WO2016052998A1 - 라이오셀 크림프 섬유 - Google Patents
라이오셀 크림프 섬유 Download PDFInfo
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- WO2016052998A1 WO2016052998A1 PCT/KR2015/010319 KR2015010319W WO2016052998A1 WO 2016052998 A1 WO2016052998 A1 WO 2016052998A1 KR 2015010319 W KR2015010319 W KR 2015010319W WO 2016052998 A1 WO2016052998 A1 WO 2016052998A1
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- lyocell
- crimp
- fiber
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- fibers
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Classifications
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
- D01F2/08—Composition of the spinning solution or the bath
- D01F2/10—Addition to the spinning solution or spinning bath of substances which exert their effect equally well in either
Definitions
- the present invention relates to lyocell fibers, and more particularly to lyocell crimp fibers.
- Fibers when viewed in shape, are linear objects that are flexible, thin, and have a very high degree of fineness, that is, a ratio of length to thickness. These fibers can be classified into long fibers, brisket fibers and short fibers in terms of form, and natural fibers and artificial fibers in terms of raw materials.
- fiber has been closely related to human life. Early fiber was mainly used as a raw material for coating in the form of natural fiber such as cotton, hemp, wool and silk fiber.
- natural fiber such as cotton, hemp, wool and silk fiber.
- textiles have been expanded not only for coating materials but also for industrial purposes, and the field of artificial fibers has been newly opened to meet the rapidly increasing demands as the culture and population increase.
- viscose rayon has been widely used in the past as a fiber having excellent gloss and color development comparable to silk.
- viscose rayon has a rather complicated manufacturing process, and as many chemicals are used to melt wood pulp, controversy over environmental issues and wastewater treatment has been ongoing. Accordingly, regenerated fibers such as rayon-based regenerated fibers and cellulose acetate, which will replace existing viscose rayon fibers such as cupra rayon and lyocell, have emerged.
- lyocell fibers made from natural pulp and amine oxide hydrates exhibit superior tensile properties and feel compared to conventional regenerated fibers, and amine oxide solvents used in the production of lyocell fibers are recyclable and biodegradable at disposal. As it does not generate any contaminants in the production process, research on lyocell fibers as an environmentally friendly recycled fiber is becoming more active.
- lyocell fibers for example, as described in U.S. Patent Nos. 4,416,698 and 4,246,221 by spinning a spinning dope dissolved in amine oxide (NMMO), and solidified it to prepare a filament In other words, it is processed after washing and drying.
- NMMO amine oxide
- the lyocell fibers are not naturally crimped, so that they can be usefully compressed by using wet steam according to the method described in EP 797,696, or using dry steam according to the method described in EP 703,997. Crimp can be provided by the stuffer box crimping process.
- the present invention is intended to provide a lyocell crimp fiber having excellent crimp number and crimp stability and improved bulging properties.
- cream lyocell multifilament prepared by spinning lyocell spinning dope comprising cellulose pulp and N-methylmorpholine-N-oxide (NMMO) aqueous solution It is prepared by ping, and is a lyocell crimp fiber, characterized in that the swelling index is defined by the following formula 1 800 to 2,000.
- NMMO N-methylmorpholine-N-oxide
- Inflation Index Inflation Factor (BF) ⁇ Number of Crimps per Inch (CN)
- Equation 2 the inflation factor in Equation 1 is defined by Equation 2 below.
- Inflation factor ⁇ (width change of fiber before and after permanent deformation) ⁇ (change in length of fiber before and after permanent deformation) ⁇ ⁇ 100
- the lyocell spinning dope is 6 to 16% by weight of cellulose pulp based on the total weight of the spinning dope; And it may be to include 84 to 94% by weight N-methylmorpholine-N-oxide aqueous solution.
- the cellulose pulp may have an alpha-cellulose content of 85 to 97% by weight based on the total weight of pulp, and a degree of polymerization (DPw) of 600 to 1700.
