Transesterification process for production of (meth)acrylate ester monomers
A technology of alkyl acrylate and transesterification, which is used in catalyst activation/preparation, reaction preparation of ester groups and hydroxyl groups, chemical instruments and methods, etc., and can solve problems such as catalysts failing to function.
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Embodiment 1
[0062] Example 1 describes a single one-shot mixed salt transesterification catalyst capable of producing the desired product even when the dehydration step used to reduce the water content of the reaction mixture is omitted.
[0063] Add the mixture of the following components into the equipment equipped with temperature display / temperature controller, magnetic stirrer, mixed gas (8% O 2 to 92%N 2 ) injection inlet, 1 inch diameter 10-plate Oldershaw column equipped with distillation head, proportional removal of distillate-vapor pressure thermostat and stepwise distillate receiver in a 2-liter 4-neck flask: 260.3 grams (2.0 moles ) 1-hydroxyethylene urea (HEEU), 680.8 g (6.8 moles) methyl methacrylate (MMA), 1.0 g (0.006 moles) 4-hydroxy-2,2,6,6-tetramethylpiperidine Oxygen radical (4-hydroxy TEMPO, free radical), 2.77 grams (0.02 mole) of potassium carbonate and 1.49 grams (0.02 mole) of potassium chloride. The mixture was then heated (at a rate of 2.3°C / min) to 98°C whil...
Embodiment 2
[0065] Example 2 demonstrates the re-use of used recovered catalyst in subsequent reactions.
[0066] Add the mixture of the following components into the equipment equipped with temperature display / temperature controller, magnetic stirrer, mixed gas (8% O 2 to 92%N 2 ) injection inlet, 1 inch diameter 10-plate Oldershaw column with distillation head, distillation rate of distillate-vapor pressure thermostat and stepwise distillate receiver in a 2-liter 4-neck flask: 260.3 grams (2.0 moles) 1-hydroxyethyleneurea (HEEU), 680.8 grams (6.8 moles) methyl methacrylate (MMA), 1.0 grams (0.006 moles) 4-hydroxy-2,2,6,6-tetramethyl piperidinyloxy radical (4-hydroxy TEMPO, free radical), 2.77 grams (0.02 moles) of potassium carbonate and 1.49 grams (0.02 moles) of potassium chloride. The mixture was then heated (at a rate of 2.3°C / min) to 98°C while removing the reaction azeotrope MMA-methanol. During the reaction, the mixture was stirred, sprayed with a mixed gas, and continuously h...
Embodiment 3
[0068] Example 3 shows how the above heterogeneous catalyst system prepares MEEU with a lower ratio of MMA:HEEU (3.2:1).
[0069] Add the mixture of the following components into the equipment equipped with temperature display / temperature controller, magnetic stirrer, mixed gas (8% O 2 to 92%N 2 ) injection inlet, 1 inch diameter 10-plate Oldershaw column equipped with distillation head, distillation rate of distillate-vapor pressure thermostat and step-by-step distillate receiver in a 2-liter 4-neck flask: 260.3 g ( 2.0 moles) 1-hydroxyethyleneurea (HEEU), 640.5 grams (6.4 moles) methyl methacrylate (MMA), 1.0 grams (0.006 moles) 4-hydroxy-2,2,6,6-tetramethyl Piperidinyloxy radical (4-hydroxy TEMPO, free radical). The mixture was then heated (at a rate of 2.3°C / min) to 98°C while removing the reaction azeotrope MMA-methanol. During the reaction, the mixture was stirred, sprayed with a mixed gas, and continuously heated to reflux under a vacuum of 700 mm Hg, while removing ...
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