WO2006016753A1

WO2006016753A1 - Functional synthetic fiber and method of producing the same

Info

Publication number: WO2006016753A1
Application number: PCT/KR2005/002546
Authority: WO
Inventors: Won-Bae Kim
Original assignee: Kim, Sang-Bo
Priority date: 2004-08-11
Filing date: 2005-08-04
Publication date: 2006-02-16
Also published as: KR100749762B1; KR20060014646A

Abstract

Disclosed is a functional synthetic fiber and a method of producing the same. The method includes wet-pulverizing a functional material so that a particle size of the functional material does not exceed 1/3 of a desired fiber diameter, drying the pulverized functional material, and re- pulverizing the dried functional material so that the particle size of the dried functional material does not exceed 3/4 of the desired fiber diameter, to produce a master batch chip. The production of the functional synthetic fiber is consecutively carried out for 3 days or more, and the functional synthetic fiber has deodorization, antibacterial properties, whiteness of 93 % or more, and tenacity of 3.8 g/d or more. The functional synthetic fiber is advantageous in that it is possible to conduct consecutive production for 3 days or more, excellent deodorization and an¬ tibacterial properties are assured, and whiteness and tenacity are improved to a level similar to a typical synthetic fiber, thereby avoiding the disadvantages of conventional functional synthetic fiber.

Description

FUNCTIONALSYNTHETICFIBERANDMETHODOF

PRODUCINGTHESAME

Technical Field

[1] The present invention relates, in general, to a functional synthetic fiber and a method of producing the same and, more particularly, to a functional synthetic fiber which has excellent properties, such as whiteness, antibacterial properties, and de- odorization, and which assures excellent productivity, and a method of producing the same. Background Art

[2] Since synthetic fiber has poorer absorption ability than natural fiber, it provides an environment suitable for bacteria, molds and the like due to sweat and miscellaneous organics secreted by humans, and thus, it may emit an offensive odor and infect humans in extreme cases because of the propagation of microorganisms.

[3] To avoid the above disadvantages, much effort has been made to produce a synthetic fiber having excellent antibacterial properties and deodorization by conducting antibiotic and deodorization processes, by reforming a polymer, or by employing an antibiotic material in a post-process. A method of spraying a liquid treating agent containing a functional material on a fiber in a post-process to achieve a coating is disclosed in Japanese Pat. Laid-Open Publication Nos. Sho. 59-134418 and 61-17567, but the above patents are problematic in that the functions of products man¬ ufactured according to the method are not maintained for a long time.

[4] Methods of adding functional inorganic materials to a synthetic fiber, particularly a polyester fiber, may be usually classified into polymerization and master batch methods. Of them, the polymerization method mixes inorganic powder with ethylene glycol, which acts as a raw material in a polymerization process conducted to produce a chemical resin for fibers, in a slurry state, and feeds the resulting slurry into a poly¬ merization device to complete the polymerization. However, the polymerization process is problematic in that when silver (Ag) ions are used as a functional material, the silver ions react on the high temperature polymerization, bringing about dis¬ coloration of a polyester compound into dark gray or yellow gray. Since a grey yarn of a fiber produced using the discolored compound has poor properties, it is valueless as a fiber. Korean Pat. Laid-Open Publication No. 1998-0033454, entitled "Process of producing a polyester fiber having antibiotic and deodorization functions", may be cited as an example.

[5] The master batch method includes producing a master batch chip, in which a functional material is contained in a resin chip in a high concentration, using an extruder, and spinning the master batch chip in conjunction with another resin containing no functional material to produce a grey yarn. The method is advantageous in that, unlike the polymerization method, discoloration does not occur even though silver ions are used as the functional material, but has a disadvantage of cohesion of the functional material in the master batch. The conventional master batch method is disadvantageous in that the cohesion of the functional material causes clogging of a filter and increased pack pressure during a spinning process, and thus, it is practically impossible to produce the fiber. Korean Pat. No. 83808, entitled "An artificial fiber containing a native stone and its fiber products", and Korean Pat. No. 267351, entitled "A method of producing an illite synthetic fiber" may be taken as instances.

