KR102205528B1 - Method of manufacturing wet type aramid non-woven fabric - Google Patents

Method of manufacturing wet type aramid non-woven fabric Download PDF

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KR102205528B1
KR102205528B1 KR1020150112400A KR20150112400A KR102205528B1 KR 102205528 B1 KR102205528 B1 KR 102205528B1 KR 1020150112400 A KR1020150112400 A KR 1020150112400A KR 20150112400 A KR20150112400 A KR 20150112400A KR 102205528 B1 KR102205528 B1 KR 102205528B1
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filaments
aramid
nonwoven fabric
filament
organic solvent
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KR1020150112400A
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KR20170018589A (en
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구남대
김진일
박영철
이민호
이재영
서혁진
장승호
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코오롱인더스트리 주식회사
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    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING 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
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40Non-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
    • D04H1/42Non-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
    • D04H1/4326Condensation or reaction polymers
    • D04H1/4334Polyamides
    • D04H1/4342Aromatic polyamides
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING 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
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/70Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
    • D04H1/72Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
    • D04H1/724Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged forming webs during fibre formation, e.g. flash-spinning
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING 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
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/70Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
    • D04H1/72Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
    • D04H1/732Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by fluid current, e.g. air-lay

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Artificial Filaments (AREA)

Abstract

본 발명은 -CN기가 치환된 방향족기를 포함하는 아라미드 공중합체가 용해되어 있는 중합용매를 방사구금을 통해 필라멘트 형태로 방사한 후 방사되어 응고 전인 필라멘트들에 공기를 분사하여 상기 필라멘트들을 분산 및 교차시켜 필라멘트 웹을 형성한 다음, 상기 필라멘트 웹(Web)을 응고액으로 처리하여 필라멘트내 용매를 제거한 후, 차례로 수세 및 건조하여 습식 아라미드 부직포를 제조한다.
본 발명은 농황산에 의한 설비부식 없이도 아라미드 필라멘트들로 구성된 부직포를 제조할 수 있다. 또한 본 발명은 종래 아라미드 단섬유 제조공정과 비교시 공정이 간소화되고, 제조원가가 저렴해지고 생산성도 향상된다.
In the present invention, a polymerization solvent in which an aramid copolymer containing an aromatic group substituted with a -CN group is dissolved is spun in a filament form through a spinneret and then spun into the filaments before solidification by spraying air to disperse and cross the filaments. After the filament web is formed, the filament web is treated with a coagulating solution to remove the solvent in the filament, and then washed and dried with water to prepare a wet aramid nonwoven fabric.
The present invention can manufacture a nonwoven fabric composed of aramid filaments without equipment corrosion caused by concentrated sulfuric acid. In addition, the present invention simplifies the process, lowers the manufacturing cost, and improves productivity as compared to the conventional aramid short fiber manufacturing process.

Description

습식 아라미드 부직포의 제조방법{Method of manufacturing wet type aramid non-woven fabric}Method of manufacturing wet type aramid non-woven fabric

본 발명은 습식 아라미드 부직포의 제조방법에 관한 것으로서, 보다 구체적으로는 아라미드 필라멘트들로 구성된 부직포를 간소화된 공정과 높은 생산성으로 제조할 수 있는 습식 아라미드 부직포의 제조방법에 관한 것이다.The present invention relates to a method of manufacturing a wet aramid nonwoven fabric, and more specifically, to a method of manufacturing a wet aramid nonwoven fabric capable of manufacturing a nonwoven fabric composed of aramid filaments with a simplified process and high productivity.

이하, 본 발명에서는 아라미드 필라멘트들이 서로 얽히면서 교차점에서 서로 접착된 구조인 스펀본드(Spunbond)타입 또는 멜트브로운(Meltbrown)타입의 아라미드 부직포를 통칭하여 "아라미드 부직포"라고 한다.Hereinafter, in the present invention, the aramid nonwoven fabric of a spunbond type or meltbrown type, which is a structure in which aramid filaments are entangled with each other and bonded to each other at the intersection point, is collectively referred to as "aramid nonwoven fabric".

아라미드 단섬유들로 구성된 아라미드 단섬유 부직포는 내열성 및 내약품성이 뛰어나 고온 등의 극한 환경에서 사용되는 필터 소재 등으로 사용된다.Short aramid fibers composed of short aramid fibers are excellent in heat resistance and chemical resistance and are used as filter materials used in extreme environments such as high temperatures.

