Purification of acetylene-terminated polyimide oligomers
AssigneeThe United States of America as represented by the Secretary of the Air Force
InventorsMichael A. Lucarelli, Lewellyn G. Picklesimer
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Abstract
A process for purifying an acetylene-terminated polyimide oligomer containing residual solvent in which the oligomer is initially dissolved in the same solvent used as the reaction medium in its synthesis. After precipitating the oligomer from solution by mixing with an aqueous solution of potassium or sodium chloride, the precipitated oligomer is washed successively with a plurality of liquids of decreasing polarity to provide an oligomer free of residual solvent.
Claims4
A process for purifying an acetylene-terminated polyimide oligomer containing a residual amount of the solvent used as the reaction medium in its synthesis which comprises the steps of:
- (a) dissolving the oligomer in the same solvent used as the reaction medium in its synthesis;
- (b) mixing the resulting solution with an aqueous solution of potassium or sodium chloride, thereby causing the oligomer to precipitate from solution;
- (c) separating the precipitated oligomer from the aqueous solution;
- (d) successively washing the separated oligomer at least once in each of a series of five liquid baths of decreasing polarity, the first of said baths consisting essentially of water, the second of said baths consisting essentially of a mixture of methanol and water, the third of said baths consisting essentially of methanol, the fourth of said baths consisting essentially of a mixture of ether and methanol, and the fifth of said baths consisting essentially of ether;
- and
- (e) recovering and drying the purified oligomer from the said fifth bath.
A process for purifying an acetylene-terminated polyimide oligomer containing a residual amount of 1-methyl-3-pyrrolidinone, said oligomer having the following structural formula:
- ##STR2## wherein n is 1 or 2, said process comprising the steps of:
- (a) dissolving the oligomer in 1-methyl-2-pyrrolidinone;
- (b) mixing the resulting solution with an aqueous solution containing about 4 to 10 weight percent potassium or sodium chloride, thereby causing the oligomer to precipitate from solution;
- (c) separating the precipitated oligomer from the aqueous solution;
- (d) successively washing the precipitated oligomer at least once in each of a series of five liquid baths, said baths consisting essentially of (1) water, (2) a mixture of methanol and water, (3) methanol, (4) a mixture of ether and methanol, and (5) ether;
- and
- (e) recovering and drying the purified polymers from the last bath.
Dependencies are inferred from the claim text.