[6] To avoid the above disadvantages, Korean Pat. Laid-Open Publication Nos.

2004-004559 and 2004-0016676 employed inorganic particles which include particles having an average particle size of 0.5 D or less in an amount of 60 % or more so as to prevent cohesion of a functional material. However, since the above patents un¬ desirably prevent the cohesion of the inorganic particles, it is impossible to produce a synthetic fiber having desired properties, and it is impossible to realize mass- production because of poor workability.

[7] For example, it is impossible to realize consecutive production for 24 hours or more using a polyester staple fiber for clothes containing 1 wt% or more of functional material. Consecutive production must be carried out for at least 3 days, preferably 5 days or more, and more preferably 7 days or more in order to assure economic efficiency in the course of producing the synthetic fiber. Disclosure of Invention Technical Problem

[8] Therefore, the present invention has been made keeping in mind the above problems occurring in the prior arts, and an object of the present invention is to provide a functional synthetic fiber having excellent antibacterial properties and deodorization.

[9] Another object of the present invention is to provide a functional synthetic fiber si¬ multaneously having whiteness of 93 % or more and tenacity of 3.8 g/d or more.

[10] A further object of the present invention is to provide a method of producing a functional synthetic fiber, for which consecutive production can be realized for 3 days or more.

Technical Solution

[11] The present inventor has conducted extensive studies to accomplish the above objects, resulting in the finding that when a method of producing a functional synthetic fiber in a master batch manner comprises wet-pulverizing the functional material so that a particle size of the functional material does not exceed 1/3 of a desired fiber diameter, drying the pulverized functional material, and re-pulverizing the dried functional material so that the particle size of the dried functional material does not exceed 3/4 of the desired fiber diameter to separate cohered particles of the functional material, dispersibility is improved and re-cohesion is prevented, and thus, it is possible to produce fiber having desired properties, and workability is significantly improved, making consecutive production for 3 days or more possible. Advantageous Effects

[12] As apparent from the above description, a functional synthetic fiber according to the present invention is advantageous in that it is possible to conduct consecutive production for 3 days or more, excellent deodorization and antibacterial properties are assured, and whiteness and tenacity are improved to a level similar to a typical synthetic fiber, thereby avoiding the disadvantages of conventional functional synthetic fiber.

Brief Description of the Drawings

[13] The above and other objects, features and other advantages of the present invention will be more clearly understood from the following detailed description taken in conjunction with the accompanying drawings, in which:

[14] FIGS. 1 to 7 illustrate particle size distributions of functional materials employed in the present invention;

[15] FlG. 8 is an electron microscope picture of functional powder according to preparation example 3;

[16] FlG. 9 is an electron microscope picture of a master batch chip produced using the functional powder according to preparation example 3; and

[17] FlG. 10 is an electron microscope picture of a synthetic fiber produced using the master batch chip of FlG. 9. Best Mode for Carrying Out the Invention

[18] Hereinafter, a detailed description will be given of the present invention.

[19] Since it was found that a functional synthetic fiber produced through a poly¬ merization method had very poor properties, such as whiteness and deodorization, and thus, it was impossible to commercialize the functional synthetic fiber, much effort has been made to produce a functional synthetic fiber using a master batch method. For example, Korean Pat. Laid-Open Publication Nos. 2004-004559 and 2004-0016676 suggest fine pulverization of a functional material for improving workability.

[20] However, no matter how finely the functional material is pulverized, particles con¬ stituting the functional material re-cohere during a drying process, and thus, the above patents cannot provide a desirable solution. Accordingly, heretofore, the synthetic fiber having a predetermined level of properties and functions has not been mass-produced.