아라미드 단섬유 부직포를 제조하는 종래기술로는 미국등록특허 제3,869,428호 등에 기재된 바와 같이 파라페닐렌디아민(방향족 디아민)이 용해되어 있는 유기용매 내에 테레프탈로일디클로라이드(방향족 디에시드 할라이드)를 상기 파라페닐렌디아민과 동일한 몰량(Molar amount)으로 첨가, 중합하여 아라미드 중합체를 제조한 다음, 제조된 아라미드 중합체를 농황산에 녹여 방사용액을 제조한 다음, 제조된 방사용액을 방사구금을 통해 필라멘트상으로 방사, 응고, 수세 및 건조하여 아라미드 필라멘트를 제조한 다음, 제조된 아라미드 필라멘트를 절단하여 아라미드 단섬유(Staple)를 제조한 다음, 상기 아라미드 단섬유들을 카딩기에서 공급, 처리하여 아라미드 단섬유 웹을 제조한 다음, 제조된 상기 아라미드 단섬유 웹을 니들펀칭하여 아라미드 단섬유 부직포를 제조하는 방법이 사용되어 왔다.As a prior art for producing aramid short fiber nonwoven fabric, terephthaloyl dichloride (aromatic diecid halide) is added to the paraphenylenediamine in an organic solvent in which paraphenylenediamine (aromatic diamine) is dissolved, as described in U.S. Patent No. 3,869,428. The aramid polymer was prepared by adding and polymerizing the same molar amount as the rendiamine, and then dissolving the prepared aramid polymer in concentrated sulfuric acid to prepare a spinning solution, and then spinning the prepared spinning solution in a filament shape through a spinneret, Coagulation, washing and drying to prepare an aramid filament, then cutting the prepared aramid filament to prepare short aramid fibers (Staple), and then supplying and processing the short aramid fibers in a carding machine to prepare a short aramid fiber web Next, a method of producing a short aramid fiber nonwoven fabric by needle punching the prepared short aramid fiber web has been used.

상기 종래방법은 아라미드 단섬유 웹을 제조하는 공정이 너무 복잡하여 생산성이 떨어지는 문제점이 있었다.The conventional method has a problem in that the process of manufacturing the short aramid fiber web is too complicated and productivity is degraded.

상기 종래방법을 사용하는 방사용액에는 농황산이 포함되어 생산설비의 부식이 심하게 발생되었고, 농황산의 회수설비도 복잡해지는 문제가 있었다.Since the spinning solution using the conventional method contained concentrated sulfuric acid, corrosion of the production facility was severely generated, and the recovery facility for concentrated sulfuric acid was also complicated.

그로인해, 상기 종래방법으로는 아라미드 단섬유 부직포를 생산할 수 있으나, 아라미드 장섬유(필라멘트)들이 서로 얽히면서 접착된 스펀본드 타입 또는 멜트브로운 타입의 아라미드 부직포를 제조하기 어려운 문제점이 있었다.For this reason, the conventional method can produce aramid short fiber nonwoven, but there is a problem in that it is difficult to produce a spunbond type or melt blown type aramid nonwoven in which long aramid fibers (filaments) are entangled and bonded.

본 발명의 과제는 아라미드 필라멘트들로 구성된 스펀본드 타입 또는 멜트브로운 타입의 아라미드 부직포를 간소한 공정 및 높은 생산성으로 제조할 수 있는 방법을 제공하는 것이다.An object of the present invention is to provide a method for manufacturing a spunbond type or melt blown type aramid nonwoven fabric composed of aramid filaments with a simple process and high productivity.

이와같은 과제를 달성하기 위해서, 본 발명에서는 -CN기가 치환된 방향족기를 포함하는 아라미드 공중합체가 용해되어 있는 중합용매를 방사구금을 통해 필라멘트 형태로 방사한 후, 방사되어 응고 전인 필라멘트들에 공기를 분사하여 상기 필라멘트들을 분산 및 교차시켜 필라멘트 웹을 형성한 다음, 상기 필라멘트 웹(Web)을 응고액으로 처리하여 필라멘트내 용매를 제거한 후, 차례로 수세 및 건조하여 습식 아라미드 부직포를 제조한다.In order to achieve such a problem, in the present invention, a polymerization solvent in which an aramid copolymer containing an aromatic group substituted with a -CN group is dissolved is spun in a filament form through a spinneret, and then spun into the filaments before solidification. After spraying to form a filament web by dispersing and crossing the filaments, the filament web is treated with a coagulating solution to remove the solvent in the filament, and then washed and dried in sequence to prepare a wet aramid nonwoven fabric.

