KR101877730B1 - Melt-blown fiber web improved electrical conductivity and manufacturing method thereof - Google Patents
Melt-blown fiber web improved electrical conductivity and manufacturing method thereof Download PDFInfo
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- 239000000835 fiber Substances 0.000 title claims abstract description 38
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 11
- 238000007747 plating Methods 0.000 claims abstract description 29
- 239000008188 pellet Substances 0.000 claims abstract description 18
- 230000003213 activating effect Effects 0.000 claims abstract description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 38
- 229910052759 nickel Inorganic materials 0.000 claims description 19
- 230000004913 activation Effects 0.000 claims description 14
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 12
- 239000004743 Polypropylene Substances 0.000 claims description 11
- 229920001155 polypropylene Polymers 0.000 claims description 11
- 238000009987 spinning Methods 0.000 claims description 10
- -1 polypropylene Polymers 0.000 claims description 9
- 229920005989 resin Polymers 0.000 claims description 7
- 239000011347 resin Substances 0.000 claims description 7
- 229910001510 metal chloride Inorganic materials 0.000 claims description 5
- 241000080590 Niso Species 0.000 claims description 4
- HGGYAQHDNDUIIQ-UHFFFAOYSA-L dichloronickel;hydrate Chemical compound O.Cl[Ni]Cl HGGYAQHDNDUIIQ-UHFFFAOYSA-L 0.000 claims description 4
- LKNLEKUNTUVOML-UHFFFAOYSA-L nickel(2+);sulfate;hydrate Chemical compound O.[Ni+2].[O-]S([O-])(=O)=O LKNLEKUNTUVOML-UHFFFAOYSA-L 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims 3
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical group C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims 1
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- BBMHARZCALWXSL-UHFFFAOYSA-M sodium dihydrogenphosphate monohydrate Chemical compound O.[Na+].OP(O)([O-])=O BBMHARZCALWXSL-UHFFFAOYSA-M 0.000 claims 1
- 239000001119 stannous chloride Substances 0.000 claims 1
- 235000011150 stannous chloride Nutrition 0.000 claims 1
- PKIDNTKRVKSLDB-UHFFFAOYSA-K trisodium;2-hydroxypropane-1,2,3-tricarboxylate;hydrate Chemical compound O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O PKIDNTKRVKSLDB-UHFFFAOYSA-K 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 15
- 239000000463 material Substances 0.000 abstract description 8
- 239000011358 absorbing material Substances 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 3
- 239000011810 insulating material Substances 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 14
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 10
- 208000012886 Vertigo Diseases 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 238000001125 extrusion Methods 0.000 description 4
- 239000000155 melt Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 3
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000007772 electroless plating Methods 0.000 description 2
- 238000005338 heat storage Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910001453 nickel ion Inorganic materials 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 229910052763 palladium Inorganic materials 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 238000005453 pelletization Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229920005594 polymer fiber Polymers 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 239000011232 storage material Substances 0.000 description 2
- 101150003085 Pdcl gene Proteins 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000003373 anti-fouling effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000009931 harmful effect Effects 0.000 description 1
- 238000002074 melt spinning Methods 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- 239000002952 polymeric resin Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 229910001432 tin ion Inorganic materials 0.000 description 1
Images
Classifications
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/44—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling
- D04H1/46—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling by needling or like operations to cause entanglement of fibres
- D04H1/492—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling by needling or like operations to cause entanglement of fibres by fluid jet
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4282—Addition polymers
- D04H1/4291—Olefin series
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/49—Oxides or hydroxides of elements of Groups 8, 9,10 or 18 of the Periodic Table; Ferrates; Cobaltates; Nickelates; Ruthenates; Osmates; Rhodates; Iridates; Palladates; Platinates
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
- H05K9/009—Electromagnetic shielding materials, e.g. EMI, RFI shielding comprising electro-conductive fibres, e.g. metal fibres, carbon fibres, metallised textile fibres, electro-conductive mesh, woven, non-woven mat, fleece, cross-linked
-
- D—TEXTILES; PAPER
- D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
- D10B2401/00—Physical properties
- D10B2401/16—Physical properties antistatic; conductive
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Mechanical Engineering (AREA)
- Nonwoven Fabrics (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
Description
본 발명은 멜트블로운 섬유웹에 관한 것으로서, 더욱 상세하게는 멜트블로운 섬유웹의 전기전도성을 향상시키는 기술에 관한 것이다.The present invention relates to a meltblown fiber web, and more particularly to a technique for improving the electrical conductivity of a meltblown fiber web.