[21] The present invention provides a method of producing a functional synthetic fiber, which includes wet-pulverizing a functional material so that a particle size (100 %) of the functional material does not exceed 1/3 of the desired fiber diameter, drying the pulverized functional material, and re-pulverizing the dried and cohered functional material so that a particle size (99 %) of the functional material does not exceed 3/4 of the desired fiber diameter, thereby avoiding poor workability caused by cohesion. The re-pulverized particles do not cohere during long-term storage as well as during production. Preferably, the re-pulverization may be conducted in such a manner that the cohered functional material is preliminarily pulverized using a pin mill and then re- pulverized using a jet mill, or alternatively, the pulverization may be conducted without the preliminary pulverization. Efficiency of re-pulverization may be improved by reducing cohesion strength between the particles using a dispersing agent before the drying process, but it is difficult to desirably prevent cohesion using only the dispersing agent.

[22] When the particle size (100 %) of the wet-pulverized functional material is more than 1/3 of the desired fiber diameter, the fiber has poor tenacity and yarn cutting may occur in the course of producing the fiber. Additionally, when the particle size (99 %) of the re-pulverized functional material is more than 3/4 of the desired fiber diameter even though the particle size of the wet-pulverized material does not exceed 1/3 of the desired fiber diameter, yarn cutting occurs and pack pressure is rapidly increased, and thus, it is impossible to conduct consecutive production.

[23] In this case, the term "fiber diameter" does not mean a diameter of a spun fiber, but a diameter of a drawn final fiber after a spinning process.

[24] The functional material available to the present invention is a natural or an artificial mineral, which is exemplified by a mineral capable of emitting anions or far infrared rays, such as elvan, amphibole, zeolite, calcium phosphate, zirconium phosphate, jade stone, mica, kaolin, talc, and tourmaline, a mineral capable of blocking ultraviolet rays or electromagnetic waves, or a mineral having hygroscopicity and deodorization. Of them, zeolite on which silver (Ag) ions having antibacterial properties are supported is more preferable. Having excellent deodorization and hygroscopicity, the zeolite has ion exchange property, and thus, it is suitable to support the silver ions. The zeolite on which the silver ions are supported may be used while being mixed with other functional materials according to the necessity.

[25] When the silver ions are supported by the functional material, the silver ions are used in an amount of 0.1 - 10 wt%, and preferably 0.3 - 5 wt%. Even though the amount is more than the above range, the antibacterial properties are not improved any more, but the fiber is discolored. It is preferable that the functional material be added to the synthetic fiber in an amount of 0.1 - 3 wt%, when the amount is more than the above range, properties of the synthetic fiber are reduced. Similar efficiency is assured even though nano-silver is mixed with the mineral instead of silver ions.

[26] A master batch chip contains the functional material in an amount of 1 - 20 wt%, and preferably 5 - 15 wt%. It is preferable that a resin chip be pulverized and then mixed with the functional material in the course of producing the master batch chip so as to uniformly disperse the functional material in the master batch chip. Furthermore, the use of a twin screw extruder having two screws may improve dispersibility of the functional material in the course of producing the master batch chip. A filter available to the present invention is an automatically changeable multiple filter, which can increase the yield of the master batch chip and improve productivity. It is preferable that the functional material and resin chip be dried in the course of producing the master batch chip, but the drying process may be omitted when reduction of properties of the master batch chip and fiber is not important.

[27] The master batch chip is spun while being mixed with a chip, and a mixing ratio is controlled so that a content of the functional material in a typical fiber is 0.1 - 3.0 wt%. When the content of the functional material is more than the above range, spinning efficiency is rapidly reduced.

[28] The functional synthetic fiber produced through the above procedure has excellent deodorization and antibacterial properties, and whiteness of 93 % or more after a dyeing process. Furthermore, in the case of a polyester filament and a polyester staple fiber, tenacity is 3.8 g/d and 5.0 g/d, which are similar to properties of typical synthetic fiber.

[29] A better understanding of the present invention may be obtained through the following preparation examples, comparative preparation examples, examples and comparative examples which are set forth to illustrate, but are not to be construed as the limit of the present invention. In the examples, only a polyester fiber typically used as a fiber for clothes is described, but it is to be understood that the present invention may be applied to other synthetic fibers, such as nylon and polypropylene. Also, the examples employ a synthetic fiber for clothes having fineness of 3 deniers or less.

