Thermoplastic (CO)polyimides and synthesis methods
a technology of thermoplastics and polyimides, applied in the field of aromatic polyimides, can solve the problems of significant decomposition of polyimide matrix, coloration harmful to the production of “attractive” parts, and high processing temperatures to allow conversion by conventional processes for processing thermoplastics
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example 2
Preparation of Polyimide PI MPMDPMA From a Tetraacid at 300° C.
[0203]The salt of example 1 is heated at 10° C. / min up to 300° C. while flushing with nitrogen and is then immediately cooled to ambient temperature.[0204]The thermal properties of the polyimide formed are measured: M.p.=322° C. (enthalpy of fusion ΔHf=38 J / g) and Tc=236° C. The M.p. and Tc temperatures turn out to be lower than those measured on the polyimide prepared according to example 1. It is thus preferable to carry out the polymerization at a temperature lower than the melting point of the salt.
example 3
Preparation of Polyimide PI MPMDPMA From a Diester Diacid at 200° C.
[0205]A pyromellitic anhydride diester-diacid derivative is prepared from the reaction of the pyromellitic anhydride with ethanol. 15 g (0.069 mol) of 99.7% pyromellitic anhydride (RN CAS: 89-32-7) supplied by Lonza are introduced into a round-bottom flask containing 300 ml of anhydrous absolute ethanol (5.14 mol). The reaction medium is brought to reflux for 3 hours. The ethanol opens the anhydride functional groups and produces a pyromellitic anhydride diester-diacid derivative. The product is recovered by evaporation of the excess ethanol in a rotary evaporator. A white powder is obtained. The chemical structure of the diester-diacid derived from pyromellitic anhydride is confirmed by NMR analysis in deuterated DMSO.
[0206]A salt of MPMD and of the diester-diacid derived from pyromellitic anhydride is prepared by addition of a solution containing 5 ml of absolute ethanol and 0.272 g (2.34 mmol) of 99% 2-methylpent...
example 4
Preparation of Polyimide PI MPMDPMA From a Dianhydride in Solution
[0210]1.45 g (6.6 mmol) of 99% pyromellitic anhydride and 20 ml of 1,3-dimethyl-2-imidazolidinone (RN CAS: 80-73-9), as polar aprotic solvent, are introduced into a 50 ml two-necked round-bottom flask equipped with a reflux condenser and with a dropping funnel. The reaction medium is stirred at ambient temperature and then 0.774 g (6.6 mmol) of 99% 2-methylpentane-1,5-diamine (MPMD) is added via the dropping funnel. The reaction medium is subsequently brought to 140° C. and is maintained at 140° C. for 1 hour. After cooling, the solution of polyamic acid formed is precipitated from 100 ml of ethanol. The precipitate (orange-colored solid) is recovered by filtration and then brought to 200° C. for 30 min. The polymer obtained is orange-yellow in color and exhibits the following thermal properties: M.p.=339° C., Tc=301° C., Tg=191° C.
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