Method for preparing fine spherical polycarbonate powders and method for preparing high molecular weight polycarbonate resin using same
Provided are a method for preparing fine round powdery polycarbonate and a method for preparing a high molecular weight polycarbonate resin using the same. More specifically, provided are a method for preparing fine round powdery polycarbonate, comprising (A) polymerizing non-phosgene polycarbonate, (B) extruding the polycarbonate into fine round powdery amorphous polycarbonate, (C) surface-crystallizing the fine round powdery amorphous polycarbonate in the presence of a solvent or dispersion medium, and (D) drying the surface-crystallized fine round powdery polycarbonate, and a method for preparing high molecular weight polycarbonate resin capable of obtaining polycarbonates with various molecular weights ranging from low molecular weights to high molecular weights by continuously using the obtained fine round powdery polycarbonate via a solid state polymerization step. In accordance with the methods, it is possible to remarkably simplify crystallization of amorphous polycarbonate and thus to realize process continuousness and economical efficiency enabling commercial mass-production, and to overcome production of high molecular weight polycarbonate, the most serious problem of conventional non-phosgene melt polymerization processes.
1. A method for preparing a high molecular weight polycarbonate resin using fine round powdery polycarbonate, comprising:
(A) supplying an aromatic dihydroxy compound and diarylcarbonate to stirred polymerization apparatus and melt-polymerizing an aromatic dihydroxy compound and diarylcarbonate into amorphous polycarbonate or a prepolymer thereof with a weight-average molecular weight of 20,000 g/mol or less;
(B) extruding the melted amorphous polycarbonate or a prepolymer thereof into a fine round powdery amorphous polycarbonate or a prepolymer thereof without performing a separate grinding process, by an extruder with a cutter and an extrusion die having microscopic holes with a size of 100 to 900 microns;
(C) surface-crystallizing the extruded fine round powdery amorphous polycarbonate or prepolymer thereof in the presence of a solvent or dispersion medium which directly contacts the extruded fine round powdery amorphous polycarbonate or prepolymer thereof after said extruding, wherein a non-solvent is used as the dispersion medium for maintaining the extruded fine round powdery amorphous polycarbonate or prepolymer thereof in a fine round powder shape;
(D) drying the fine round powdery polycarbonate or prepolymer thereof and maintaining the fine round powder shape, wherein the dispersion medium is separated from the fine round powdery polycarbonate or prepolymer thereof, returned to a micro extrusion die line, and then reused;
(E) conveying the dried fine round powdery polycarbonate or prepolymer thereof to a solid state polymerization apparatus; and
(F) performing a solid state polymerization to continuously separate and discharge the conveyed fine round powdery polycarbonate or the prepolymer thereof, using a solid state polymerization apparatus, based on the molecular weight thereof,
wherein the steps (A) to (F) are performed via a continuous single process.
2. The method according to claim 1 , wherein in the solid state polymerization, phenol is removed from the fine round powdery polycarbonate or a prepolymer thereof under an inert gas atmosphere or vacuum at a temperature of 150 to 230° C. to increase the degree of polymerization.
3. The method according to claim 1 , wherein the solid state polymerization apparatus is a vertical, horizontal or diagonal solid state polymerization apparatus.
4. The method according to claim 3 , wherein the solid state polymerization apparatus is provided with one to three polycarbonate resin discharge lines.
5. The method according to claim 1 , wherein the amorphous polycarbonate or prepolymer thereof is prepared by a non-phosgene polymerization process.
6. The method according to claim 1 , wherein step (B) is carried out using one selected from a group consisting of a single-screw extruder, a twin-screw extruder, a multi-screw extruder and a banbury type extruder.
7. The method according to claim 1 , wherein the step (C) is carried out at a temperature of 50 to 200° C.
8. The method according to claim 1 , wherein the fine round powdery polycarbonate or a prepolymer thereof surface-crystallized in step (C) has a crystallinity of 10 to 50%.
9. The method according to claim 1 , wherein step (D) is carried out by separating the surface-crystallized find round powdery polycarbonate or prepolymer thereof from the solvent or dispersion medium using a centrifugal separator, and vacuum-drying, dehumidification-drying or hot-air drying.
10. The method according to claim 1 , wherein the fine round powdery polycarbonate or prepolymer thereof dried in step (D) has a water content less than 0.1%.