[30]

[31] PREPARATION EXAMPLE 1

[32]

[33] 1000 kg of zeolite having an average particle size of 4 D, on which 3 wt% silver ions were supported, was dispersed in water to produce slurry containing 35 % solids. The slurry was pulverized using a partially stabilized zirconia bead having a size of 1.5 mm in a horizontal bead mill having a capacity of 50 liters. A packing fraction of the bead was 77 vol% of the capacity of the bead mill, and the pulverization was repeated 100 times in a pass manner in which the slurry was completely passed through the bead mill and then discharged. A passing speed of the slurry was ten times the capacity of the bead mill per hour.

[34] The pulverized slurry was subjected to a particle-size analysis to measure a particle size distribution of non-cohered particles, resulting in the finding that a particle size of 50 % was 0.50 D, a particle size of 90 % was 1.82 D, a particle size of 99 % was 3.35 D, and a particle size of 100 % was 4.19 D (FlG. 1).

[35] The pulverized slurry was put in a vessel and then dried in an electric furnace, and dried powder was passed through a pin mill three times to be preliminarily pulverized so as to have a particle size of 10 meshes or less, thereby producing preliminarily pulverized functional powder 1.

[36]

[37] PREPARATION EXAMPLE 2

[38]

[39] 1000 kg of coarse particles which had a particle size of 100 meshes and included

2.5 parts by weight of zeolite on which 3 wt% silver ions were supported, 2 parts by weight of muscovite, 1 part by weight of jade, and 0.5 parts by weight of kaolin mixed with each other were dispersed in water to produce slurry containing 35 % solids. The slurry was pulverized using a partially stabilized zirconia bead having a size of 1.5 mm in a horizontal bead mill having a capacity of 50 liters. A packing fraction of the bead was 77 vol% of the capacity of the bead mill, and the pulverization was repeated 150 times in a pass manner in which the slurry was completely passed through the bead mill and then discharged. A passing speed of the slurry was ten times the capacity of the bead mill per hour.

[40] The pulverized slurry was subjected to a particle-size analysis to measure the particle size distribution of non-cohered particles, resulting in the finding that a particle size of 50 % was 0.63 D, a particle size of 90 % was 1.07 D, a particle size of 99 % was 1.97 D, and a particle size of 100 % was 2.28 D (HG. 2).

[41] The pulverized slurry was put in a vessel and then dried in an electric furnace, and dried powder was passed through a pin mill three times to be preliminarily pulverized so as to have a particle size of 10 meshes or less, thereby producing preliminarily pulverized functional powder 2.

[42]

[43] COMPARATIVE PREPARATION EXAMPLE

[44]

[45] The preliminarily pulverized functional powder 1 produced according to preparation example 1 was re-pulverized using a pilot-scaled jet mill (Jet Pulverizer Co. Inc. in USA: 8" Orbital Micron-Master) in conditions that air pressure was 7.5 atm and a feeding amount was 20 kg/h, thereby producing re-pulverized functional powder. [46] Particle sizes of 50 %, 90 %, 99 %, and 100 % of the re-pulverized functional powder were 0.92 D, 5.96 D, 15.52 D, and 26.2 D, respectively (FlG. 3). [47]

[48] PREPARATION EXAMPLE 3

[49] [50] The procedure of comparative preparation example was repeated except that a feeding amount of functional powder was 15 kg/h. Particle sizes of 50 %, 90 %, 99 %, and 100 % of the re-pulverized functional powder were 0.88 D, 4.76 D, 10.50 D, and

16.57 D, respectively (HG. 4). [51]

[52] PREPARATION EXAMPLE 4

[53] [54] The procedure of comparative preparation example was repeated except that a feeding amount of functional powder was 10 kg/h. Particle sizes of 50 %, 90 %, 99 %, and 100 % of the re-pulverized functional powder were 0.75 D, 3.52 D, 7.55 D, and 10.48

D, respectively (FIG. 5). [55]

[56] PREPARATION EXAMPLE 5

[57] [58] The procedure of comparative preparation example was repeated except that a feeding amount of functional powder was 5 kg/h. Particle sizes of 50 %, 90 %, 99 %, and 100 % of the re-pulverized functional powder were 0.67 D, 3.01 D, 6.20 D, and 7.72 D, respectively (FIG. 6). [59]

[60] PREPARATION EXAMPLE 6

[61] [62] The procedure of preparation example 5 was repeated except that re-pulverization was conducted using the functional powder 2 according to preparation example 2.

