Method for the manufacture of a poly(imide) prepolymer powder and varnish, poly(imide) prepolymer powder and varnish prepared thereby, and poly(imide) prepared therefrom
A method for manufacturing a poly(imide) prepolymer powder includes combining a bisanhydride powder or organic diamine and a solvent comprising an alcohol, a water-soluble ketone or water to form a mixture, adding an organic diamine or bisanhydride powder to the mixture to form a poly(imide) prepolymer, and removing the solvent to provide the poly(imide) prepolymer powder. A method for manufacturing a poly(imide) prepolymer varnish includes combining a bisanhydride powder or organic diamine and a solvent comprising an alcohol, a water-soluble ketone or water to form a mixture, and adding an organic diamine or bisanhydride powder to the mixture to form a poly(imide) prepolymer. The method of manufacturing the varnish further includes at least one of adding an effective amount of a secondary or tertiary amine to solubilize the poly(imide) prepolymer powder, heating the mixture to a temperature effective to provide the varnish, or agitating the mixture to provide the varnish. The poly(imide) prepolymer powder and varnish can have a residual organic diamine content of less than or equal to 1000 ppm. A poly(imide) polymer prepared from the prepolymer powder or varnish is also disclosed.
1. A method for the manufacture of a poly(imide) prepolymer powder, the method comprising,
combining a bisanhydride powder or an organic diamine and a solvent comprising a C 1-6 alcohol, water soluble ketone, water, or a combination comprising at least one of the foregoing to form a mixture;
adding an organic diamine or a bisanhydride powder to the mixture under conditions effective to form a poly(imide) prepolymer, provided that when the bisanhydride powder is combined with the solvent, the organic diamine is added to the mixture to form the poly(imide) prepolymer, and when the organic diamine is combined with the solvent, the bisanhydride powder is added to the mixture to form the poly(imide) prepolymer; and
removing the solvent to provide the poly(imide) prepolymer powder;
wherein the poly(imide) prepolymer powder has a residual organic diamine content of less than or equal to 1000 ppm.
2. The method of claim 1 , further comprising
heating the mixture comprising the poly(imide) prepolymer to a temperature effective to provide a homogenous solution comprising dissolved poly(imide) prepolymer; and
subsequently removing the solvent to provide the poly(imide) prepolymer powder.
3. The method of claim 1 , wherein the solvent comprises acetone, methyl ethyl ketone, or a combination comprising at least one of the foregoing and water.
4. The method of claim 1 , wherein the C 1-6 alcohol comprises methanol, ethanol, n-propanol, isopropanol, or a combination comprising at least one of the foregoing.
5. The method of claim 1 , wherein
combining the bisanhydride powder or the organic diamine and the solvent is at a temperature of 5 to 30° C.;
adding the organic diamine or the bisanhydride powder is at a temperature of 5 to 30° C.; and
wherein a reaction time sufficient to provide the poly(imide) prepolymer is greater than 5 minutes.
6. The method of claim 1 , further comprising adding
an end-capping agent to the slurry;
a branching or crosslinking agent;
or both.
7. A poly(imide) prepolymer powder prepared by the method of claim 1 .
8. A poly(imide) prepolymer powder having a residual organic diamine content of less than or equal to 1000 ppm.
9. The poly(imide) prepolymer powder of claim 7 , wherein the poly(imide) prepolymer powder comprises less than 1 wt % of a halogenated solvent, N-methyl pyrrolidone, dimethylacetamide, N,N-dimethyl formamide, tetrahydrofuran, sulfolane, anisole, cyclohexanone, cyclopentanone, dimethylsulfoxide, or a combination comprising at least one of the foregoing.
10. A method of making a poly(imide), the method comprising heating the poly(imide) prepolymer powder of claim 7 to a temperature of greater than 150° C. to provide the poly(imide).