Method of crystallizing low-molecular polycarbonate and process for producing polycarbonate resin from the same
A polycarbonate, low-molecular-weight technology for the production of high-molecular-weight polycarbonates with excellent color tone with less gel content
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Embodiment 1
[0112]228 parts by weight of 2,2-bis(hydroxyphenyl)propane, 223 parts by weight of diphenyl carbonate, 0.009 parts by weight of tetramethyl Ammonium hydroxide and 0.00014 parts by weight of bisphenol A disodium salt were dissolved by stirring the mixture at 180° C. for 30 minutes under nitrogen. Subsequently, the pressure was gradually lowered while the temperature was raised, and they were reacted while the phenol produced was distilled off until the final state of 220° C. and 30 mmHg was reached. The low molecular weight polycarbonate (oligomer) obtained at this time had an intrinsic viscosity [η] of 0.015 and a glass transition temperature (Tg) of 116°C. Reference Example 2: Synthesis Example of Crystallized Aromatic Polycarbonate
Embodiment 2
[0112]228 parts by weight of 2,2-bis(hydroxyphenyl)propane, 223 parts by weight of diphenyl carbonate, 0.009 parts by weight of tetramethyl Ammonium hydroxide and 0.00014 parts by weight of bisphenol A disodium salt were dissolved by stirring the mixture at 180° C. for 30 minutes under nitrogen. Subsequently, the pressure was gradually lowered while the temperature was raised, and they were reacted while the phenol produced was distilled off until the final state of 220° C. and 30 mmHg was reached. The low molecular weight polycarbonate (oligomer) obtained at this time had an intrinsic viscosity [η] of 0.015 and a glass transition temperature (Tg) of 116°C. Reference Example 2: Synthesis Example of Crystallized Aromatic Polycarbonate
[0113] A part of the low-molecular-weight polycarbonate (oligomer) obtained in the above-mentioned Reference Example 1 was taken out and subjected to heat treatment at 180° C. for 4 hours in a nitrogen atmosphere. During the 1 hour heat treatm...
Embodiment 3
[0119] By using a twin-screw extruder, 475 parts by weight of the low-molecular-weight polycarbonate obtained in the above-mentioned Reference Example 1 and 25 parts by weight of the crystalline polycarbonate powder obtained in Reference Example 2 were melt-mixed, and then Extrude at 220°C, and dip the extruded product in a phenol bath heated at 60°C for 5 minutes after cutting. After impregnation, the phenol was removed by filtration and the polymer was dried at 90°C for 1 hour to obtain a crystalline product with a particle size of 0.6-1.4 mm. The resulting crystalline product was further heated at 180°C for 1 hour to promote crystallization. The crystalline product had an intrinsic viscosity [η] of 0.25, a melting point of 240.2°C, a ΔH of 47.5 J / g, and a crystallinity of 23%, during which generation of fine particles was hardly detectable.
[0120] By using the obtained polycarbonate, solid phase polymerization was carried out at 220°C for 10 hours in the same manner as i...
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