Particle sizes of 50 %, 90 %, 99 %, and 100 % of the re-pulverized functional powder were 0.73 D, 2.98 D, 5.54 D, and 6.63 D, respectively (FlG. 7). [63]

[64] EXAMPLES 1 - 4 AND COMPARATIVE EXAMPLE

[65] [66] 50 kg of functional powders produced according to comparative preparation example and preparation examples 3 - 6 were each mixed with 450 kg of polyester chip to produce master batch chips (MB 1 - 5) each containing 10 wt% of functional powder. The polyester chip used to produce the master batch chip had an intrinsic viscosity of 0.65, and was preliminarily pulverized to be smoothly mixed with the powder, so that a content of the powdery chip having a particle size of 1 mm or less was around 10 wt%. A scanning electron microscope picture of the functional powder produced through preparation example 3 as shown in FlG. 8 was compared to that of MB 2 photographed using an electron microscope with a magnification of 2500 as shown in FlG. 9, resulting in the finding that cohered large-sized particles were spon¬ taneously separated in the course of producing the master batch chip and dispersibility of the particles was excellent.

[67] To increase dispersibility of the functional powder, the functional powder was mixed with the partially pulverized polyester chip in a rotary mixer and then fed into a twin screw extruder, thereby creating the master batch chip. At this time, the filter used had a 200 mesh screen size.

[68] Each master batch chip (MB 1 - 5) was mixed with a polyester chip so that the content of the functional material in a fiber was 1.0 wt%, thereby producing a grey yarn of D.T.Y of 100 deniers/48 filaments, and properties of each grey yarn are described in the following Table 1.

[69] [70] Table 1

[71] *Whiteness: whiteness after a white dyeing process [72] [73] From Table 1, it can be seen that workability and tenacity of the fiber are sig¬ nificantly reduced in the case of the comparative example in which a particle size of 99 % of the used functional powder is more than 3/4 of a fiber diameter (average diameter is 14.5 D), but workability and tenacity of the fiber are improved to a level similar to a typical synthetic fiber having no functional powder in the case of using the functional powder having the particle size smaller than the particle size of 99 %.

[74] A section of the fiber according to example 1 is shown in FlG. 10, in which a particle size of 99 % is 3/4 of a fiber diameter. When the fiber is compared to those of FIGS. 8 and 9, it can be seen that the fiber does not contain cohered coarse particles and that the dispersibility of the functional powder in the fiber is excellent. Because of excellent dispersibility, properties of the fiber are kept at a desired level and it is possible to conduct consecutive production.

[75] In other words, when the particle size of 99 % of the re-pulverized powder does not exceed 3/4 of the fiber diameter, coherence of the functional powder does not occur any more during the production of the master batch chip and while spinning the fiber, and the cohered particles are spontaneously separated into individual particles, which do not negatively affect properties or workability of the fiber.

[76]

[77] EXAMPLE 5

[78]

[79] Preliminarily pulverized functional powder produced according to the same procedure as preparation example 2 was re-pulverized using a jet mill for mass- production (Jet pulverizer Co. Inc. in USA: 24" orbital Micron-Master). Particle sizes of 50 %, 90 %, 99 %, and 100 % of the re-pulverized functional powder were 0.71 D, 2.85 D, 5.47 D, and 6.63 D. 50 tons of master batch chip were produced using the above powder according to the same procedure as the above examples, and the master batch chip was mixed with a polyester chip and fed into a commonly used spinning device to produce a polyester staple fiber of 1.4 deniers/38 mm containing 1.0 wt% of functional material. The staple fiber had a tenacity of 5.9 g/d and whiteness of 95 %, and consecutive production time was 10 days, which approximates the 15 days consecutive production time of polyester fiber.