- DPw degree of polymerization
- the lyocell crimp fiber according to the embodiment, the number of crimps per inch (CN) is 25 to 39 / inch, the swelling factor (BF) defined by the formula 2 may be 30 to 50.
- the lyocell multifilament may be made of a lyocell monofilament having a tensile strength of 2.0 to 3.5 g / d.
- the lyocell monofilament may have a fineness of 1.0 to 8.0 denier and an elongation of 5 to 13%.
- the lyocell crimp fiber according to the present invention is excellent in the effect of improving the bulkiness, and excellent in the shape stability of the crimp. As a result, when applied as a garment and industrial materials, even a small amount of fibers can be expected to be equal to or higher than the conventional physical properties.
- cream lyocell multifilament prepared by spinning a lyocell spinning dope comprising cellulose pulp and N-methylmorpholine-N-oxide (NMMO) aqueous solution It is prepared by ping, and can provide a lyocell crimp fiber, characterized in that the swelling index is defined by the following formula 1 800 to 2,000.
- NMMO N-methylmorpholine-N-oxide
- Inflation Index Inflation Factor (BF) ⁇ Number of Crimps per Inch (CN)
- Equation 2 the inflation factor in Equation 1 is defined by Equation 2 below.
- Inflation factor ⁇ (width change of fiber before and after permanent deformation) ⁇ (change in length of fiber before and after permanent deformation) ⁇ ⁇ 100
- Crimping which is a general term for crimping filaments, is also called crimping, and it is used to artificially fabricate fabrics made by spinning in a fibrous form to give texture like natural fibers.
- the processing method to form is called. Since the crimped fiber has a space where air can exist between the fiber bundles, it can form a large volume even at the same weight, thereby ensuring a soft texture and warmth. In addition, breathability may be secured, and antimicrobial effects may be exerted by ensuring breathability. Moreover, if the material of the fiber itself is a biodegradable environment-friendly material such as the lyocell of the present invention, the effect can be doubled.
- crimped lyocell fibers can be used as textile materials for winter clothing, quilts, medical fibers, hygiene products, including outdoor wear, innerwear, hats, sports socks, underwear, etc.
- the material may be usefully used for tire cords, various filters, mechanical rubber good (MRG) such as hose reinforcement, cement reinforcement, and automobile interior reinforcement.
- MRG mechanical rubber good
- the bulging index defined as in Equation 1 in the present invention is a value determined by the swelling factor, which is the width change rate compared to the length change rate before and after the permanent deformation and the number of crimps per inch formed in the lyocell fiber, as shown in the formula. Larger means more bloat factor or number of crimps per inch. Accordingly, the swelling index can easily determine the degree of swelling of the lyocell fibers. If the swelling index is less than 800, it is difficult to satisfy both the number of crimps and the swelling factor to a sufficient level, and the inflation index exceeds 2000. It may be desirable for the inflation index to meet the range as there may be a limit.
- the bulging factor defined by the percentage value of the width change rate to the fiber length change before and after permanent deformation as shown in Equation 2 satisfies 30 to 50. It is preferable that the number of crimps (CN) measured per inch is satisfied to 25 to 39 / inch.
- "permanent deformation" as defined in the present invention means a point in which the crimp is not restored to its original form when the crimp-formed fiber is pulled and released, and in the present invention, 4 kg of lyocell crimp fiber is tested.
- the present invention can use the tension at the 4kg.f load as the basis of the permanent strain.
- the crimp is well formed, the number of crimps per inch is sufficient, so that the fiber is well inflated by the crimp before the permanent deformation occurs, but after the permanent deformation has occurred, the degree of swelling is significantly reduced, so that the rate of change of width is considerably large. Is observed.
- the crimp is not formed properly, there is little difference in the degree of swelling by the crimp before and after permanent deformation.
- the swelling factor is larger as described above, it can be interpreted that the swelling property is excellent by sufficient crimping, and as a result, a satisfactory level of swelling index value can be obtained.
