Production method for carrying out low boiling point recycling on ethyl acetoacetate
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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
Active Publication Date: 2017-05-31
NANTONG ACETIC ACID CHEM
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Combustible, there is a danger of burning when expos
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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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Abstract
The invention discloses a production method for carrying out low boiling point recycling on ethyl acetoacetate. The production method comprises the following steps: adding ethyl alcohol and a catalyst triethylene diamine in a reaction kettle; carrying out heating reflux; dropwise adding diketene; keeping warm; cooling a reaction solution after a reaction is completed; adding concentrated sulfuric acid; keeping warm; filtering; carrying out continuous rectification on filtrate; rectifying to obtain a low-boiling-point substance; adding acid in the low boiling point for esterifying; rectifying to obtain the low-boiling-point substance at normal pressure after carrying out the heating reflux for 1 to 2 hours; stopping rectifying after rising the kettle temperature to be 115 to 125 DEG C; cooling to 40 to 50 DEG C; neutralizing by using solid base; enabling a neutralized material to enter a conventional negative pressure rectifying system, and rectifying to obtain an ethyl acetoacetate finished product, wherein the content of the ethyl acetoacetate finished product is greater than 99.0 percent, the acidity is smaller than 0.05 percent, and the product recovery rate is 95 percent or above. According to the production method disclosed by the invention, loss of the ethyl acetoacetate is reduced, the total yield of the ethyl acetoacetate is increased, a resource can be recycled and reutilized, and the cost is reduced.
Description
technical field [0001] The invention relates to the field of chemical industry, in particular to a method for recovering ethyl acetoacetate. Background technique [0002] Ethyl acetoacetate, English name: Ethyl acetoacetate, alias: ethyl acetoacetate, molecular formula and molecular weight: C6H8O3=130.14 [0003] Physical and chemical properties: Soluble in organic solvents, it turns purple when it meets ferric chloride. When it is hydrolyzed with dilute acid or dilute alkali, it will generate acetone, ethanol and carbon dioxide. Appearance: Colorless liquid with aromatic odor. Melting point (ketone formula) / °C: -39, (alcohol formula) / °C: -44. Boiling point (101.3kPa) / °C: 180.8. Relative density: 1.02126, refractive index (20°C): 1.4192, flash point (closed cup) / °C: 84.4. Viscosity (25°C) / mPa.s: 1.5081, surface tension (20°C) / mN / m: 32.51 [0004] Soluble in organic solvents, 12% dissolved in water at 25°C, 4.9% dissolved in ethyl acetoacetate in water, miscible with eth...
Claims
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