본 발명은 농황산에 의한 설비부식 없이도 아라미드 필라멘트들로 구성된 부직포를 제조할 수 있다. 또한 본 발명은 종래 아라미드 단섬유 제조공정과 비교시 공정이 간소화되고, 제조원가가 저렴해지고 생산성도 향상된다.The present invention can produce a nonwoven fabric composed of aramid filaments without equipment corrosion caused by concentrated sulfuric acid. In addition, the present invention simplifies the process, lowers the manufacturing cost, and improves productivity as compared to the conventional aramid short fiber manufacturing process.

이하, 본 발명을 상세하게 설명한다.Hereinafter, the present invention will be described in detail.

본 발명은 먼저, -CN 기를 포함하는 방향족 디아민이 용해되어 있는 유기용매에 테레프탈로일 디클로라이드를 첨가, 반응시켜 -CN기가 치환된 방향족기를 포함하는 아라미드 공중합체가 용해되어 있는 중합용액을 제조한다.In the present invention, first, terephthaloyl dichloride is added to an organic solvent in which an aromatic diamine containing a -CN group is dissolved and reacted to prepare a polymerization solution in which an aramid copolymer containing an aromatic group substituted with the -CN group is dissolved. .

구현일례로서, -CN기를 포함하는 방향족 디아민으로 시아노-파라-페닐렌 디아민을 단독으로 유기용매에 용해시킬 수 있다.As an exemplary embodiment, cyano-para-phenylene diamine may be dissolved in an organic solvent alone as an aromatic diamine containing a -CN group.

또 다른 구현일례로서, -CN기를 포함하는 방향족 디아민으로 시아노-파라-페닐렌 디아민과 파라페닐렌 디아민을 1:9~9:1의 몰비로 유기용매에 용해 시킬 수도 있다.As another embodiment, cyano-para-phenylene diamine and paraphenylene diamine as an aromatic diamine containing -CN group may be dissolved in an organic solvent in a molar ratio of 1:9 to 9::1.

구체적으로 먼저, 유기용매에 무기염을 용해시킨 다음 여기에 시아노기(-CN)를 포함하는 방향족 디아민을 첨가하여 용해시킨다.Specifically, first, an inorganic salt is dissolved in an organic solvent, and then an aromatic diamine containing a cyano group (-CN) is added thereto to dissolve it.

이때 시아노기(-CN)를 포함하는 방향족 디아민으로 파라페닐렌디아민과 시아노-파라-페닐렌디아민을 1:9~9:1의 몰비로 용해할 수도 있고, 시아노-파라-페닐렌디아민을 단독으로 용해할 수도 있다.At this time, as an aromatic diamine containing a cyano group (-CN), paraphenylenediamine and cyano-para-phenylenediamine may be dissolved in a molar ratio of 1:9 to 9:1, or cyano-para-phenylenediamine Can also be dissolved alone.

상기 유기용매의 구체적인 예로는 N-메틸-2-피롤리돈(NMP), N,N-디메틸아세트아미드(DMAc), 헥사메틸포스포아미드(HMPA), N,N,N',N'-테트라메틸 우레아(TMU), N,N-디메틸포름아미드(DMF), 또는 이들의 혼합물을 들 수 있고, N-메틸-2-피롤리돈(NMP)인 것이 보다 바람직하다.Specific examples of the organic solvent include N-methyl-2-pyrrolidone (NMP), N,N-dimethylacetamide (DMAc), hexamethylphosphoamide (HMPA), N,N,N',N'- Tetramethyl urea (TMU), N,N-dimethylformamide (DMF), or a mixture thereof, and more preferably N-methyl-2-pyrrolidone (NMP).

상기 무기염은 방향족 폴리아미드의 중합도를 증가시키기 위하여 첨가하는 것으로서, 그 구체적인 예로는 CaCl2, LiCl, NaCl, KCl, LiBr 및 KBr 등과 같은 할로겐화 알칼리 금속염 또는 할로겐화 알칼리 토금속염을 들 수 있다. 이들 무기염은 단독으로 또는 2종 이상의 혼합물의 형태로 첨가될 수 있다. The inorganic salt is added to increase the degree of polymerization of the aromatic polyamide, and specific examples thereof include a halogenated alkali metal salt or a halogenated alkaline earth metal salt such as CaCl 2 , LiCl, NaCl, KCl, LiBr and KBr. These inorganic salts may be added alone or in the form of a mixture of two or more.

