M5 is a new high-performance fiber produced by Akzo-Nobel laboratories. M5 is a rigid-rod polymer called PIPD or poly{2,6-diimidazo[4,5-β:4`,5`-ε]pyridinylene-1,4-(2,5-dihydroxy)phenylene}. M5 fiber is prepared through condensation polymerization of tetraaminopyridine and dihydroxyterephthalic acid using diphosphorus pentoxide. The polymer mixture is then heated and extruded to form brightly blue M5 fibers, which are washed to remove residual chemicals.
5. • As a result of research in Akzo-Nobel
laboratories a new high-performance fibre,
known as ‘M5’, has been produced.
6. • The polymer is poly{2,6-diimidazo[4,5-β:4`,5`-ε]pyridinylene-
1,4-(2,5-dihydroxy)phenylene} or PIPD
7. • Two methods have proved effective in preparing
high modulus, high tenacity (HM-HT) polymer
fibres:
(a) perfecting the drawing technique of precursor
fibres to attain draw ratios far above ten, as in the
well-known polyethylene Dyneema and Spectra
yarns.
(b) manipulating rigid rod-like molecules into fibres
that are already very highly oriented in the as-spun
state, as in PPTA fibres.
8. polymerization
• M5 fiber is prepared by condensation polymerization
between tetraaminopyridine and dihydroxyterephtha
lic acid using diphosphorus pentoxide as a
dehydrating agent.
9.
10. • A much greater step forward was achieved by
the synthesis of the TAP-DHTA 1 : 1 complex,
or TD salt.
• it precipitates in a high yield from the
combination of aqueous solutions of TAP HCl
salt and DHTA Na or K salt.
11. • A fast polymerisation cycle (typically 4–5 h,
rather than >24 h according to Ref. 24) now
yields high MW polymer much more
consistently than in the case where amine and
acid components are weighed separately:
12. • The polymerization of homopolymer consists
of taking TD salt, polyphosphoric acid and
P2O5 with a trace of tin powder into the
reactor, displacing air by nitrogen and raising
the reaction temperature to 140 °C.
• Mixing for at least 1.5 h at that temperature
before taking the mixture to 180 °C and
stirring for another 1–2 h yields the spinning
solution.
13. • The solution becomes liquid crystalline about
1 h after it reaches 140 °C.
14. • The P2O5 content of the solvent system
controls the final molecular weight, and
obviously only the highest purity TD salt will
deliver the highest MW polymers.
15. • The polymer mixture is then heated and
extruded to form brightly blue polymer fibers.
The fibers are then washed extensively with
water and base in order to remove
the phosphoric acid generated by the
hydration of diphosphorus pentoxide from the
polymer.
