GB1188936A - Obtaining Filaments from Polyamide Acid Salts - Google Patents

Obtaining Filaments from Polyamide Acid Salts

Info

Publication number
GB1188936A
GB1188936A GB39805/66A GB3980566A GB1188936A GB 1188936 A GB1188936 A GB 1188936A GB 39805/66 A GB39805/66 A GB 39805/66A GB 3980566 A GB3980566 A GB 3980566A GB 1188936 A GB1188936 A GB 1188936A
Authority
GB
United Kingdom
Prior art keywords
acid
salt
polyamide
solution
filaments
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
GB39805/66A
Inventor
Alan Buckley
John David Seddon
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Imperial Chemical Industries Ltd
Original Assignee
Imperial Chemical Industries Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Imperial Chemical Industries Ltd filed Critical Imperial Chemical Industries Ltd
Priority to GB39805/66A priority Critical patent/GB1188936A/en
Priority to US661537A priority patent/US3529051A/en
Priority to DE19671669465 priority patent/DE1669465A1/en
Priority to LU54424D priority patent/LU54424A1/xx
Priority to BE703539D priority patent/BE703539A/xx
Publication of GB1188936A publication Critical patent/GB1188936A/en
Expired legal-status Critical Current

Links

Classifications

    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/60Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/74Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polycondensates of cyclic compounds, e.g. polyimides, polybenzimidazoles

Abstract

1,188,936. Producing filaments of polyamide acids or salts thereof. IMPERIAL CHEMICAL INDUSTRIES Ltd. 16 Aug., 1967 [6 Sept., 1966], No. 39805/66. Addition to 1,121,325. Heading B5B. Filaments of polyamide acids or salts thereof suitable for conversion into polyimide filaments are produced by spinning an aqueous solution of an organic base salt of a polyamide acid as claimed in the parent Specification (wherein there is claimed an aqueous solution of a salt of a polyamide acid with a salt-forming organic base present in at least the stoichiometric amount required to neutralize all the free carboxylic acid groups in the polyamide acid) into an aqueous or a water-miscible coagulant bath which chemically interacts with the organic base salt to regenerate the polyamide acid or otherwise convert the salt into an insoluble form and withdrawing from the coagulant bath a coherent filament. The spinning solution may be a solution of a trialkylamine salt of the polyamide derived from pyromellitic dianhydride and a diamine of the general formula wherein X is a divalent bridging group or a divalent atom such as O or S and the phenyl groups are further substituted or are unsubstituted. The coagulant bath may be an acid solution and the spun salt may be converted into the free polyamide acid. The filaments produced may be subjected to thermal imidization under a tension not exceeding 0À5 gm./ denier, preferably less than 0À2 gram denier, the filament thereafter optionally being hot drawn. Conversion techniques and methods of processing filaments of polyimide precursors are described in Specification 1,038,738. The solutes in the coagulation bath may be hydrochloric acid, trichloracetic acid, calcium hydroxide, calcium chloride, ferric chloride, silver nitrate or metal chelates. The solvents for the solutes may be lower molecular weight monohydric alcohols, e.g. methanol, and lower molecular weight esters, e.g. ethyl acetate. The preferred coagulant bath is an aqueous methanolic solution of hydrochloric acid. Preferred amongst organic bases are trialkylamines, especially triethyl- and trimethylamine. In an example, an 80 gm. /litre solution of the triethylamine salt of the polyamide acid derived from 4,4<SP>1</SP>-diaminodiphenyl ether and pyromellitic acid dianhydride in equal volumes of water and isopropanol is extruded into a 3À5% V./V. solution of concentrated hydrochloric acid in water maintained at 10‹ C. Draw-down in the coagulant bath is between 1À3 and 2À0 x. The as-spun filament, after washing with aqueous methanol to remove residual coagulant, is dried in air at 100‹ C. and then heated at 300‹ C. in the absence of imposed tension to convert the polyamide acid into the polyimide. The polyimide filament is drawn at a draw ratio of 1À5 over a curved heated plate held at 550‹ C.
GB39805/66A 1966-09-06 1966-09-06 Obtaining Filaments from Polyamide Acid Salts Expired GB1188936A (en)

