Depolymerization method of polycarbonate resin having fluorene structure
A polycarbonate resin, depolymerization technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of bisphenols stability, different solubility, etc., and achieve remarkable results
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[0049] Hereinafter, although an Example is given and this invention is demonstrated in more detail, this invention is not limited to these Examples.
[0050] For each measured value of the bisphenoxyl fluorenes and the polycarbonate resin, the following methods and measurement conditions were followed.
[0051] [1] HPLC purity
[0052] The area percentage value when HPLC measurement was performed under the following measurement conditions was taken as the HPLC purity of each component.
[0053] ・Device: "LC-2010AHT" manufactured by Shimadzu Corporation
[0054] ・Column: "L-column ODS" produced by the Chemical Substance Evaluation Research Institute of the General Incorporated Foundation
[0055] (5μm, 4.6mmφ×250mm)
[0056] ·Column temperature: 40℃
[0057] Detection wavelength: UV 254nm,
[0058] Mobile phase: A solution = water, B solution = acetonitrile
[0059] ·Mobile phase flow rate: 1.0ml / min
[0060] Mobile phase gradient: B solution concentration: 30% (0 minute...
Synthetic example 1
[0067] 20.00 parts by weight of 9,9-bis[4-(2-hydroxyethoxy)phenyl]fluorene (HPLC purity 98.7%, melting point 161° C.), 10.10 parts by weight of diphenyl carbonate, and sodium bicarbonate as a polymerization catalyst 2.2×10 -5 Add parts by weight into a reaction vessel equipped with a stirrer and a distillation device, heat to 200° C. under a nitrogen atmosphere, and stir for 20 minutes to completely melt. Then, the degree of reduced pressure in the reaction container was adjusted to 27 kPa, and it stirred at 200 degreeC for 40 minutes, 210 degreeC for 40 minutes, and 220 degreeC for 50 minutes. Then adjust the decompression degree and temperature, stir at 24kPa, 230°C for 30 minutes, and stir at 20kPa, 240°C for 50 minutes, then use 1 hour to make the decompression degree in the reaction vessel below 133Pa, and at 240°C, 133Pa or less The mixture was stirred for 1 hour to obtain a polycarbonate resin (weight-average molecular weight: 28,000, glass transition temperature: 152°...
Synthetic example 2
[0069] 18.09 parts by weight of 9,9-bis[2-(2-hydroxyethoxy)-4-methylphenyl]fluorene (HPLC purity 99.0%, melting point 172°C), 8.60 parts by weight of diphenyl carbonate and as a polymer Catalyst sodium bicarbonate 2.0 x 10 -5 Add parts by weight into a reaction vessel equipped with a stirrer and a distillation device, heat to 200° C. under a nitrogen atmosphere, and stir for 20 minutes to completely melt. Then, the degree of reduced pressure in the reaction container was adjusted to 27 kPa, and it stirred at 200 degreeC for 30 minutes, 210 degreeC for 50 minutes, and 220 degreeC for 30 minutes. Then adjust the decompression degree and temperature, stir at 24kPa, 230°C for 30 minutes, and stir at 20kPa, 240°C for 50 minutes, then use 1 hour to make the decompression degree in the reaction vessel below 133Pa, and at 240°C, 133Pa or less The mixture was stirred for 30 minutes under the condition of , to obtain a polycarbonate resin (weight average molecular weight: 27500, glass ...
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