- the swelling factor may be 30 or more, considering the minimum number of crimps to be secured (25 / inch), and the number of crimps may not be increased indefinitely. Inflation factor can also be difficult to exceed 50 because there is no.
- lyocell crimp fiber of the present invention having the above-described swelling characteristics can be prepared through the same steps (S1) to (S5).
- (S1) is a step of spinning a lyocell spinning dope comprising cellulose pulp and an aqueous N-methylmorpholine-N-oxide (NMMO) solution.
- the lyocell spinning dope is 6 to 16% by weight of cellulose pulse;
- N-methylmorpholine-N-oxide aqueous solution of 84 to 94% by weight, the cellulose pulp may have an alpha-cellulose content of 85 to 97% by weight, and a degree of polymerization (DPw) of 600 to 1700. have.
- the content of the cellulose pulp is less than 6% by weight, it is difficult to realize the fibrous form and characteristics, and if more than 16% by weight, it is difficult to dissolve in the aqueous phase and the tensile strength may be unnecessarily high.
- the content of the N- methyl morpholine-N-oxide aqueous solution is less than 84% by weight is not preferable because the melt viscosity is significantly high, if more than 94% by weight spinning yarn is significantly lowered to produce a uniform fiber in the spinning step It can be difficult.
- the step of ejecting from the spinneret using the spinning dope may be performed under a spinning temperature of 80 to 130 °C.
- the spinneret serves to discharge the spinning dope on the filament into the coagulating liquid in the coagulation bath through the air gap section.
- the spinning temperature is out of the spinning temperature, the flow rate of the spinning dope is poor or the viscosity of the spinning dope is lowered to control the discharge amount. It can be difficult.
- Step (S2) is a step of solidifying the lyocell spinning dope spun in the step (S1) to obtain a lyocell multifilament
- the solidification of the (S2) step is air quenching to supply cooling air to the spinning dope to solidify Primary coagulation step by Air Quenching (Q / A);
- step (S1) After discharging the spinning dope through the spinneret in step (S1), it can be passed through the air gap section, which is a space between the spinneret and the coagulation bath.
- the air gap section cooling air is supplied from the air cooling unit located inside the donut-shaped mold to the outside of the mold, and the first solidification may be performed by air quenching to supply the cooling air to the spinning dope.
- the factors affecting the properties of the lyocell multifilament obtained in the step (S2) is the temperature and wind speed of the cooling air in the air gap section
- the solidification of the (S2) step is a temperature of 4 to 15 °C and 5 to
- the cooling air having a wind speed of 50 m / s may be supplied to the spinning dope to solidify. If the temperature of the cooling air is less than 4 ° C. during the first solidification, the surface of the detention quickly cools down, and the lyocell multifilament is also unevenly solidified, resulting in poor spinning processability. Inadequately done, this can also adversely affect radiation fairness.
- the wind speed of the cooling air is less than 5 m / s during the first solidification, the primary solidification by the cooling air is not sufficiently performed, resulting in poor radiation fairness, and a trimming occurs. May be impaired by air, resulting in poor spinning fairness.
- the spinning dope may be supplied to a coagulation bath containing a coagulation liquid and secondary coagulation may proceed.
- the temperature of the coagulating liquid is preferably 30 ° C. or less for proper progress of secondary coagulation, but the coagulation temperature is not too high so that the coagulation rate can be controlled appropriately.
- the coagulating solution is not particularly limited because it can be prepared and used in a conventional composition in the art.
- Step (S3) is a step of washing the lyocell multifilament obtained in the step (S2). Specifically, after introducing the lyocell multifilament obtained in the step (S2) to the traction roller, it can be washed by introducing into the washing bath.
- a washing liquid of 0 to 100 °C temperature can be used, water can be used as the washing liquid, and other additive components as necessary You can also include more.
- Step (S4) is an step of tanning the lyocell multifilament washed in the step (S3), it is preferable to perform the drying after the tanning.
