Production method for carrying out low boiling point recycling on ethyl acetoacetate
A technology of ethyl acetoacetate and its production method, which is applied in the chemical industry, can solve problems such as combustion, and achieve the effects of reducing losses, increasing total yield, and reducing costs
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Embodiment 1
[0023] Embodiment 1 (reaction part):
[0024] Add 500kg of ethanol as a catalyst and 1.4kg of triethylenediamine in the reaction kettle, raise the temperature to reflux, add 913.1kg of diketene dropwise, raise the temperature to 110°C and keep it warm, after the reaction is completed, cool the reaction solution to 30°C, add 0.61kg of concentrated sulfuric acid, and keep it warm for 30 minutes , Filtration, and continuous distillation of the filtrate to obtain ethyl acetoacetate and low boilers.
Embodiment 2
[0025] Embodiment 2 (reaction part)
[0026] Add 500kg of ethanol to the reaction kettle as a catalyst and 0.12kg of triethylenediamine, raise the temperature to reflux, add 702.3kg of diketene dropwise, raise the temperature to 130°C and keep it warm, after the reaction is completed, cool the reaction solution to 30°C, add 0.05kg of concentrated sulfuric acid, and keep it warm for 30 minutes , Filtration, and continuous distillation of the filtrate to obtain ethyl acetoacetate and low boilers.
Embodiment 3
[0028] In the reactor, add 4000kg of low boilers obtained in reference to Example 1 (the content of ethyl acetoacetate is 36.5%, acetic acid is 12.1%, and ethanol is 25.6%), the temperature is raised to 80° C. for reflux, and 800 g of vitriol oil is added, and the esterification reaction is 1 Hours, normal pressure rectification to remove low boiling, the temperature of the kettle is raised to 120°C, the rectification is completed, cooled to 35°C and the reaction is completed, adding 170g of solid sodium hydroxide for neutralization, and after neutralization, it is passed through a conventional negative pressure rectification tower. Ethyl acetoacetate 1400.1kg, ethyl acetoacetate content is 99.6%, acidity is 0.041%, product recovery rate is 95.9%.
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