고분자를 이용한 섬유웹은 산업용 섬유소재로 널리 사용되고 있다. 현재에는 이들 섬유에 방오성, 항균성, 흡음성, 자외선 차단성, 전자파 차폐성등 여러 특수 기능을 부여한 고부가 기능성 섬유에 대한 연구개발이 활발하게 수행되고 있다. 하지만 고분자 기반 섬유는 전기부도체이기 때문에 발생한 정전기를 방전하지 못할 뿐만 아니라 전자파를 투과시키는 단점이 있어, 정전기 및 전자파 방지를 위한 소재로 활용이 어려운 실정이다.Fiber webs using polymers are widely used as industrial textile materials. At present, research and development on high value-added functional fibers imparting various special functions such as antifouling property, antibacterial property, sound absorption property, ultraviolet light shielding property and electromagnetic wave shielding property to these fibers are actively carried out. However, since polymer-based fibers are electrically insulated, they can not discharge generated static electricity and transmit electromagnetic waves. Therefore, it is difficult to use them as a material for preventing static electricity and electromagnetic waves.
최근 전자·통신기기의 사용의 급격한 증가로 전자파의 폐해에 관한 우려와 관심이 높아지고, 전자파가 인체에 부정적인 영향을 미치는 연구결과가 발표되면서 전자파 차폐 기술개발에 관심이 높아지고 있다. 차폐소재로서 섬유는 고분자 수지를 사용하여 저가로 양산화가 가능하며, 정량화를 동시에 충족시킬 수 있다. 하지만 고분자 섬유의 전기전도성이 현저히 떨어져 이를 보완하는 기술개발이 시급한 실정이다.Recently, as the use of electronic and communication devices has been rapidly increasing, there has been a growing concern and concern about the harmful effects of electromagnetic waves, and as a result of research on electromagnetic waves having a negative effect on the human body, interest in the development of electromagnetic wave shielding technology is increasing. As a shielding material, fibers can be mass-produced at a low cost by using a polymer resin, and can be quantified at the same time. However, it is urgent to develop a technology that compensates for the electrical conductivity of the polymer fibers.
본 발명의 목적은 전기전도성이 향상된 멜트블로운 섬유웹을 제공함에 있다.It is an object of the present invention to provide a meltblown fibrous web having improved electrical conductivity.
또한 본 발명의 다른 목적은 전기전도도가 향상 된 멜트블로운 섬유웹을 제공함으로써, 상기 섬유웹을 여과재, 흡수재, 흡음재, 절연재, 축열재 및 전자파 차폐제로 활용하는 방안을 제공함에 있다.Another object of the present invention is to provide a method for utilizing the fiber web as a filter medium, an absorbing material, a sound absorbing material, an insulating material, a heat storage material and an electromagnetic wave shielding material by providing a meltblown fiber web having improved electrical conductivity.
상기 목적을 달성하기 위하여, 본 발명은 전기전도성이 향상된 멜트블로운 섬유웹의 제조방법을 제공한다. 상기 멜트블로운 섬유웹의 제조방법은 폴리프로필렌(Polypropylene, PP) 수지를 용융압출하여 펠릿을 제조하는 펠릿제조단계, 펠릿을 열풍기류에 분사하여 섬유웹을 제조하는 방사단계, 금속염화물로 섬유웹 표면을 활성화 시키는 활성화 단계 및 표면이 활성화된 섬유웹을 니켈 도금하는 도금단계를 포함하는 것을 일 측면으로 한다.In order to achieve the above object, the present invention provides a method for producing a meltblown fibrous web having improved electrical conductivity. The method for producing the meltblown fibrous web includes a pellet manufacturing step for producing pellets by melt extruding a polypropylene (PP) resin, a spinning step for producing a fiber web by spraying the pellets into a hot air stream, An activation step of activating the surface, and a plating step of nickel plating the surface-activated fibrous web.
