methods and conditions are as follows.

An image of fibrils generated by an optical microscope was analyzed to determine the number of fibrils generated per unit length. This degree of fibrillation can be represented by the following general formula (1).

[Formula 1]

Fibrillation degree (grade) = number of fibrils / filament unit length (0.1 瞧) _

Class 0 = Fibrill 0

Grade 1 = number of fibrils <10

Tier 2 = number of fibrils <20

Tier 3 = number of fibrils <50

Grade 4 = number of fibrils <100 Grade 5 = number of fibrils> 100 The results of Experimental Examples 1 to 4 are shown in Table 1 below.

TABLE 1

Referring to Table 1, it was confirmed that the lyocell staple fiber prepared in the example exhibited higher strength and remarkably superior fibrillation degree while showing an elongation equal to or higher than that of the conventional comparative fiber. Therefore, it was confirmed that the staple fiber of the embodiment can be used suitably as a high-quality apparel fiber, etc., while exhibiting excellent texture and the like with excellent fibrillation while maintaining excellent strength and elongation. [Explanation of code]

11: gear pump

12: Radiation detention

13: Miungo fiber

14 ： The first unpleasant bath

15: the second unpleasant desire

16: towing

17 ： washing machine

18: drying device

Claims

[Patent Claims]

[Claim 11

Cotton linter pulp; And

A lyocell spinning dope comprising an aqueous solution of N-methylmorpholine-N-oxide (N-methy lmorphol i ne-N-ox i de; NMMO).

[Claim 2]

The method of claim 1,

Cotton 1 inter pulp 6-16 weight ¾; And

A lyosal spinning dope comprising 84 to 94% by weight of an aqueous N-methylmorpholine-N-oxide solution.

[Claim 3]

The method of claim 1,

The lyocell spinning dope in which the weight ratio of N-methylmorpholine-N-oxide and water in the N-methylmorpholine-N-oxide aqueous solution is 91: 9 to 83:17.

[Claim 4]

The method of claim 1,

The cotton linter filler lyosal spinning dope comprising an alpha-cel lulose of 99% by weight or more.

[Claim 5]

Discharging the spinning dope of any one of claims 1 to 4 from a spinneret;

Passing the discharged dope through a bath to form a filament; Washing the filament having passed through the arch bath; And

Method for producing a lyocell filament fiber comprising the step of drying the washed filament.

[Claim 6]

The method of claim 5,

Discharging the spinning dope from the spinneret is a method for producing a lyocel filament fiber made ^at 80 to 130 ^° C.

[Claim 7]

The method of claim 5,

Drying the washed filament is a method of producing a lyocell filament fiber comprising the step of imparting a tension of 0.1 to lg / d to the filament at 80 to 200 ^° C.

[Claim 8]

A lyocell filament fiber made from the spinning dope according to claim 1.

[Claim 9]

The method of claim 8,

Lyocell filament fibers having a degree of fibrillation of at least a grade.

[Claim 10]

The method of claim 8,

A lyocel filament fiber having 4-8 g / d strength and an initial modulus of 150-230 g / d.

[Claim 111]

Discharging a spinning dope comprising a cotton linter film and an aqueous solution of N-methylmorpholin ine-N-oxide (NMM0) from the spinneret; Passing the discharged dope through a coagulation bath to form a filament; Washing the filament having passed through the arch bath;

Drying the washed filaments;

Imparting crimp to the dried filaments; And

Method for producing a lyocell staple fiber comprising the step of cutting the filament imparted with the crimp.

[Claim 12]

The method of claim 11,

In the step of applying the crimp, to the filament

A process for producing a lyocel staple fiber that imparts 8-20 pieces / inch crimp.

[Claim 13]

The method of claim 11,

In the cutting step, the method for producing a lyo-seal staple fiber to cut the filament to a length of 20 to 200mm.

[Claim 14]

A lyocel staple fiber prepared by the manufacturing method according to any one of claims 11 to 13, having a length of 20 to 200 mm, and having a degree of fibrillation of at least one grade.

[Claim 15]

The method of claim 14,

Lyocell staple fiber with 3-8 g / d strength and elongation at break of 9.5-12.0¾.