- the tanning can be carried out in such a way that the multifilament is completely submerged and buried in the tanning and the amount of tanning applied to the filament by the weaving rollers attached to the entry and exit rolls of the tanning unit.
- the emulsion reduces the friction that occurs when the filament is in contact with the drying roller and the guide, the crimp step, so that the crimp can be formed well.
- the lyocell monofilament constituting the lyocell multifilament prepared through the steps (S1) to (S4) is preferably the strength of 2.0g / d to 3.5g / d.
- the monofilament means a filament that is discharged through various holes of the spinneret and separated from the fiberized multifilament through solidification, washing, and emulsion treatment, and the strength of the monofilament is separated from the fiberized multifilament. It may refer to the strength of a filament of one ol.
- the physical properties such as touch, volume, heat retention, and water absorption are most often improved. Therefore, the minimum strength is secured, but the strength does not have to be excellent. In other words, if the strength of the lyocell monofilament is less than 2.0 g / d, the spinning processability may be lowered. If the lyocell monofilament is more than 3.5 g / d, an excessively high load may be applied to the swelling through the open island after the crimp formation. not.
- the lyocell monofilament preferably has a fineness of 1.0 to 8.0de in consideration of swelling property. If the fineness of the monofilament is lower than 1.0 de (denier), the twisting between adjacent monofilaments may occur during the opening after crimping, and the opening rate may decrease. If the fineness of the monofilament is higher than 8.0de, the crimp number increases. Since more steam and pressure have to be applied, it is not desirable for energy efficiency and the weight of the final product can be increased relatively even at the same swelling.
- the lyocell monofilament may have an elongation of 5 to 13%, and when the elongation is less than 5%, the fiber may be easily cut at the time of opening after crimp formation, thereby lowering the yield. Not only is it difficult to control to exceed 13%, but given the application of crimping fibers, it is not necessary to meet further superior elongation.
- step (S5) is a step of crimping the lyocell multifilament emulsion treated in the step (S4).
- the swelling property may be determined in step S5, and the crimp may be formed by supplying steam and applying pressure to the lyocell multifilament.
- the crimping means is a stuffer box, and the stuffer box may be a means including a steam box and a press roller.
- the crimping method it is preferable to raise the temperature of the filament by first passing the lyocell multifilament through a steam box and imparting steam at 0.1 to 1.0 kgf / cm 2. At this time, if the supply amount of steam of the steam box is less than 0.1 kgf / cm2, the crimp is not formed smoothly in the press roller or even if the crimp is formed, the heat setting is not achieved, the shape can not be maintained, if it exceeds 1.0 kgf / cm2 in the stopper box The temperature rises above 120 ° C and the filaments stick together, preventing them from passing through the stopper box.
- the lyocell multifilament may be supplied to a press roller and pressed at a pressure of 1.5 to 2.0 kgf / cm 2 to form a crimp.
- the pressure for pressing the press roller is less than 1.5 kgf / cm2
- the desired number of crimps are not formed
- the pressure exceeds 2.0kgf / cm2 the pressing force is too strong, this too filament may not pass through the stopper box.
- the number of crimps formed while passing through the stopper box is very important, and the number of crimps is preferably 25 to 39 / inch per inch. If the number of crimps is less than 25 / inch, the opening factor is not easy, so the inflation factor defined by Equation 1 is less than 30, and the swelling characteristic in the width direction may be poor, and the crimp number may be increased even if the pressure of the press roller is increased. Forming more than 39 / inch can be limiting.
- a cellulose pulp having a degree of polymerization (DPw) 820 and an alpha cellulose content of 93.9% was mixed with an NMMO / H20 mixed solvent (weight ratio 90/10) having a propylate content of 0.01% by weight to prepare a spinning dope for producing lyocell fibers having a concentration of 12% by weight. It was.
- the spinning dope was maintained at a spinning temperature of 110 ° C. in the spinning nozzle of the spinneret, and was controlled by spinning the discharge amount and spinning speed of the spinning dope so that the single fineness of the filament was 3.37 denier.