바람직하게는, 펠릿제조단계는 폴리프로필렌 수지를 온도 130 내지 200℃에서 용융압출한다. 또한 열풍기류는 공기 공급속도 80 내지 400m/s. 공기 공급온도 200 내지 350℃인 고속 열풍기류이다.Preferably, the pelletizing step melt-extrudes the polypropylene resin at a temperature of 130 to 200 캜. Also, the hot air current is supplied at an air supply speed of 80 to 400 m / s. And an air supply temperature of 200 to 350 ° C.
바람직하게는, 방사단계의 분사된 펠릿은 회전속도 60 내지 150mm/s인 수집체로 수집한다.Preferably, the injected pellets of the spinning stage are collected with an aggregate having a rotational speed of 60 to 150 mm / s.
바람직하게는, 금속염화물은 염화주석(SnCl2) 및 염화팔라듐(PdCl2) 중에서 선택되는 1이상이다. 또한 도금단계는 황산니켈 수화물(NiSO4·6H2O) 200 내지 350g/L, 염화니켈 수화물(NiCl2·6H2O) 30 내지 60g/L를 포함하는 도금액을 사용한다.Preferably, the metal chloride is at least one selected from tin chloride (SnCl 2 ) and palladium chloride (PdCl 2 ). Further, the plating step uses a plating solution containing 200 to 350 g / L of nickel sulfate hydrate (NiSO 4 · 6H 2 O) and 30 to 60 g / L of nickel chloride hydrate (NiCl 2 · 6H 2 O).
상기와 같은 본 발명에 따르면, 전기전도성이 향상 된 멜트블로운 섬유웹을 제공하는 효과가 있다.According to the present invention, it is possible to provide a meltblown fibrous web having improved electrical conductivity.
또한 전기전도도가 향상 된 멜트블로운 섬유웹을 제공함으로써, 상기 섬유웹을 여과재, 흡수재, 흡음재, 절연재, 축열재 및 전자파 차폐제로 활용하는 방안을 제공하는 효과가 있다.Further, by providing a meltblown fibrous web having improved electrical conductivity, it is possible to provide a method of utilizing the fibrous web as a filter medium, an absorbing material, a sound absorbing material, an insulating material, a heat storage material, and an electromagnetic wave shielding material.
또한 섬유웹 제조 시 멜트블로운 공정을 적용함으로서, 전기전도도가 향산된 섬유웹을 대량생산이 가능하다.In addition, by applying the meltblown process in the production of fiber web, it is possible to mass-produce a fibrous web having improved electrical conductivity.
도 1은 본 발명의 일 실시예에 따른 멜트블로운 섬유웹 제조과정의 도식화한 것이다.FIG. 1 is a schematic view of a process for producing a meltblown fiber web according to an embodiment of the present invention.
이하, 본 발명을 상세히 설명한다.Hereinafter, the present invention will be described in detail.
본 발명의 일 형태에 따른 전기전도성이 향산된 멜트블로운 섬유웹의 제조방법은 폴리프로필렌(Polypropylene, PP) 수지를 용융압출하여 펠릿을 제조하는 펠릿제조단계, 펠릿을 열풍기류에 분사하여 섬유웹을 제조하는 방사단계, 금속염화물로 섬유웹 표면을 활성화시키는 활성화 단계 및 표면이 활성화된 섬유웹을 니켈 도금하는 도금단계를 포함한다.A method for producing a meltblown fibrous web enriched with electrical conductivity according to an embodiment of the present invention includes the steps of producing a pellet by melt extruding a polypropylene (PP) resin, pelletizing the pellet into a hot air stream, An activation step of activating the fiber web surface with metal chloride, and a plating step of nickel plating the surface-activated fiber web.
펠릿제조단계는 폴리프로필렌 수지를 130 내지 200℃에서 용융압출하는 것을 특징으로 한다. 구체적으로, 펠릿제조단계는 압출구는 3구이며, 직경은 5mm인 단축 압출성형기를 사용하고, 최종적으로 직경 2mm, 길이 10mm인 나노 복합형 펠릿을 제조한다. The pellet production step is characterized in that the polypropylene resin is melt-extruded at 130 to 200 ° C. Specifically, in the pellet production step, a nanocomposite pellet having a diameter of 2 mm and a length of 10 mm is finally manufactured using a single extrusion extruder having three extruded sections and a diameter of 5 mm.
