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 technology of polyimide and prepolymer powder, which is applied in the field of manufacturing of polyimide prepolymer powder and varnish prepared thereby, and polyimide powder and varnish prepared therefrom. it can solve the problems of adding removal and recycling costs, void production of coated articles, and residual solvents
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example 1
e) Prepolymer Powder Formation Using Methanol as Dispersion Medium
[0071]Poly(imide) prepolymer powder was formed from the reaction of a dianhydride and a diamine as a slurry in an alcohol solvent. Bisphenol A Dianhydride (BPA-DA) was ground using a lab grinder to form particles having a maximum diameter of less than or equal to 300 micrometers. In a three neck glass reactor equipped with an agitator, a nitrogen inlet, and a cold water-circulating reflux condenser, the ground BPA-DA powder (800 grams, 1.537 moles) and methanol (1600 grams) were added to form a slurry. The slurry was stirred under nitrogen atmosphere at 23° C. for ten minutes. To the slurry, an equimolar amount of para-phenylene diamine (PPD) powder (166.2 grams, 1.537 moles) was added slowly to the BPA-DA slurry with continuous agitation under nitrogen. The slurry was further stirred under nitrogen atmosphere at 23° C. for 5 hours. During the course of the reaction, a small amount of the slurry (2 gram portions) was ...
examples 2-6
Formation From Prepolymer Powder
[0075]Example 1E poly(imide) prepolymer powder (2 grams) was transferred to a PTFE-coated aluminum tube. The contents were heated to 385° C. under constant purging with nitrogen for 15 minutes. The resulting poly(imide) polymer block was made into a thin film by heating at 380° C. under pressure (1400 psi, 9.65 MPa). The molecular weight of the resulting polymer film (shown as Example 1F in Table 3 below) was determined using gel permeation chromatography (GPC). For molecular weight analysis by GPC, the poly(imide) (0.015 grams) was dissolved in 10 milliliters of a solvent mixture of methylene chloride and hexafluoroisopropyl alcohol (70:30 v / v). A 10 microliter sample of the polymer solution was analyzed by GPC. The molecular weight of the poly(imide) was determined relative to polystyrene standards.
[0076]As shown in Table 3, high molecular weight poly(imide) (e.g., weight average molecular weight of greater than 55,000 grams per mole) can be formed ...
example 7
on of Poly(imide) Prepolymer Solution with Tertiary Amine from a Prepolymer Slurry
[0079]BPA-DA powder (170 grams; 0.3266 moles) and methanol (250 grams) were taken in a three neck 2 liter glass reactor equipped with a stirrer, nitrogen inlet, and a cold water circulating refluxing condenser to form a slurry. The slurry was stirred under a nitrogen atmosphere at 23° C. To the slurry, PPD powder (35.3069 grams; 0.3265 moles) was added slowly. The mixture was stirred for 3 hours under nitrogen atmosphere at 50° C. During the course of the reaction, 0.3 grams of the slurry was removed periodically and dried in a vacuum oven at 80° C. to remove the solvent. The resulting dried prepolymer powder was evaluated for residual monomers using the HPLC method, as described above. After 3 hours of reaction, low levels of PPD residual monomer (<10 ppm) were noted, indicating completion of the reaction.
[0080]Triethylamine (47.5 grams, 0.4694 moles) was added to the reactor and continued agitation a...
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