상기 무기염의 첨가량은 유기용매 중량 대비 2~5중량% 정도인 것이 바람직하다.The amount of the inorganic salt added is preferably about 2 to 5% by weight based on the weight of the organic solvent.

다음으로는, 상기와 같이 -CN기를 포함하는 방향족 디아민이 첨가, 용해된 유기용매에 테레프탈로일 디클로라이드를 상기 방향족 디아민 성분과 동일한 몰량(Molar amount)으로 첨가하여 공중합 아라미드 중합체를 포함하는 중합용매를 제조한다.Next, a polymerization solvent containing a copolymerized aramid polymer by adding terephthaloyl dichloride in the same molar amount as the aromatic diamine component to the dissolved organic solvent by adding an aromatic diamine containing -CN as described above. To manufacture.

다음 공정으로는, 상기 중합용액을 방사구금을 통해 필라멘트상으로 방사한 후, 방사되어 응고 전인 필라멘트들에 공기를 분사하여 상기 필라멘트들을 분산 및 교차시켜 필라멘트 웹(Web)을 제조한다.In the next process, the polymerization solution is spun into filaments through a spinneret, and then air is sprayed on the filaments that are spun and before solidification to disperse and cross the filaments to produce a filament web.

이때, 방사되어 응고 전인 필라멘트에 공기를 분사함과 동시에 정전기를 부여하여 상기 필라멘트들을 웹(Web) 형태로 분산 및 교차시켜 스펀본드(Spunbond) 타입의 부직포를 제조하거나, 또 다른 구현예로서 방사구금 직하 위치에서 방사되어 응고 전인 필라멘트에 고압의 공기를 분사하여 상기 필라멘트들을 연신시킴과 동시에 웹(Web) 형태로 분산/교차시켜 멜트브로운(Meltbrown) 타입의 부직포를 제조한다.At this time, the spunbond type nonwoven fabric is manufactured by spraying air to the filaments that are spun and before solidification and at the same time giving static electricity to disperse and cross the filaments in a web form, or as another embodiment, spinneret A high-pressure air is sprayed on the filaments that are spun from a direct position and before solidification to stretch the filaments and at the same time disperse/cross the filaments in a web form to produce a meltbrown type nonwoven fabric.

다음 공정으로는, 상기 필라멘트 웹(Web)을 응고액으로 처리하여 필라멘트내 용매를 제거하는 응고공정을 실시한다.In the next step, a solidification step of removing the solvent in the filament by treating the filament web with a solidifying solution is performed.

상기 응고액으로는 물을 사용하거나 상기 유기용매 수용액을 사용할 수 있다.Water or the organic solvent aqueous solution may be used as the coagulant.

다음 공정으로는, 응고 공정을 거친 상기 필라멘트 웹(Web)을 수세 및 건조하여 본 발명의 습식 아라미드 부직포를 제조한다.In the next step, the filament web that has undergone a coagulation process is washed with water and dried to prepare the wet aramid nonwoven fabric of the present invention.

본 발명은 농황산에 의한 설비부식 없이도 아라미드 필라멘트들로 구성된 부직포를 제조할 수 있다. 또한 본 발명은 종래 아라미드 단섬유 제조공정과 비교시 공정이 간소화되고, 제조원가가 저렴해지고 생산성도 향상된다.The present invention can produce a nonwoven fabric composed of aramid filaments without equipment corrosion caused by concentrated sulfuric acid. In addition, the present invention simplifies the process, lowers the manufacturing cost, and improves productivity as compared to the conventional aramid short fiber manufacturing process.

이하, 실시예를 통하여 본 발명을 구체적으로 살펴본다.Hereinafter, the present invention will be described in detail through examples.

그러나, 하기 실시예는 본 발명의 바람직한 구현일례일뿐, 본 발명의 보호범위를 한정하는 것으로 해석되어서는 안된다.However, the following examples are only examples of preferred embodiments of the present invention, and should not be construed as limiting the protection scope of the present invention.

실시예 1Example 1

3중량%의 CaCl2를 포함하는 N-메틸-2-피롤리돈(NMP) 유기용매를 질소 분위기 하에서 반응기 내에 넣고, 파라-페닐렌디아민(p-phenylenediamine) 50 몰%와 시아노-파라-페닐렌디아민(cyano-p-phenylenediamine) 50 몰%를 상기 반응기에 넣고 녹여서 혼합용액을 제조하였다.N-methyl-2-pyrrolidone (NMP) organic solvent containing 3% by weight of CaCl 2 was put into the reactor under a nitrogen atmosphere, and 50 mol% of para-phenylenediamine and cyano-para- 50 mol% of phenylenediamine (cyano-p-phenylenediamine) was added to the reactor and dissolved to prepare a mixed solution.

