Production method for carrying out low boiler recycling on methyl acetoacetate
A technology for the production of methyl acetoacetate, which is applied in the chemical industry, can solve problems such as combustion, and achieve the effects of reducing losses, reducing costs, and improving total yield
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[0021] Example 1 (Reaction part):
[0022] Add 1.8kg of methanol 500kg catalyst triethylenediamine into the reaction kettle, raise the temperature to reflux, add 1312.5kg of diketene dropwise, raise the temperature to 115°C and keep it warm. After the reaction is completed, lower the temperature of the reaction solution to 30°C, add 0.79kg of concentrated sulfuric acid and keep it warm for 30 minutes , Filtration, and continuous distillation of the filtrate to obtain methyl acetoacetate and low boilers.
Example Embodiment
[0023] Example 2 (Reaction part)
[0024] Add methanol 500kg catalyst triethylenediamine 0.15kg to the reaction kettle, raise the temperature to reflux, add 1009.6kg diketene dropwise, raise the temperature to 130℃ and keep it warm. After the reaction is completed, cool the reaction solution to 30℃, add 0.06kg of concentrated sulfuric acid and keep it for 30 minutes , Filtration, and continuous distillation of the filtrate to obtain methyl acetoacetate and low boilers.
Example Embodiment
[0025] Example 3
[0026] Add 4000 kg of low boilers obtained in reference example 1 into the reactor (the content of methyl acetoacetate is 46.5%, acetic acid is 12.1%, methanol is 25.6%), the temperature is raised to 60°C and refluxed, 900g of concentrated sulfuric acid is added, and esterification reaction 1 After hours, the low boiling point was distilled out under normal pressure, the temperature of the kettle was raised to 120℃, the rectification was finished, and 188g of solid sodium hydroxide was added to neutralize after cooling to 44℃. After neutralization, it was rectified by a conventional negative pressure rectification tower. Methyl acetoacetate is 1781.9 kg, the content of methyl acetoacetate is 99.5%, the acidity is 0.045%, and the product recovery rate is 95.8%.
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