CHEN Jiansheng, ZUO Hongun, HE Guanjun, FAN Lin, YANG Shiyong. Synthesis and Characterization of 4-Phenylethynylphthalic Anhydride Terminated Oligoimides and Polyimides. [J]. Acta Polymerica Sinica (4):337-342(2008)
DOI:
CHEN Jiansheng, ZUO Hongun, HE Guanjun, FAN Lin, YANG Shiyong. Synthesis and Characterization of 4-Phenylethynylphthalic Anhydride Terminated Oligoimides and Polyimides. [J]. Acta Polymerica Sinica (4):337-342(2008) DOI: 10.3724/SP.J.1105.2008.00337.
Synthesis and Characterization of 4-Phenylethynylphthalic Anhydride Terminated Oligoimides and Polyimides
Thermosetting phenylethynyl terminated polyimides are well known for their super thermo-oxidative stability and excellent toughness
and have been widely used in aerospace area.PETI-5 (PhenylEthynyl Terminated Imide-5) developed by NASA is the-state-of-art of this type polyimides
while it is a semi-crystalline polyimide with melting temperature of 353℃ near the crosslinking temperature of phenylethynyl groups
which made it difficult for PETI-5 to fabricate complex shape parts.In the pursuit of novel phenylethynyl terminated polyimides with high melt processability
researchers have developed several polyimides by introduction of fluorine groups and twisty structures.In this paper
a series of oligoimides (PIO) with calculated molecular weight of 5000 were prepared using flexible dianhydride of 4
4′-oxydiphthalic anhydride (ODPA)
and mixtures of two diamines of 1
3-bis(4-aminophenoxy)benzene (1
3
4-APB) and 3
4′-oxydianiline (3
4′-ODA) in the presence of 4-phenylethynylphthalic anhydride (4-PEPA) as endcapping agent in order to enhance the processability.In addition
oligoimides (PIB) using 3
3′
4
4′-biphenyltetracarboxylic-dianhydride (s-BPDA) were also prepared for comparison.Effects of the kind of dianhydride and diamine on their properties and melt processabilities were systematically investigated.Experimental results indicated that PIO was amorphous in nature
and exhibited low melt viscosity and high melt viscosity stability at elevated temperatures
and with the increase of the content of 1
3
4-APB the melt viscosity decreased correspondingly.The PIB is semi-crystalline in nature and exhibited high melt viscosity at elevated temperatures
meanwhile
the melt temperature of PI-B was close to the cure temperature of phenylethynyl groups
which reduced the processability.The molecular weight-controlled oligoimides could be thermally cured at 371℃ to yield thermosetting polyimides by polymer chain extension and crosslinking of phenylethynyl groups.All cured resins showed good thermal stability with 5% weight loss temperature of500℃
and high glass transition temperatures of243℃.In addition
with the increase of the content of 1
3
4-APB
the glass transition temperatures of PIO cured resin decreased from 281 to 243℃.PIO-2 cured resin also exhibited good mechanical properties with tensile strength of 102 MPa
tensile modulus of 1.8 GPa
high break elongation of 10%
flexural strength of 142 MPa and flexural modulus of 3.1 GPa.