이어서 상기 혼합용액이 담긴 반응기에 테레프탈로일 디클로라이드 100몰%를 첨가하여 공중합 아라미드 중합체를 포함하는 중합용액을 제조하였다.Subsequently, 100 mol% of terephthaloyl dichloride was added to the reactor containing the mixed solution to prepare a polymerization solution containing a copolymerized aramid polymer.

이어서, 상기 중합용액을 방사구금을 통해 필라멘트 상으로 압출한 후 방사되어 응고 전인 상기 필라멘트들에 공기를 분사하면서 정전기를 부여하여 상기 필라멘트들을 분산 및 교차시켜 필라멘트 웹(Web)을 제조하였다.Subsequently, the polymerization solution was extruded onto a filament through a spinneret and spun to give static electricity while spraying air on the filaments before solidification, thereby dispersing and crossing the filaments to prepare a filament web.

상기와 같이 제조된 필라멘트 웹(Web) 내에서 서로 교차하는 필라멘트 간의 교차점에서는 필라멘트들이 본딩(bonding)되어 있었다.In the filament web prepared as described above, the filaments were bonded at the crossing points between the filaments crossing each other.

다음으로는, 상기와 같이 제조된 웹(Web)을 물(응고액) 속으로 통과시켜 필라멘트들 내에 남아있는 용매를 제거하는 응고 공정을 실시한 다음, 응고 공정을 거친 상기 필라멘트 웹(Web)을 수세 및 건조하여 스펀본드(Spunbond) 타입의 습식 부직포를 제조하였다.Next, a solidification process in which the prepared web is passed through water (coagulation solution) to remove the solvent remaining in the filaments, and then the filament web after the solidification process is washed with water. And dried to prepare a spunbond type wet nonwoven fabric.

실시예 2Example 2

3중량%의 CaCl2를 포함하는 N-메틸-2-피롤리돈(NMP) 유기용매를 질소 분위기 하에서 반응기 내에 넣고, 시아노-파라-페닐렌디아민(cyano-p-phenylenediamine) 100 몰%를 상기 반응기에 넣고 녹여서 혼합용액을 제조하였다.N-methyl-2-pyrrolidone (NMP) organic solvent containing 3% by weight of CaCl 2 was put in a reactor under a nitrogen atmosphere, and 100 mol% of cyano-p-phenylenediamine was added. Put in the reactor and melted to prepare a mixed solution.

이어서 상기 혼합용액이 담긴 반응기에 테레프탈로일 디클로라이드 100몰%를 첨가하여 공중합 아라미드 중합체를 포함하는 중합용액을 제조하였다.Subsequently, 100 mol% of terephthaloyl dichloride was added to the reactor containing the mixed solution to prepare a polymerization solution containing a copolymerized aramid polymer.

이어서, 상기 중합용액을 방사구금을 통해 필라멘트 상으로 압출한 후 방사구금 직하의 위치에서 방사되어 응고 전인 상기 필라멘트들에 공기를 분사하여 상기 필라멘트들을 연신 및 분산시켜 필라멘트 웹(Web)을 제조하였다.Subsequently, the polymerization solution was extruded onto a filament through a spinneret, and then spun at a position directly under the spinneret, and air was sprayed on the filaments before solidification to stretch and disperse the filaments to prepare a filament web.

상기와 같이 제조된 필라멘트 웹(Web) 내에서 서로 교차하는 필라멘트 간의 교차점에서는 필라멘트들이 본딩(bonding)되어 있었다.The filaments were bonded at the crossing points between the filaments crossing each other in the filament web prepared as described above.

다음으로는, 상기와 같이 제조된 웹(Web)을 물(응고액) 속으로 통과시켜 필라멘트들 내에 남아있는 용매를 제거하는 응고 공정을 실시한 다음, 응고 공정을 거친 상기 필라멘트 웹(Web)을 수세 및 건조하여 멜트브로운(Meltblown) 타입의 습식 부직포를 제조하였다.Next, a solidification process in which the prepared web is passed through water (coagulation solution) to remove the solvent remaining in the filaments, and then the filament web after the solidification process is washed with water. And dried to produce a melt blown (Meltblown) type wet nonwoven fabric.