[80]

[81] EXAMPLE 6

[82]

[83] Deodorization of the functional fiber produced according to example 5 was tested, with the result that deodorizations of formaldehyde, ammonia, and toluene were 68 %, 59 %, and 47 % based on 1 hour, respectively, which correspond to 2 ? 3 times the level of typical polyester fiber.

[84]

[85] EXAMPLE 7

[86]

[87] The functional fiber (1.4 denier and 38 mm) produced according to example 5 was spun in a single manner to have 40 embroideries, and a spun grey yarn was woven so as to have a warp density of 118 plies and a weft density of 88 plies per 1 inch. After a woven cloth was cut in a size of 3 X 3 cm, mite avoidance of a cut sample was tested. In the case of an "invasion prevention method" in which it was observed whether a mite moved from a medium to an enticing material contained in the test sample or not, the mite avoidance was 95.1 %, and in the case of a "diffusion prevention method" in which selective invasion of the mite into enticing material mixed with the test sample was observed, the mite avoidance was 95.7 %. Additionally, in the case of a "test-tube method" in which transmittance of a mite through the test sample to the enticing material was observed, the mite avoidance was 99.9 %.

[88]

[89] EXAMPLE 8

[90]

[91] Antibacterial properties of a sample produced through example 6 were tested using staphylococcus aureus ATCC 6538 and Klebsiella pneumoniae ATCC 4352 as test bacteria (test method: KS K 0693-2001). When cotton was used as a control after 18 hours since bacteria was inoculated into a medium, the bacteria were propagated by 47 times. However, when the fiber produced according to example 5 was added into a medium, the number of the bacteria was reduced by 99.9 % or more.

[92]

[93] EXAMPLE 9

[94]

[95] The cloth produced according to example 7 was cut so as to have a warp side of 30 cm and a weft side of 3 cm to produce a sample. When an edge of the sample was dipped in water and left for 10 min, the sample absorbed water to a position of 25 mm from the edge thereof due to a capillary action. However, in the case of a typical polyester cloth woven according to the same procedure as example 7, an absorption height of water for 10 min was merely 1 mm (test method: KS K 0815-2001.6.27. 1 B METHOD).

[96] Accordingly, it can be seen that the fiber of the present invention has excellent hy- groscopicity. The reason for this is considered that zeolite, which is added to the fiber and acts as a functional material, has excellent hygroscopicity, and particles of the functional material uniformly dispersed form a plurality of fine holes in the fiber in the course of drawing the fiber after a spinning process.

Claims

[1] A method of producing a functional synthetic fiber, in which a master batch chip containing a high concentration of functional material is prepared, mixed with a chip, and spun so that a content of the functional material is 0.1 - 3.0 wt% in a typical master batch manner, comprising: wet-pulverizing the functional material so that a particle size of 100 % of the functional material does not exceed 1/3 of a desired fiber diameter; drying the wet-pulverized functional material; and re-pulverizing the dried functional material so that a particle size of 99 % of the dried functional material does not exceed 3/4 of the desired fiber diameter to produce the master batch chip.

[2] The method as set forth in claim 1, wherein the functional material is zeolite.

[3] The method as set forth in claim 1, wherein silver ions are supported in an amount of 0.1 - 10 wt% on the functional material.

[4] The method as set forth in claim 1, wherein the master batch chip is prepared by mixing a pulverized resin chip with a powdery functional material.

[5] The method as set forth in claim 1, wherein a spinning process is conducted con¬ tinuously for 3 days or more.

[6] The method as set forth in claim 1, wherein a spinning process is conducted con¬ tinuously for 5 days or more.

[7] A functional synthetic fiber produced through the method according to any one of claims 1 to 6.

[8] The functional synthetic fiber as set forth in claim 7, wherein the functional synthetic fiber has deodorization, antibacterial properties, and tenacity of 3.8 g/d or more.

[9] The functional synthetic fiber as set forth in claim 7 or 8, wherein the functional synthetic fiber has tenacity of 5.0 g/d or more.

[10] The functional synthetic fiber as set forth in any one of claims 7 to 9, wherein the functional synthetic fiber has whiteness of 93 % or more.