- Spinning dope on the filament discharged from the spinning nozzle was supplied to the coagulating liquid in the coagulation bath through the air gap section.
- the cooling air in the air gap section first solidifies the spinning dope at 8 °C temperature and 10m / s wind speed.
- the coagulating solution was used at a temperature of 25 °C, concentration of 85% by weight of water and 15% by weight of NMMO. At this time, the coagulant concentration was continuously monitored using a sensor and a refractometer.
- the filament stretched in the air layer through the towing roller is washed by the washing liquid sprayed from the washing machine to remove the remaining NMMO, and evenly squeezes the oil into the filament, and then squeezes it again so that the oil content of the filament is 0.2 % Was maintained and dried to 150 °C in a drying roller to prepare a lyocell filament.
- the prepared lyocell crimp fiber was cut to a length of 200 mm in a tension free state, and then fixed to the first point (0 mm position) and the middle point (100 mm position). Then, the tensile force was applied at the 200mm point to extend the length 50% (50mm), and the end point was fixed at the extended position. Then, the tension of the 100 mm point was released to disperse the tension, and a micrograph was taken to obtain the number of crimps (Crimp Number, CN) formed per 10 mm, and converted into CPI (counts per inch). Was measured as 7 (ea / inch).
- the lyocell crimp fiber is manufactured by applying the same method as in Preparation Example 1, but the number of crimps is 15 (ea / inch), 20 (ea / inch), and 25 (ea /) by changing the pressure of the press roller. inches), 30 (ea / inch) and 39 (ea / inch), Preparation Examples 2 to 6 were prepared. However, even if the press roller pressure was changed, the number of crimps did not increase any more, and the production example produced only up to 39 ea / inch.
- Preparation Example 4 except that steam (120 ° C.) having a pressure of 1.0 kgf / cm 2 was applied to the steam box in order to heat setting the lyocell fibers in the stuffer box before passing them through the press roller.
- Lyocell crimp fibers (Examples 1 to 3) having crimp counts of 25 (ea / inch), 30 (ea / inch), and 39 (ea / inch) were prepared by applying the same method as in the above.
- Crimp number is 7 (ea / inch), 15 (ea / inch) and by applying the same method as Preparation Examples 1 to 3, respectively, except that steaming is performed in the stuffer box as in Examples 1 to 3. 20 (ea / inch) lyocell crimp fiber Comparative Examples 1 to 3 were prepared.
- Inflation factor ⁇ (change in fiber width before and after permanent deformation) ⁇ (change in length of fiber before and after permanent deformation) ⁇ ⁇ 100
- the inflation index was calculated by multiplying the crimp number of each of Examples 1 and 2 and Comparative Examples 1 and 2 and the measured inflation factor as shown in Equation 2 below, and the values thereof were reflected in Table 1 below.
- the inflation factor does not increase to 30 if the heat setting is not performed, and if the number of crimps does not reach 25 even if the heat setting is performed, both the inflation factor and the inflation index are high. It appeared to be difficult to secure.