방사단계의 열풍기류는 공기 공급 속도 80 내지 400m/s, 공기 공급 온도 200 내지 350℃인 고속 열풍기류인 것을 특징으로 한다. 상기 공기 공급 온도는 200 내지 350℃인 것이 바람직하다. 방사온도가 200℃미만일 경우 혼합물이 완전히 용융되지 않아 섬유가 끊어지거나 뭉치는 현상이 발생하고, 350℃를 초과할 경우 공기 공급 온도를 유지하는 비용이 증가하므로 바람직하지 않다.The hot air stream in the spinning stage is a high-speed hot air stream having an air supply rate of 80 to 400 m / s and an air supply temperature of 200 to 350 ° C. The air supply temperature is preferably 200 to 350 ° C. When the spinning temperature is lower than 200 ° C, the mixture is not completely melted and the fibers are broken or aggregated. When the temperature exceeds 350 ° C, the cost of maintaining the air supply temperature is increased.
또한 방사단계는 분사된 펠릿을 회전속도 600 내지 150mm/s인 수집체로 수집하는 것을 특징으로 한다. 수집체의 속도가 600mm/s 이상인 경우 나노섬유가 용융방사 후 수집체에서 연속적으로 수집되지 못해 끊어지는 현상이 발생해 바람직하지 못하며, 수집체의 속도가 150mm/s 이하인 경우는 용융방사 후 나노섬유가 적절한 속도로 수집되지 못해 섬유가 뭉치므로 바람직하지 않다.The spinning step is also characterized by collecting the injected pellets with an aggregate having a rotational speed of 600 to 150 mm / s. If the velocity of the collecting body is 600 mm / s or more, the nanofibers can not be continuously collected from the collecting body after the melt-spinning process, which is undesirable. If the speed of the collecting body is 150 mm / s or less, Can not be collected at an appropriate speed and the fibers are bundled, which is not desirable.
활성화단계의 금속염화물은 염화주석(SnCl2) 및 염화팔라듐(PdCl2) 중에서 선택되는 1이상인 것을 특징으로 한다. 염화주성 또는 염화팔라듐으로 활성화 시킬 경우 섬유 표면에 주석 이온과 팔라듐 이온이 형성된다. 상기 섬유표면에 형성된 주석이온과 팔라듐이온은 환원제로서 성능이 우수하여 니켈도금 효율을 향상시킨다.The metal chloride in the activation step is characterized by being at least one selected from tin chloride (SnCl 2 ) and palladium chloride (PdCl 2 ). When activated by chlorination or palladium chloride, tin and palladium ions are formed on the fiber surface. The tin ions and palladium ions formed on the surface of the fiber have excellent performance as a reducing agent, thereby improving the nickel plating efficiency.
도금단계는 황산니켈 수화물(NiSO4·6H2O) 200 내지 350g/L, 염화니켈 수화물(NiCl2·6H2O) 30 내지 60g/L를 포함하는 도금액을 사용하는 것을 특징으로 한다. 황산니켈 수화물이 200g/L 이하의 농도인 경우 니켈의 환원이 일어나기에 충분하지 못한 농도이며, 350g/L의 농도의 경우 니켈 이온이 과량 함유 되어 뭉침 현상이 발생할 수 있기 때문에 바람직하지 않다. 또한, 염화니켈 수화물의 경우 또한 30g/L의 농도는 환원이 일어나기에 충분하지 못한 농도이며, 60g/L의 농도의 경우 과량의 니켈 이온으로 뭉침 현상이 발생하기 때문에 바람직하지 않다.The plating step is characterized by using a plating solution containing 200 to 350 g / L of nickel sulfate hydrate (NiSO 4 · 6H 2 O) and 30 to 60 g / L of nickel chloride hydrate (NiCl 2 · 6H 2 O). When the concentration of nickel sulfate hydrate is less than 200 g / L, the concentration is not enough to cause reduction of nickel. When the concentration of 350 g / L is excessive, nickel ions are excessively contained and aggregation may occur. Also, in the case of nickel chloride hydrate, the concentration of 30 g / L is not enough to cause reduction, and the concentration of 60 g / L is not preferable because excessive nickel ions may cause aggregation.
