Method for the recovery of compounds deriving from the synthesis of aryl ether ketones
A technology of aryl ether ketone and composition, applied in chemical instruments and methods, separation methods, vertical tube evaporators, etc., can solve the problems of large volume and cost, and achieve simplicity and cost, minimize volume and harmful properties, and reduce cost effect
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Embodiment 1
[0263] Embodiment 1: collect the synthesis residual solvent and Reactant
[0264] The residue composition derived from the synthesis of 1,4-bis(4-phenoxybenzoyl)benzene was heated under a vacuum of 23 mmHg in a Rotavap (rotating flask) apparatus in which the flask was heated at 170 °C by a hot oil bath. heating. Despite recovering essentially all of the ODCB and greater than 80% of the DPE, the concentrated residue formed a skin on the interior surface of the spinner flask that could only be removed by scraping.
Embodiment 2-8
[0265] Example 2-8: Synthesis from 1,4-bis(4-phenoxybenzoyl)benzene or PEKK recovered by thin film evaporator residual solvents and reactants
[0266] The synthesis residue composition derived from the synthesis of 1,4-bis(4-phenoxybenzoyl)benzene and / or PEKK as previously described in Example 1 was continuously fed into a Pilot scale thin film evaporator (TFE). The TFE is heated by hot oil through a jacket and operates under a vacuum in the range of 500-3000 Pa. The temperature of the concentrated residue leaving the evaporator was measured and controlled within the range of 160-175°C by adjusting the heating oil temperature and vacuum. The residual composition originating from the synthesis of 1,4-bis(4-phenoxybenzoyl)benzene or PEKK or a mixture of these two in the range of 100-250 kg / hr.m 2 The rate of continuous feeding. TFE rotor corresponding to 70-280s -1 Operate under the speed range of the shear rate.
[0267] The TFE vapor was condensed and collected, and t...
Embodiment 9
[0273] Example 9: Recovery of Residual Solvent and Reactants by Thin Film Evaporator with Further Use of Displacement Compounds
[0274] The residue feed was the same as Example 6, with 5 kg of molten "displacer" wax (stearin or hydrogenated soybean oil) co-fed to the evaporator per lb of residue feed to the evaporator. 250s at 10 Torr vacuum and 213°C -1 Operating the TFE at a shear rate increased the recovery of ODCB and DPE to 99.98% and 99.88%, respectively, and reduced the concentration of ODCB in the concentrated residue to 945ppm, making the concentrated residue "harmless" under current U.S. regulations. of".
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