Preparation and properties of fibers produced from a cellulose/complex PA solvent system precipitating in diverse coagulants

Ethanol, as the first coagulation bath, and several common organic solvents, as well as aqueous solutions of NH₄Cl, NaHCO₃ and NaOH were explored and demonstrated to be adopted as the second coagulation bath for cellulose/phosphoric acid/tetraphosphoric acid (cellulose/complex PA solvent) solution to produce novel cellulose fibers by two-stage dry-wet spinning in a laboratory scale, and effect of coagulants, cellulose concentration, solvent concentration (P₂O₅ concentration) and coagulation temperature on crystal structure and properties of corresponding fibers were investigated. Surface morphology of regenerated fibers as-spun from different coagulants was observed by scanning electronic microscope (SEM), indicating that methanol and 8 wt% NaOH aqueous solution all rendered cellulose fibers relatively dense and smooth surface. X-ray diffraction (XRD) analysis showed that cellulose fiber precipitated from 8 wt% NaOH aqueous solution had pronounced characteristic peak of cellulose II than those of fibers precipitated from other coagulants, and highest crystallinity and orientation. Meanwhile, those two coagulants referred above also gave cellulose fibers relatively higher tensile strength under the same prerequisite. TGA curves exhibited that fibers were thermally stable produced from two salt aqueous solutions (8 wt% NH₄Cl and NaHCO₃) since they had the relatively higher onset decomposition temperatures. By evaluating the effect of cellulose concentration, P₂O₅ concentration and coagulation temperature on the structure and properties of asprepared fibers, it was preferable to produce cellulose fiber from a solution at 20 wt% cellulose concentration, 73 % P₂O₅ concentration, and coagulating in methanol at coagulation temperature of 60 °C at the second-stage.