Methods of purification of 2-aryl-3,3-bis(4-hydroxyaryl)phthalimidines, and polymers derived therefrom
A technology of benzopyrrolone and hydroxyaryl, applied in the field of purification of 2-aryl-3,3-bis(4-hydroxyaryl)benzopyrrolone and polymers derived therefrom, can solve the problem of phenolphthalein Derivatives are lengthy resources, phenolphthalein derivatives are difficult to prepare and separate, dense and other issues
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Embodiment 1A
[0087] 70 kilograms (kg) of phenolphthalein containing 10 wt% water, 98.75 kg aniline, and 22 kg HCl (32 wt% in water) were combined in a 200 liter (L) glass-lined reactor equipped with an overhead condenser. The reaction mixture was heated at 100 to 120 °C and passed through a wiped film evaporator to remove water as an aniline-water azeotrope. The reaction mixture was then heated at 170°C (internal temperature) and continued until the measured concentration of phenolphthalein in the reaction mass was about 1 wt%. The reaction mass was then cooled to 150 to 160°C. The reaction mixture was added to another reactor containing about 650 kg of NaOH (7 wt% to 10 wt% in water). Once the reaction mixture was mixed with aqueous NaOH, it was cooled to about 100°C. The resulting alkaline solution was continuously treated with aniline at a flow rate of about 40 kg / hr at a rate of about 70 kg / hour (hr) in a structured packing extraction column to remove aminophenol impurities. Traces ...
Embodiment 1B
[0093] 70.0 kg of phenolphthalein containing 10 wt% water, 98.75 kg of aniline and 22 kg of HCl (32 wt% in water) were combined in a 200 L glass lined reactor equipped with an overhead condenser. The reaction mixture was heated at 100 to 120 °C and passed through a wiped film evaporator to remove water as an aniline-water azeotrope. The reaction mixture was then heated at 170°C (internal temperature). The reaction was continued until phenolphthalein was about 1 wt% in the reaction mass as measured by HPLC. A portion of this reaction mixture was withdrawn and named Sample 1-1.
[0094] The reaction mass was then cooled to 150 to 160°C. The reaction mixture was added to another reactor containing about 600 kg of NaOH (7 wt% to 10 wt% in water). Once the reaction mixture was mixed with aqueous NaOH, it was cooled to about 100°C. The obtained alkaline solution was continuously treated with aniline at a flow rate of 53 kg / hr at a rate of 67 kg / hr in a structured packing extract...
Embodiment 2
[0102] Mix 300 mL of methanol and 29 mL of HCl in a 1 L glass reactor with an anchor stirrer. 150 mL of the carbon-treated base solution from Example 1A was slowly added to the reactor. The reaction mixture was heated at reflux (about 63°C) for 1 hour, then cooled and maintained at 25°C for 1 hour. The temperature was maintained for a further 30 minutes and then cooled to 10°C. The obtained crystalline solid was filtered and washed with 100 mL of hot water. The isolated product was dried and weighed to 9.2 g.
[0103] The HPLC analysis of the isolated products is given in Table 3.
[0104] table 3
[0105]
[0106] is not detected.
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