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- Chemical Kinetics & Catalysis (AREA)
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- Textile Engineering (AREA)
- Artificial Filaments (AREA)
- Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
Abstract
Description
Sample | 열고정 처리 유무 | Cr. No.(CN) | ΔL1) | ΔW2) | BloomingFactor | 부풀림지수(BFxCN) |
제조예 1 | X | 7 | 80 | 4 | 5.0 | 35.0 |
제조예 2 | X | 15 | 77 | 5 | 6.5 | 97.5 |
제조예3 | X | 20 | 76 | 7 | 9.2 | 184.0 |
제조예 4 | X | 25 | 70 | 10 | 14.3 | 357.5 |
제조예 5 | X | 30 | 68 | 10 | 14.7 | 441.0 |
제조예 6 | X | 39 | 65 | 10 | 15.4 | 600.6 |
비교예 1 | O | 7 | 78 | 4 | 5.1 | 35.7 |
비교예 2 | O | 15 | 73 | 5 | 6.8 | 102.0 |
비교예 3 | O | 20 | 65 | 7 | 10.7 | 214.0 |
실시예 1 | O | 25 | 62 | 22 | 35.4 | 885.0 |
실시예 2 | O | 30 | 60 | 24 | 40.0 | 1,200.0 |
실시예 3 | O | 39 | 58 | 27 | 46.5 | 1,813.5 |
Claims (7)
- 셀룰로오스 펄프 및 N-메틸모폴린-N-옥사이드(N-methylmorpholine-N-oxide; NMMO) 수용액을 포함하는 라이오셀 방사 도프를 방사하여 제조된 라이오셀 멀티 필라멘트를 크림핑하여 제조되며,하기 식 1로 정의되는 부풀림 지수가 800 내지 2,000인 것을 특징으로 하는 라이오셀 크림프 섬유;(식 1) 부풀림 지수 = 부풀림 인수(BF) × 인치당 크림프 개수(CN)이때, 상기 식 1에서 부풀림 인수는 하기 식 2로 정의되는 것이다.(식 2) 부풀림 인수={(영구변형 전·후 섬유의 폭변화)÷(영구변형 전·후 섬유의 길이변화)}×100
- 제 1 항에 있어서, 상기 라이오셀 방사 도프는 방사도프 총 중량 기준 셀룰로오스 펄프 6 ~ 16 중량%; 및 N-메틸모폴린-N-옥사이드 수용액 84 ~ 94 중량%를 포함하는 것임을 특징으로 하는 라이오셀 크림프 섬유.
- 제 2 항에 있어서, 상기 셀룰로오스 펄프는 펄프 총 중량 기준 알파-셀룰로오스 함량이 85 ~ 97중량%이고, 중합도(DPw)가 600 ~ 1700인 것임을 특징으로 하는 라이오셀 크림프 섬유.
- 제 1 항에 있어서, 상기 라이오셀 크림프 섬유는 인치당 크림프 수가 25 내지 39개/inch이고, 상기 식 2로 정의되는 부풀림 인수가 30 내지 50인 것을 특징으로 하는 라이오셀 크림프 섬유.
- 제 1 항에 있어서, 상기 라이오셀 멀티 필라멘트는 인장강도가 2.0 내지 3.5 g/d인 라이오셀 모노필라멘트로 이루어진 것임을 특징으로 하는 라이오셀 크림프 섬유.
- 제 5 항에 있어서, 상기 라이오셀 모노필라멘트는 섬도가 1.0 내지 8.0 데니어인 것을 특징으로 하는 라이오셀 크림프 섬유.
- 제 5 항에 있어서, 상기 라이오셀 모노필라멘트는 신도가 5 내지 13%인 것을 특징으로 하는 라이오셀 크림프 섬유.
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JP2017513701A JP2017528616A (ja) | 2014-09-30 | 2015-09-30 | リヨセルクリンプ繊維 |
CN201580050416.7A CN107075739B (zh) | 2014-09-30 | 2015-09-30 | 莱赛尔卷曲纤维 |
US15/512,969 US20170292207A1 (en) | 2014-09-30 | 2015-09-30 | Lyocell crimped fiber |
EP15847023.7A EP3202959A4 (en) | 2014-09-30 | 2015-09-30 | Lyocell crimped fiber |
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KR1020150136000A KR102157887B1 (ko) | 2014-09-30 | 2015-09-25 | 라이오셀 크림프 섬유 |
KR10-2015-0136000 | 2015-09-25 |
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US20100281662A1 (en) * | 2007-07-11 | 2010-11-11 | Lenzing Aktiengesellschaft | Filling Fiber With Improved Opening Performance, Method For Its Production And Its Use |
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- 2015-09-30 WO PCT/KR2015/010319 patent/WO2016052998A1/ko active Application Filing
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