KR930013263A - Process for spinning with a solution of polyamide-imide based on tolylene or meta-phenylene diisocyanate and fibers made thereof - Google Patents

Process for spinning with a solution of polyamide-imide based on tolylene or meta-phenylene diisocyanate and fibers made thereof Download PDF

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KR930013263A
KR930013263A KR1019920025530A KR920025530A KR930013263A KR 930013263 A KR930013263 A KR 930013263A KR 1019920025530 A KR1019920025530 A KR 1019920025530A KR 920025530 A KR920025530 A KR 920025530A KR 930013263 A KR930013263 A KR 930013263A
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chain
imide
chain order
rate
present
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KR100198184B1 (en
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미쇼 필립
뻬리에 마리-에브
뤼쏘 쟝
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롱 쁠랑 피브르
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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
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/74—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polycondensates of cyclic compounds, e.g. polyimides, polybenzimidazoles
    • 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
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/60—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides

Abstract

Process for obtaining PAI fibres by spinning PAI in solution and the fibres thus obtained. They are obtained by dry or wet spinning in dimethylalkyleneurea, followed by removal of the solvent and overdrawing at elevated temperature. The yarns and fibres obtained originate from PAI based on tolylene or meta-phenylene diisocyanate and on an aromatic acid anhydride and/or an aromatic dianhydride, and optionally on one or a number of diacidic compounds. They exhibit an excellent thermomechanical behaviour and allow access to very low filament counts.

Description

톨릴렌 또는 메타-페닐렌 디이소시아네이트 기재 폴리아미드-이미드의 용액으로 방사하는 방법 및 그 것으로 만든 섬유Process for spinning with a solution of polyamide-imide based on tolylene or meta-phenylene diisocyanate and fibers made therefrom

본 내용은 요부공개 건이므로 전문내용을 수록하지 않았음As this is a public information case, the full text was not included.

Claims (19)