Claims (8)

(ⅰ) -CN 기를 포함하는 방향족 디아민이 용해되어 있는 유기용매에 테레프탈로일 디클로라이드를 첨가, 반응시켜 -CN기가 치환된 방향족기를 포함하는 아라미드 공중합체가 용해되어 있는 중합용액을 제조하는 공정;
(ⅱ) 상기 중합용액을 방사구금을 통해 필라멘트상으로 방사한 후, 방사되어 응고 전인 필라멘트들에 공기를 분사함과 동시에 정전기를 부여하여 상기 필라멘트들을 분산 및 교차시켜 필라멘트 웹(Web)을 제조하는 공정;
(ⅲ) 상기 필라멘트 웹(Web)을 응고액으로 처리하여 필라멘트내 용매를 제거하는 응고 공정; 및
(ⅳ) 응고 공정을 거친 상기 필라멘트 웹(Web)을 수세 및 건조하는 공정;을 포함하는 것을 특징으로 하는 습식 아라미드 부직포의 제조방법.
(I) adding terephthaloyl dichloride to an organic solvent in which an aromatic diamine containing a -CN group is dissolved, and reacting to prepare a polymerization solution in which an aramid copolymer containing an aromatic group substituted with a -CN group is dissolved;
(Ii) After spinning the polymerization solution into filaments through a spinneret, air is sprayed on the filaments that are spun and before solidification, and at the same time, static electricity is applied to disperse and cross the filaments to produce a filament web. fair;
(Iii) a coagulation step of removing the solvent in the filament by treating the filament web with a coagulating solution; And
(Iv) a process of washing and drying the filament web (Web) that has undergone a solidification process with water.
제1항에 있어서, 응고액은 물 및 물과 유기용매의 혼합물 중에서 선택된 1종인 것을 특징으로 하는 습식 아라미드 부직포의 제조방법.The method of claim 1, wherein the coagulating solution is one selected from water and a mixture of water and an organic solvent. 제1항에 있어서, 상기 유기용매는 N-메틸-2-피롤리돈(NMP), N,N-디메틸아세트아미드(DMAC), 헥사메틸포스포아미드(HMPA), N,N,N',N'-테트라메틸 우레아(TMU) 및 N,N-디메틸포름아미드(DMF) 중에서 선택된 1종 또는 2종 이상의 혼합물인 것을 특징으로 하는 습식 아라미드 부직포의 제조방법.The method of claim 1, wherein the organic solvent is N-methyl-2-pyrrolidone (NMP), N,N-dimethylacetamide (DMAC), hexamethylphosphoamide (HMPA), N,N,N', A method for producing a wet aramid nonwoven fabric, characterized in that it is one or a mixture of two or more selected from N'-tetramethyl urea (TMU) and N,N-dimethylformamide (DMF). 삭제delete 제1항에 있어서, 방사구금 직하 위치에서 방사되어 응고 전인 필라멘트에 공기를 분사하여 상기 필라멘트들을 분산과 동시에 연신시키는 것을 특징으로 하는 습식 아라미드 부직포의 제조방법.The method of claim 1, wherein the filaments are spun at a position directly under the spinneret and sprayed onto the filaments before solidification to disperse and simultaneously stretch the filaments. 제1항에 있어서, -CN기를 포함하는 방향족 디아민으로 시아노-파라-페닐렌디아민을 유기용매에 용해시키는 것을 특징으로 하는 습식 아라미드 부직포의 제조방법.The method for producing a wet aramid nonwoven fabric according to claim 1, wherein cyano-para-phenylenediamine is dissolved in an organic solvent as an aromatic diamine containing a -CN group. 제1항에 있어서, -CN기를 포함하는 방향족 디아민으로 시아노-파라-페닐렌디아민과 파라페닐렌디아민을 1:9~9:1의 몰비로 유기용매에 용해시키는 것을 특징으로 하는 습식 아라미드 부직포의 제조방법.The wet aramid nonwoven fabric according to claim 1, wherein cyano-para-phenylenediamine and paraphenylenediamine are dissolved in an organic solvent in a molar ratio of 1:9 to 9:1 as aromatic diamines containing -CN group. Method of manufacturing. 제1항에 있어서, 상기 중합용액 내에 무기염이 첨가되어 있는 것을 특징으로 하는 습식 아라미드 부직포의 제조방법.The method for producing a wet aramid nonwoven fabric according to claim 1, wherein an inorganic salt is added to the polymerization solution.
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