이하, 실시예를 통하여 본 발명을 더욱 상세히 설명하고자 한다. 이들 실시예는 오로지 본 발명을 예시하기 위한 것으로서, 본 발명의 범위가 이들 실시예에 의해 제한되는 것으로 해석되지는 않는 것은 당업계에서 통상의 지식을 가진 자에게 있어서 자명할 것이다.Hereinafter, the present invention will be described in more detail with reference to Examples. It is to be understood by those skilled in the art that these examples are for illustrative purposes only and that the scope of the present invention is not construed as being limited by these examples.
실시예Example 1. One.
폴리프로필렌(PP) 수지를 압출성형기를 이용하여 130℃의 온도로 용융압출하여 펠릿을 제조한다. 제조된 펠릿은 멜트블로운(melt-blown)기기를 이용하여 공기공급속도 80m/s, 공기공급온도 200℃인 고속 열풍기류에 분사시켜 방사한다. 이때의 수집체의 회전속도는 60mm/s로 하고, 방사구금과 수집체간의 거리(die-to-collector-distance, DCD)를 100mm로 방사하여 고분자 섬유웹을 제조한다.The polypropylene (PP) resin is melt-extruded at a temperature of 130 캜 using an extruder to produce pellets. The prepared pellets are sprayed into a high-speed hot air stream having an air supply rate of 80 m / s and an air supply temperature of 200 ° C by means of a melt-blown apparatus. The spinning speed of the collector at this time is 60 mm / s, and the distance between the spinneret and the collector (DCD) is 100 mm to produce a polymer fiber web.
제조된 섬유웹을 5M 질산수용액으로 30분 동안 전처리하고, 세척 및 건조한다. 또한 질산수용액으로 전처리 된 섬유웹을 염화주석(SnCl2)용액에서 5분 동안 활성화 시킨 후 세척한다. 그리고 염화팔라듐(PdCl2) 용액에서 5분 동안 활성화시킨다. 활성화 된 섬유웹을 니켈 무전해 도금액에 넣어, 온도 50℃에서 1분간 담지하여 니켈이 코팅된 멜트블로운 섬유웹을 제조한다. 상기 니켈 무전해 도금액의 조성은 NiSO46H2O 280g/L, NiCl26H2O 40g/L, Na3C6H5O71.5H2O 15g/L, NaH2PO22H2O 100g/L, NH4Cl 100g/L 및 PbNO3 30g/L이다.The prepared fibrous web is pretreated with 5M nitric acid aqueous solution for 30 minutes, washed and dried. Also, the fibrous web pretreated with aqueous nitric acid solution is activated for 5 minutes in tin chloride (SnCl 2 ) solution and then washed. And activated in a solution of palladium chloride (PdCl 2 ) for 5 minutes. The activated fiber web is placed in a nickel electroless plating solution and is held at a temperature of 50 ° C for 1 minute to prepare a nickel-coated meltblown fiber web. The composition of the nickel electroless plating solution NiSO 4 6H 2 O 280g / L , NiCl 2 6H 2 O 40g / L, Na 3 C 6 H 5 O 7 1.5H 2 O 15g / L, NaH 2 PO 2 2H 2 O 100g / L, NH 4 Cl 100 g / L and PbNO 3 30 g / L.
실시예Example 2. 2.
상기 실시예 1과 동일하게 실시하되, 공기공급속도를 100m/s, 수집체의 회전속도 80mm/s로 한다. 또한 염화주석(SnCl2)용액과 염화팔라듐(PdCl2)을 이용한 활성화를 각각 10분간 수행한다. 또한 도금을 온도 60℃에서 3분간 수행하여 니켈이 코팅된 멜트블로운 섬유웹을 제조한다.The same procedure as in Example 1 was carried out except that the air supply rate was 100 m / s and the rotation speed of the collector was 80 mm / s. Activation with tin chloride (SnCl 2 ) solution and palladium chloride (PdCl 2 ) is also carried out for 10 minutes each. The plating was also carried out at a temperature of 60 캜 for 3 minutes to prepare a nickel-coated meltblown fiber web.