열기계적 작용이 개선된 폴리아미드-이미드 기재 얀 및 섬유의 제조방법에 있어서, a)-디메틸알킬렌우레아중의 중합체의 용액을 방사시키고, 이 경우 상기 중합체는 -하기식의 아미드-이미드 사슬순서(A):In a process for producing polyamide-imide based yarns and fibers with improved thermomechanical action, a) a solution of a polymer in dimethylalkyleneurea is spun, in which case the polymer is an amide-imide of the formula Chain order (A): 를 함유하며, [상기식에서, Ar1은 톨릴렌 및/또는 메타-페닐렌 2가 방향족 라디칼을 나타내고, Ar3은 3가의 방향족 라디칼을 나타내며, Ar3은 4가의 방향족 라디칼을 나타내고, R은 2가의 방향족 라디칼을 나타내며, M은 알칼리 금속 또는 알칼 토금속이고, 30∼80중량%의 디메틸알킬렌우레아(DMAU) 및 20∼70중량%의 물을 함유하는 수성 응고 매질중에서, -사슬 순서 (A)는 0∼100%의 비율로 존재하고, -사슬 순서 (B)는 0∼5%의 비율로 존재하며, -사슬 순서(C)는 0∼100% 미만의 비율로 존재하고, -사슬 순서(D)는 0∼100% 미만의 비율, 바람직하게는 0~80%의 비율로 존재하며, 사슬순서 (A)+(B)+(C)+(D)의 합은 100%이다], b)- 얻어진 필라멘트를 적어도 2배의 연실율로 연산시키며, c) -어떤 공지방법으로 필라멘트에서 잔류 용매를 제거하고 필라멘트를건조시키며, d) -필라멘트를 적어도 250℃의 온도에서 적어도 2배의 연신율로 연신시켜 총연신율이 적어도 5배가 되도록 연신시킴을 특징으로 하는, 폴리아미드-이미드 기재 얀 및 섬유의 제조방법.Containing, and [wherein, Ar 1 is tolylene and / or a meta-phenylene divalent represents an aromatic radical, Ar 3 denotes a trivalent aromatic radical, Ar 3 denotes a tetravalent aromatic radical, R is 2 Represents an aromatic aromatic radical, M is an alkali metal or an alkaline earth metal, and in an aqueous coagulation medium containing 30 to 80% by weight of dimethylalkyleneurea (DMAU) and 20 to 70% by weight of water, the chain order (A) Is present at a rate of 0 to 100%,-chain order (B) is present at a rate of 0 to 5%,-chain order (C) is present at a rate of less than 0 to 100%, and-chain order ( D) is present in a proportion of less than 0-100%, preferably 0-80%, and the sum of the chain sequences (A) + (B) + (C) + (D) is 100%], b )-Calculate the filament obtained at least twice the rate of combustion; c)-remove any residual solvent from the filament and dry the filament by any known method; A process for producing polyamide-imide-based yarns and fibers, characterized in that stretching at a temperature of at least 250 ° C. is at least doubled so that the total elongation is at least 5 times. 제1항에 있어서, 용매가 세척함으로써 제거됨을 특징으로 하는 방법.The method of claim 1 wherein the solvent is removed by washing. 제1항에 있어서, 응고 욕(bath)의 용매 50∼65%를 함유함을 특징으로 하는 방법.A process according to claim 1 which contains 50 to 65% of the solvent of the coagulation bath. 제1항에 있어서, 총 연신이 6배가 되도록 과연신을 적어도 3배로 수행함을 특징으로 하는 방법.The method of claim 1, wherein overextension is performed at least three times such that total stretching is six times. 제1항에 있어서, 과연신을 촉매의 부재하에 적어도 300℃의 온돌 수행함을 특징으로 하는 방법.The process according to claim 1, wherein the overdrawing is carried out at least 300 DEG C in the absence of a catalyst. 열기계적 작용을 개선한 폴리아미드 이미드 기재 얀 및 섬유의 제조방법에 있어서, a)-디메틸알킬렌우레아중의 중합체의 용액을 용매의 비점에 가까운 온도나 그 보다 높은 온도로 유지되는 증발 대기로 방사하고, 여기서, 상기 중합체는 -하기식의 아미드-이미드 사슬순서(A):In the method for producing polyamide-imide-based yarns and fibers with improved thermomechanical action, a solution of the polymer in a) -dimethylalkyleneurea is subjected to an evaporating atmosphere maintained at or near the boiling point of the solvent. Spinning, wherein the polymer is an amide-imide chain sequence of formula 를 함유하며, [상기식에서, Ar1은 톨릴렌 또는 메타-페닐렌 2가 방향족 라디칼을 나타내고, Ar2은 3가의 방향족 라디칼을 나타내며, Ar3은 4가의 방향족 라디칼을 나타내고, R은 2가의 방향족 라디칼을 나타내며, M은 알칼리 금속 또는 알칼리 토금속을 나타내며, -사슬 순서 (A)는 20∼100%의 비율로 존재하고, -사슬 순서 (B)는 0∼5%의 비율로 존재하며, -사슬 순서 (C)는 0∼100% 미만의 비율로 존재하고, - 사슬 순서 (D)는 0∼100% 미만의 비율, 바람직하게는 0∼80%의 비율로 존재하며, 사슬순서 (A)+(B)+(C)+(D)의 합은 100%이다], b)필라멘트에서 잔류용매를 제거한 다음, c)총연신율이 적어도 5배가 되도록 250℃이상의 농돌 연신시킴을 특징으로 하는, 폴리아미드-이미드 기재 얀 및 섬유의 제조방법.Wherein, Ar 1 represents a tolylene or meta-phenylene divalent aromatic radical, Ar 2 represents a trivalent aromatic radical, Ar 3 represents a tetravalent aromatic radical, and R is a divalent aromatic. Represents a radical, M represents an alkali metal or an alkaline earth metal,-chain order (A) is present at a rate of 20 to 100%,-chain order (B) is present at a rate of 0 to 5%, and-chain Sequence (C) is present at a rate of less than 0-100%, chain order (D) is present at a rate of less than 0-100%, preferably at a rate of 0-80%, and chain order (A) + The sum of (B) + (C) + (D) is 100%], b) removal of residual solvent from the filaments, and c) concentrated draw stretching above 250 ° C. so that the total elongation is at least 5 times. Method for preparing amide-imide based yarns and fibers. 제6항에 있어서, 잔류 용매가 160℃ 이상의 온도로 열처리함으로써 필라멘트로부터 제거됨을 특징으로 하는 방법.7. The method of claim 6, wherein the residual solvent is removed from the filament by heat treatment at a temperature of at least 160 ° C. 제6항에 있어서, 잔류용매가 통상의 방법으로 가압하에 끓는 물로 세척하고 건조됨으로써 필라멘트로 부터 제거됨을 특징으로 하는 방법.7. A method according to claim 6, wherein the residual solvent is removed from the filament by washing with boiling water and drying under pressure in a conventional manner. 