Synthesis technique of alpha-cyanoacrylate monomer
A cyanoacrylate and synthesis process technology, applied in the preparation of carboxylic acid nitrile, the preparation of organic compounds, organic chemistry, etc., can solve the problems of large solvent usage, long production cycle, and large energy consumption, and achieve low cost, Energy saving and high yield effect
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Embodiment 1
[0020] Example 1: Add 300.0g ethyl cyanoacetate, 83.5g paraformaldehyde and catalyst (hexahydropyridine) into a 1000ml four-necked flask equipped with a stirrer, condenser and thermometer, and slowly heat under stirring. The reaction starts when the temperature reaches 60°C, the reaction temperature is increased naturally for 100 minutes, the internal temperature reaches 120°C, and the reaction is stopped by adding phosphoric acid. Add (30 g) dibutyl phthalate, and add 400 drops under heating (the oil temperature is set at 120°C) Gram benzene azeotropic dehydration. The solvent is added in about ten minutes. Finally, the residual solvent and water are removed under reduced pressure, a small amount of hydroquinone and phosphorus pentoxide are added in vacuum, and then vacuum cracking is carried out under the protection of sulfur dioxide gas (170℃---- -210℃ / 2.67KPa) to obtain a crude product. Add the crude product to the refined bottle and distill it under reduced pressure once,...
Embodiment 2
[0021] Example 2: Add 300.0g ethyl cyanoacetate, 83.5g paraformaldehyde and catalyst (KOH) into a 1000ml four-necked flask equipped with a stirrer, condenser and thermometer, and slowly heat under stirring until the internal temperature reaches Start the reaction at 60°C, naturally increase the temperature for 100 minutes, add phosphoric acid to stop the reaction, add (40g) dioctyl phthalate, and add 450g methanol dropwise under heating (the oil temperature is set to 125°C) Dehydrated. The solvent is added in about 8 minutes, and finally the residual solvent and water are removed under reduced pressure, a small amount of hydroquinone and phosphorus pentoxide are added in vacuum, and then the vacuum cracking is carried out under the protection of sulfur dioxide gas (170℃---210 ℃ / 2.67KPa) to obtain a crude product. Add the crude product to the refined bottle and distill it under reduced pressure once, add a small amount of hydroquinone and sulfur dioxide inhibitor to store, and ...
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