# US 11,993,867 B2 · Spun ABPBI fibers and process for preparing the same > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 11,993,867 B2 - Document ID: US11993867B2 - Status: Granted - Kind: B2 - Application number: 17/274,935 - Filed: 2019-09-12 - Published: 2022-02-03 - Granted: 2024-05-28 - Earliest claimed: 2018-09-12 - Assignees: Gharda Chemicals Limited - Applicants: Gharda Chemicals Limited - Inventors: Prakash D. Trivedi; Mathew Abraham; Amit Kundu - Web page: https://patentgrep.com/patent/US11993867B2 ## CPC - D01F 6/74: from polycondensates of cyclic compounds, e.g. polyimides, polybenzimidazoles - C08G 73/18: Polybenzimidazoles - D01D 5/06: Wet spinning methods {(D01D5/0046 takes precedence)} - D01D 10/06: Washing or drying - D01F: CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS - C08G: MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS - D01D: MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS ## Abstract Spun ABPBI fibers and a process for the preparing spun ABPBI fibers using a high molecular weight ABPBI dope solution suitable for spinning are provided. A process for preparing the high molecular weight ABPBI dope solution suitable for spinning is also provided. The spun ABPBI fibers can be used in the preparation of high temperature thermally resistant articles. ## Claims ### Claim 1 Spun ABPBI fibers, wherein the spun ABPBI fibers have the following properties: a. filaments in the range of 1.5 denier 12.0 denier; b. tenacity in the range of 2.5 grams per denier to 4.0 grams per denier; c. break strength in the range of 4.0 gmf to 15 gmf; and d. elongation at break in the range of 15-25%. ### Claim 2 A process for preparing poly(2,5-benzimidazole) (ABPBI) suitable for spinning, said process comprising the following steps: i. polymerizing 3,4-diaminobenzoic acid (DABA) having purity >99.5% in Methane Sulfonic acid (MSA) at a temperature in the range of 150° C. to 200° C. at a pressure in the range of 0.5 to 10 mm Hg for a time period in the range of 3 hours to 6 hours under inert atmosphere to obtain a reaction mixture; and ii. adding P2O5 in the range of 0.05 to 0.3 moles per mole of DABA to said reaction mixture at a temperature in the range of 150° C. to 200° C. for a time period in the range of 3 hours to 6 hours under inert atmosphere to obtain ABPBI suitable for spinning. ### Claim 3 (depends on 2) The process as claimed in claim 2, wherein 70 to 90% water and MSA are removed through azeotropic distillation during polymerization in step i). ### Claim 4 (depends on 2) The process as claimed in claim 2, wherein the inherent viscosity of said ABPBI in concentrated sulfuric acid is >4 dl/g. ### Claim 5 (depends on 2) The process as claimed in claim 2, wherein an endcapping agent is optionally added in step ii). ### Claim 6 (depends on 5) The process as claimed in claim 5, wherein said endcapping agent is benzoic acid. ### Claim 7 (depends on 2) A process for preparing spun ABPBI fibers, said process comprising the following steps: (a) preparing a spinning solution comprising 2 to 10% by weight of ABPBI suitable for spinning as claimed in claim 2 and methane sulfonic acid in a bath having temperature in the range of 80° C. to 90° C.; (b) extruding said spinning solution through a plurality of extrusion orifices having a diameter in the range of 20 to 200 microns to form a plurality of fibers; (c) passing said filaments through a coagulation bath to obtain coagulated fibers; (d) drawing said coagulated fibers with an initial draw ratio in the range of 2:1 to 50:1 at a temperature in the range of 400° to 500° C. to obtain drawn fibers; and (e) washing said drawn fibers obtained in step d) to remove residual non-solvent, followed by drying to obtain ABPBI fibres. ### Claim 8 (depends on 7) The process as claimed in claim 7, wherein said fibers are drawn through a drawing zone at a heat draw ratio in the range of 1.5:1 to 10:1 to obtain filaments having a denier per filament in the range of 0.05 to 0.5 and a tenacity of at least 4 grams per denier. ### Claim 9 (depends on 8) The process as claimed in claim 8, wherein said heat draw ratio is in the range of 2:1 to 6:1, preferably in the range of 2:1 to 3:1. ### Claim 10 (depends on 7) The process as claimed in claim 7, wherein said extrusion orifices are situated at a distance in the range of 1 inch to 10 inches above said coagulation bath. ### Claim 11 (depends on 7) The process as claimed in claim 7, wherein in step (b) said spinning solution is extruded at a temperature in the range of 80° C. to 90° C. ### Claim 12 (depends on 7) The process as claimed in claim 7, wherein in step (b) said plurality of extrusion orifices are in the range of 30 to 90 microns. ### Claim 13 (depends on 7) The process as claimed in claim 7, wherein in step (c) said coagulation bath is maintained at a temperature in the range of 10° C. to 25° C., preferably in the range of 15° C. and 20° C. ### Claim 14 (depends on 7) The process as claimed in claim 7, wherein in step (d) the initial draw ratio is in the range of 1.5:1 to 10:1, preferably in the range of 2:1 to 5:1. ### Claim 15 (depends on 7) The process as claimed in claim 7, wherein in step (e) said fibers are washed with water at a temperature of in the range of 50° C. to 60° C. ### Claim 16 (depends on 7) The process as claimed in claim 7, wherein in step (e) said fibers are dried while passing through said drying zone at a temperature in the range of 400° C. to 450° C. ### Claim 17 (depends on 2) The process as claimed in claim 2, wherein the poly(2,5-benzimidazole) (ABPBI) suitable for spinning to obtain spun fibers, wherein the spun ABPBI fibers have the following properties: a. filaments in the range of 1.5 denier to 12.0 denier; b. tenacity in the range of 2.5 grams per denier to 4.0 grams per denier; c. break strength in the range of 4.0 gmf to 15 gmf; and d. elongation at break in the range of 15-25%.