제6항에 있어서, 잔류 용매가 통상의 방법으로 가압하에 끓는 물로 세척하고 건조됨으로써 필라멘트로 부터 제거됨을 특징으로 하는 방법.7. A process according to claim 6, wherein the residual solvent is removed from the filament by washing with boiling water and drying under pressure in a conventional manner. 제1항 내지 제6항중 어느 한 항에 있어서, 폴리아미드-이미드의 고유점도가 0.8dl/g이상, 바람직하게는 0.9dl/g 이상임을 특징으로 하는 방법.The process according to any one of the preceding claims, characterized in that the intrinsic viscosity of the polyamide-imide is at least 0.8 dl / g, preferably at least 0.9 dl / g. 하기식의 아미드-이미드 사슬순서(A):Amide-imide chain sequence of the following formula (A): -하기식의 아미드 사슬 순서(B) :-Amide chain sequence of formula (B): -하기식의 아미드 사슬순서(C) :-Amide chain sequence of the following formula (C): -하기식의 이미드 사슬 순서(D)-Imide chain sequence of the following formula (D) 를 함유하고, 310℃에서 적어도 40%의 탄성율을 보존하고 있음을 특징으로 하는 열적으로 안정한 폴리아미드-이미드 기재 얀 및 섬유.[상기식에서, Ar1은 톨릴렌 및/또는 메타-페닐렌 2가 방향족 라디칼을 나타내고, Ar2는 3가의 방향족 라디칼을 나타내며, Ar3은 4가의 방향족 라디칼을 나타내고, R은 2가의 방향족 라디칼을 나타내며, M은 알칼리 금속 또는 알칼리 토금속을 나타내며, - 사슬 순서(A)는 20∼100%의 비유롤 존재하고, -사슬순서 (B)는 0∼5%의 비율로 존재하고, -사슬순서 (C)는 0∼100% 미만의 비율로 존재하며, - 사슬순서 (D)는 0∼100% 미만의 비율이며, 사슬순서 (A)+(B)+(C)+(D)의 합은 100% 이다]And a thermally stable polyamide-imide-based yarn and fiber, characterized in that it preserves at least 40% modulus at 310 ° C. wherein Ar 1 is tolylene and / or meta-phenylene 2 Represents an aromatic radical, Ar 2 represents a trivalent aromatic radical, Ar 3 represents a tetravalent aromatic radical, R represents a divalent aromatic radical, M represents an alkali metal or alkaline earth metal, and-a chain order (A ) Is present in a proportion of 20 to 100%,-chain order (B) is present at a rate of 0 to 5%,-chain order (C) is present at a rate of less than 0 to 100%, and-chain order (D) is less than 0 to 100%, and the chain order (A) + (B) + (C) + (D) is 100%]. 제11항에 있어서, 폴리다미드-이미드는 0.8dl/g 이상의 고유점도, 바람직하게는 039dl/g 이상의 고유점도를 가짐을 특징으로 하는 방법.12. The method according to claim 11, wherein the polyamide-imide has an intrinsic viscosity of at least 0.8 dl / g, preferably at least 039 dl / g. 제11항에 있어서, 사슬순서(A)는 50∼100%의 비율, 사슬 순서(B)는 0∼3%의 비율, 사슬순서(C)는 0∼50%의 비율, 사슬순서 (D)는 0~80%의 비율로 존재함을 특징으로 하는 얀 및 섬유.The chain order (A) is 50 to 100%, the chain order (B) is 0 to 3%, the chain order (C) is 0 to 50%, and the chain order (D). Yarns and fibers characterized in that they are present in a proportion of 0-80%. 제11항에 있어서, Ar2는 하기식의 라디칼임을 특징으로 하는 얀 및 섬유:12. Yarn and fiber according to claim 11, wherein Ar 2 is a radical of the formula: 제11항에 있어서, R은 하기식의 라디칼임을 특징으로 하는 얀 및 섬유:12. Yarn and fiber according to claim 11, wherein R is a radical of the formula: 제11항에 있어서, M이 알칼리 금속임을 특징으로 하는 얀 및 섬유.The yarn and fiber of claim 11 wherein M is an alkali metal. 제11항에 있어서, 탄성율이 적어도 50%로 보존됨을 특징으로 하는 얀 및 섬유.The yarn and fiber of claim 11 wherein the modulus of elasticity is preserved at least 50%. 제11항에 있어서, 얀 및 섬유가 1dtex 이하의 선밀도를 가짐을 특징으로 하는 얀 및 섬유.The yarn and fiber of claim 11 wherein the yarn and fiber have a linear density of 1 dtex or less. 제11항에 기재된 얀 및 섬유를 포함하는 열적으로 안정한 물품.A thermally stable article comprising the yarns and fibers of claim 11. ※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.※ Note: The disclosure is based on the initial application.
KR1019920025530A 1991-12-24 1992-12-24 Process for spinning solutions of polyamide-imides based on metaphenylene diisocyanate and fibres made thereof KR100198184B1 (en)

Applications Claiming Priority (2)

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FR9116339 1991-12-24
FR9116339A FR2685354B1 (en) 1991-12-24 1991-12-24 PROCESS FOR SPINNING POLYAMIDE-IMIDE (PAI) SOLUTIONS BASED ON TOLUYLENE OR METAPHENYLENE DIISOCYANATES AND FIBERS THUS OBTAINED.

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KR930013263A true KR930013263A (en) 1993-07-21
KR100198184B1 KR100198184B1 (en) 1999-06-15

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MXPA03008714A (en) 2002-09-26 2004-09-10 Oreal Sequenced polymers and cosmetic compositions comprising the same.
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JP2607816B2 (en) 1997-05-07
JPH06200413A (en) 1994-07-19
ATE164640T1 (en) 1998-04-15
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ES2113934T3 (en) 1998-05-16
FR2685354B1 (en) 1996-03-29
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EP0549494A1 (en) 1993-06-30
TW218898B (en) 1994-01-11
CN1077760A (en) 1993-10-27
JP2726812B2 (en) 1998-03-11
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MX9207511A (en) 1994-05-31

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