실시예Example 3. 3.
상기 실시예 2와 동일하게 실시하되, 용융압출 온도를 150℃, 공기공급속도 150m/s, 공기 공급온도를 250℃로 한다. 또한 수집체의 회전속도는 100mm/s로 하고, DCD를 120mm로 하여 방사한다. 그 후 염화주석(SnCl2)용액을 이용한 활성화 20분, 염화팔라듐(PdCl2)을 이용한 활성화를 10분간 수행한다. 또한 도금을 온도 70℃에서 5분간 수행하여 니켈이 코팅된 멜트블로운 섬유웹을 제조한다.The same procedure as in Example 2 was carried out except that the melt extrusion temperature was 150 캜, the air supply rate was 150 m / s, and the air supply temperature was 250 캜. Also, the rotation speed of the collector is 100 mm / s, and the DCD is 120 mm. Thereafter, activation with tin chloride (SnCl 2 ) solution for 20 minutes and activation with palladium chloride (PdCl 2 ) is carried out for 10 minutes. The plating was also carried out at a temperature of 70 캜 for 5 minutes to prepare a nickel-coated meltblown fiber web.
실시예Example 4. 4.
상기 실시예 3과 동일하게 실시하되, 공기공급속도 200m/s, DCD를 150mm로 하며, 그 후 염화주석(SnCl2)용액과 염화팔라듐(PdCl2)을 이용한 활성화를 각각 20분동안 수행한다. 또한 도금온도 80℃, 도금시간 10분으로 하여 니켈이 코팅된 멜트블로운 섬유웹을 제조한다.The same procedure as in Example 3 was carried out except that the air supply rate was 200 m / s and the DCD was 150 mm. After that, activation using tin chloride (SnCl 2 ) solution and palladium chloride (PdCl 2 ) was carried out for 20 minutes each. Further, a nickel-coated meltblown fiber web was prepared at a plating temperature of 80 캜 and a plating time of 10 minutes.
실시예Example 5. 5.
상기 실시예 4와 동일하게 실시하되, 용융압출 온도를 150℃, 공기공급온도를 300℃로 한다. 또한 수집체의 회전속도는 120mm/s로 하고, DCD를 200mm로 하여 방사한다. 그 후 염화주석(SnCl2)용액와 염화팔라듐(PdCl2)을 이용한 활성화를 각각 20분간 수행한다. 또한 도금온도 85℃, 도금시간 10분으로 하여 니켈이 코팅된 멜트블로운 섬유웹을 제조한다.The same procedure as in Example 4 was carried out except that the melt extrusion temperature was 150 ° C and the air supply temperature was 300 ° C. Also, the rotating speed of the collector is set to 120 mm / s and the DCD is set to 200 mm. Thereafter, activation with a solution of tin chloride (SnCl 2 ) and palladium chloride (PdCl 2 ) is carried out for 20 minutes each. Also, the nickel-coated meltblown fiber web was prepared at a plating temperature of 85 ° C and a plating time of 10 minutes.
실시예Example 6. 6.
상기 실시예 4와 동일하게 실시하되, 공기 공급속도를 300m/s로, DCD를250mm로 하여 방사한다. 그 후 염화주석(SnCl2)용액을 이용한 활성화 30분, 염화팔라듐(PdCl2)을 이용한 활성화를 45분간 수행한다. 또한 도금온도 90℃, 도금시간 20분으로 하여 니켈이 코팅된 멜트블로운 섬유웹을 제조한다.The same procedure as in Example 4 was carried out except that the air feeding rate was 300 m / s and the DCD was 250 mm. The activation is then carried out for 30 minutes with tin chloride (SnCl 2 ) solution and with palladium chloride (PdCl 2 ) for 45 minutes. Further, a nickel-coated meltblown fiber web was prepared at a plating temperature of 90 ° C and a plating time of 20 minutes.
실시예Example 7. 7.