Priority Applications (5)

Application Number Priority Date Filing Date Title
GB39805/66A GB1188936A (en) 1966-09-06 1966-09-06 Obtaining Filaments from Polyamide Acid Salts
US661537A US3529051A (en) 1966-09-06 1967-08-18 Obtaining filaments from polyamide acid salts
DE19671669465 DE1669465A1 (en) 1966-09-06 1967-08-29 Process for the production of threads from polyamide acids or salts
LU54424D LU54424A1 (en) 1966-09-06 1967-09-05
BE703539D BE703539A (en) 1966-09-06 1967-09-06

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
GB39805/66A GB1188936A (en) 1966-09-06 1966-09-06 Obtaining Filaments from Polyamide Acid Salts

Publications (1)

Publication Number Publication Date
GB1188936A true GB1188936A (en) 1970-04-22

Family

ID=10411602

Family Applications (1)

Application Number Title Priority Date Filing Date
GB39805/66A Expired GB1188936A (en) 1966-09-06 1966-09-06 Obtaining Filaments from Polyamide Acid Salts

Country Status (5)

Country Link
US (1) US3529051A (en)
BE (1) BE703539A (en)
DE (1) DE1669465A1 (en)
GB (1) GB1188936A (en)
LU (1) LU54424A1 (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2829811A1 (en) * 1978-07-06 1980-01-24 Inst Vysokomolekuljarnych Soed Polyimide fibre mfr. by spinning polyamide acid soln. - in aprotic solvent into alcohol or pptn. bath
DE3223075A1 (en) * 1981-06-22 1983-01-13 Ube Industries, Ltd., Ube, Yamaguchi METHOD FOR PRODUCING A POLYIMIDE SEPARATING MEMBRANE
AT395188B (en) * 1989-04-13 1992-10-12 Chemiefaser Lenzing Ag Process for the production of low-flammability, high- temperature-resistant, paper-like materials based on polyimide fibres

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3985934A (en) * 1974-07-26 1976-10-12 The Upjohn Company Polyimide fiber having a serrated surface and a process of producing same
US4056598A (en) * 1974-12-11 1977-11-01 United Technologies Corporation Process for forming filaments from polyamic acid
US4576857A (en) * 1983-03-14 1986-03-18 E. I. Du Pont De Nemours And Company Melt-fusible polyimides
CN113355772B (en) * 2021-06-10 2023-07-04 东华大学 Polyimide aerogel fiber and preparation method and application thereof

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3441640A (en) * 1964-12-07 1969-04-29 Celanese Corp Process for wet-spinning polybenzimidazoles
US3448068A (en) * 1966-05-05 1969-06-03 Gen Electric Polymer solutions and methods for preparing and using the same
US3440196A (en) * 1966-05-05 1969-04-22 Gen Electric Coating solutions and methods for preparing and using the same
US3440197A (en) * 1966-05-05 1969-04-22 Gen Electric Coating solutions and methods for preparing and using the same
US3453236A (en) * 1967-01-18 1969-07-01 Ashland Oil Inc Aromatic polyimideamides prepared from aromatic tetracarboxylic acid dianhydrides and aminoaromatic hydrazides

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2829811A1 (en) * 1978-07-06 1980-01-24 Inst Vysokomolekuljarnych Soed Polyimide fibre mfr. by spinning polyamide acid soln. - in aprotic solvent into alcohol or pptn. bath
DE3223075A1 (en) * 1981-06-22 1983-01-13 Ube Industries, Ltd., Ube, Yamaguchi METHOD FOR PRODUCING A POLYIMIDE SEPARATING MEMBRANE
AT395188B (en) * 1989-04-13 1992-10-12 Chemiefaser Lenzing Ag Process for the production of low-flammability, high- temperature-resistant, paper-like materials based on polyimide fibres

Also Published As

Publication number Publication date
DE1669465A1 (en) 1971-05-06
LU54424A1 (en) 1967-11-06
US3529051A (en) 1970-09-15
BE703539A (en) 1968-03-06

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Legal Events

Date Code Title Description
PS Patent sealed [section 19, patents act 1949]
PLNP Patent lapsed through nonpayment of renewal fees