상기 실시예 6과 동일하게 실시하되, 용융압출온도를 200℃, 공기공급온도를 350℃로 한다. 이 때 수집체의 회전속도는 150mm/s로하고 DCD를 300mm로 하여 방사한다. 그 후 염화주석(SnCl2)용액와 염화팔라듐(PdCl2)을 이용한 활성화를 각각 45분간 수행한다. 또한 도금온도 100℃하여 니켈이 코팅된 멜트블로운 섬유웹을 제조한다.The same procedure as in Example 6 was carried out except that the melt extrusion temperature was 200 占 폚 and the air supply temperature was 350 占 폚. At this time, the rotation speed of the collecting body is 150 mm / s and the DCD is 300 mm. Subsequently, the activation with a solution of tin chloride (SnCl 2 ) and palladium chloride (PdCl 2 ) is carried out for 45 minutes each. Further, a plating temperature of 100 占 폚 is used to produce a nickel-coated meltblown fibrous web.
실시예Example 8. 8.
상기 실시예 7과 동일하게 실시하되, 공기공급 송도를 400m/s로 하고, DCD를 400mm로 하여 방사한다. 그 후 염화주석(SnCl2)용액과 염화팔라듐(PdCl2)을 이용한 활성화를 각각 60분간 수행한다. 또한 도금시간 30분으로 하여 니켈이 코팅된 멜트블로운 섬유웹을 제조한다.The same procedure as in Example 7 was carried out except that the air feeding rate was 400 m / s and the DCD was 400 mm. Subsequently, activation with a solution of tin chloride (SnCl 2 ) and palladium chloride (PdCl 2 ) is carried out for 60 minutes each. Also, a nickel-coated meltblown fiber web was prepared at a plating time of 30 minutes.
비교예Comparative Example 1. One.
상기 실시예 5와 동일하게 과정을 실시하되, 펠릿을 제조하지 않고 방사하여 니켈이 코팅된 멜트블로운 섬유웹을 제조한다.The procedure of Example 5 was followed except that the meltblown fibrous web coated with nickel was prepared by spinning without preparing the pellets.
비교예Comparative Example 2. 2.
상기 실시예 5와 동일하게 실시하되, 무전해 니켈도금을 하지 않고 멜트블로운 섬유웹을 측정하였다. A meltblown fiber web was measured in the same manner as in Example 5 except that electroless nickel plating was not performed.
(oC)The temperature of the melt extruded part
( o C)
(m/s)Air supply speed
(m / s)
(oC)Air supply temperature
( o C)
회전속도
(mm/s)Collector
Rotation speed
(mm / s)
(mm)DCD
(mm)
활성화 시간(min)SnCl 2
Activation time (min)
활성화
시간(min)PdCl 2
Activation
Time (min)
측정예Measurement example 1. 전기전도도 측정 1. Electrical Conductivity Measurement
Four-probe point method with resistivity tester(MCP-T610,Misubishi Chemical Analytech Co., Ltd.)을 통해 각 실시예에 따라 제조된 멜트블로운 섬유웹의 비저항를 측정하였다. 측정한 비저항 값을 이용하여 전기전도도를 계산하였다.The resistivity of the meltblown fiber web prepared according to each example was measured through a four-probe point method with a resistivity tester (MCP-T610, Misubishi Chemical Analytech Co., Ltd.). The electrical conductivity was calculated using the measured resistivity values.
이상, 본 발명내용의 특정한 부분을 상세히 기술하였는바, 당업계의 통상의 지식을 가진 자에게 있어서, 이러한 구체적인 기술은 단지 바람직한 실시양태일 뿐이며, 이에 의해 본 발명의 범위가 제한되는 것이 아닌 점은 명백할 것이다. 따라서 본 발명의 실질적인 범위는 첨부된 청구항들과 그것들의 등가물에 의해 정의된다고 할 것이다. Having described specific portions of the present invention in detail, those skilled in the art will appreciate that these specific embodiments are merely preferred embodiments and that the scope of the present invention is not limited thereby. something to do. Accordingly, the actual scope of the present invention will be defined by the appended claims and their equivalents.
Claims (6)
펠릿을 열풍기류에 분사하여 섬유웹을 제조하는 방사단계;
금속염화물로 섬유웹 표면을 활성화시키는 활성화단계; 및
표면이 활성화된 섬유웹을 니켈 도금하는 도금단계를 포함하고,
상기 펠릿제조단계는 폴리프로필렌 수지를 온도 150 내지 200 ℃에서 용융압출하고,
상기 열풍기류는 공기 공급속도 200 내지 300 m/s, 공기 공급온도 250 내지 350 ℃인 고속 열풍기류이고,
상기 방사단계는 분사된 펠릿을 회전속도 100 내지 150 mm/s인 수집체로 수집하고,
상기 금속염화물은 염화주석(SnCl2) 및 염화팔라듐(PdCl2)을 중에서 선택되는 1 이상 이고,상기 도금 단계는 황산니켈 수화물(NiSO4·6H2O) 280g/L, 염화니켈 수화물(NiCl2·6H2O) 40 g/L, 시트르산나트륨 수화물(Na3C6H5O7·1.5H2O) 15g/L, 인산나트륨 수화물(NaH2PO2·2H2O) 100 g/L 를 포함하는 도금액을 사용하는 것을 특징으로 하는 전기전도성이 향상된 멜트블로운 섬유웹의 제조방법.
A pellet manufacturing step of producing a pellet by melt-extruding a polypropylene (PP) resin;
A spinning step of spinning the pellets into a hot air stream to produce a fibrous web;
An activation step of activating the fiber web surface with a metal chloride; And
And a plating step of nickel plating the surface-activated fibrous web,
The pellet-making step comprises melt-extruding the polypropylene resin at a temperature of 150 to 200 DEG C,
The hot air current is a high-speed hot air current having an air supply rate of 200 to 300 m / s and an air supply temperature of 250 to 350 DEG C,
The spinning step collecting the injected pellets with an aggregate having a rotation speed of 100 to 150 mm / s,
The metal chloride is stannous chloride (SnCl 2), and is 1 or more selected from palladium chloride (PdCl 2), the plating step of nickel sulfate hydrate (NiSO 4 · 6H 2 O) 280g / L, nickel chloride hydrate (NiCl 2 · 6H 2 O) 40 g / L, sodium citrate monohydrate (Na 3 C 6 H 5 O 7 · 1.5H 2 O) 15g / L, sodium phosphate monohydrate (NaH 2 PO 2 · 2H 2 O) to 100 g / L Wherein the plating liquid is a plating liquid containing a plating liquid.
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KR102003061B1 (en) | 2019-02-01 | 2019-07-24 | 주식회사 제타글로벌 | Method for Manufacturing carbon nanofibers and carbon nanofibers manufactured by the method |
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US3647514A (en) * | 1968-08-28 | 1972-03-07 | Knapsack Ag | Surface-pretreatment of articles made from polyethylene or polypropylene or corresponding copolymers for chemical nickel-plating |
KR100230219B1 (en) * | 1991-12-31 | 1999-11-15 | 로날드 디. 맥크레이 | Conductive fabric and method of producing same |
KR20040054320A (en) * | 2002-12-18 | 2004-06-25 | 권만천 | Method for producing textiles of shielding electromagnetic wave and roller bar therefor |
KR20050107995A (en) * | 2004-05-11 | 2005-11-16 | 최철수 | Plating process of condutivity fiber |
KR20090049692A (en) * | 2007-11-14 | 2009-05-19 | (주)메인일렉콤 | Method for manufacturing textile coated with conductive metal |
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US3647514A (en) * | 1968-08-28 | 1972-03-07 | Knapsack Ag | Surface-pretreatment of articles made from polyethylene or polypropylene or corresponding copolymers for chemical nickel-plating |
KR100230219B1 (en) * | 1991-12-31 | 1999-11-15 | 로날드 디. 맥크레이 | Conductive fabric and method of producing same |
KR20040054320A (en) * | 2002-12-18 | 2004-06-25 | 권만천 | Method for producing textiles of shielding electromagnetic wave and roller bar therefor |
KR20050107995A (en) * | 2004-05-11 | 2005-11-16 | 최철수 | Plating process of condutivity fiber |
KR20090049692A (en) * | 2007-11-14 | 2009-05-19 | (주)메인일렉콤 | Method for manufacturing textile coated with conductive metal |
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KR102003061B1 (en) | 2019-02-01 | 2019-07-24 | 주식회사 제타글로벌 | Method for Manufacturing carbon nanofibers and carbon nanofibers manufactured by the method |
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