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A kind of diketene continuous rectification process

A technology for diketene and crude diketene, which is applied in the chemical industry and can solve problems such as high energy consumption and complicated processes

Active Publication Date: 2019-07-30
NANTONG ACETIC ACID CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process introduces multiple reactions such as hydrolysis and rectification, and only treats the residue, which requires high energy consumption and relatively complicated process

Method used

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  • A kind of diketene continuous rectification process

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] After adding an appropriate amount of crude diketene (content 90%) into the film evaporator, the crude diketene enters the film evaporator continuously at 200kg / h, controls the vacuum degree -0.1MPa, and continuously discharges the material at a bottom temperature of 65°C and a top temperature of 55°C ; The discharge temperature of the primary condenser is 45°C, the output condensate is 190.8kg / h, the content of diketene is 99.2%, the discharge temperature of the secondary condenser is 10°C, and the condensate is 2kg / h; the secondary condensate is 2kg / h , residue 7kg / h, methanol 9kg / h, triethylenediamine 0.018kg / h continuously enter the esterification tank, maintain the temperature of the esterification tank at 55-60 ° C, and continuously discharge to the fuel storage tank, the distillation yield of diketene is 95.4 %, the primary finished product content is 99.2%.

Embodiment 2

[0030] After adding an appropriate amount of crude diketene (content 95%) into the film evaporator, the crude diketene enters the film evaporator continuously at 200kg / h, controls the vacuum degree -0.15MPa, and continuously discharges the material at a bottom temperature of 55°C and a top temperature of 50°C ; The discharge temperature of the primary condenser is 40°C, the output condensate is 190.4kg / h, the content of diketene is 99.3%, the discharge temperature of the secondary condenser is 0°C, and the condensate is 2kg / h; the secondary condensate is 2kg / h , residue 7.2kg / h, methanol 13.8kg / h, triethylenediamine 0.012kg / h continuously enter the esterification tank, maintain the temperature of the esterification tank at 75-80°C, and continuously discharge to the fuel storage tank, diketene rectification The rate is 95.2%, and the finished product content is 99.3%.

Embodiment 3

[0032] After adding an appropriate amount of crude diketene (content 93%) into the film evaporator, the crude diketene enters the film evaporator continuously at 200kg / h, controls the vacuum degree -0.12MPa, and continuously discharges the material at a bottom temperature of 60°C and a top temperature of 52°C ; The discharge temperature of the primary condenser is 43°C, the output condensate is 191.4kg / h, the content of diketene is 99.1%, the discharge temperature of the secondary condenser is 5°C, and the condensate is 1.8kg / h; the secondary condensate is 1.8kg / h, residue 6.8kg / h, methanol 11kg / h, triethylenediamine 0.015kg / h continuously enter the esterification tank, maintain the temperature of the esterification tank at 65-70 ° C, and continuously discharge to the fuel storage tank, diketene rectification The yield is 95.7%, and the primary product content is 99.1%.

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Abstract

The invention discloses a continuous rectification process for diketene. A diketene crude product continuously enters a film type evaporator, the vacuum degree is controlled to be -0.15 to -0.1MPa, and continuous discharge is performed at the bottom temperature of 55 to 65 DEG C and at the top temperature of 50 to 55 DEG C; continuous condensation is performed under the conditions that the discharge temperature of a primary condenser is 40 to 45 DEG C, the diketene content of a condensate is more than or equal to 99.0 percent, and the discharge temperature of a secondary condenser is 0 to 10 DEG C, wherein the diketene content of a secondary condensate is less than or equal to 10 percent; the secondary condensate, residues, methyl alcohol and a catalyst namely triethylene diamine are continuously added into an esterification reactor for continuous esterification reaction, and a reaction solution is continuously output by serving as fuel; the mass ratio of the residues and the secondary condensate to the methyl alcohol is 1:(1.0 to 1.5), the mass ratio of the residues, the secondary condensate and the methyl alcohol to the catalyst namely the triethylene diamine is 1:(0.0005 to 0.001), and the esterification reaction temperature is 55 to 80 DEG C. The continuous rectification process is used to perform continuous rectification, continuous discharge, continuous discharge of the residues and continuous treatment on the residues and a acetone condensate, thus realizing environmental protection and energy saving.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a diketene continuous rectification process. Background technique [0002] Diketene, alias: 3-hydroxybutenoic acid-β-lactone; Diketene, English name: diketene. Appearance properties: colorless liquid with pungent odor. Solubility: Soluble in water and most organic solvents; CAS No.: 674-82-8. Molecular formula: C4H4O2. Molecular weight: 84.0734. Melting point (°C): -7.5. Boiling point (°C): 127.4. Relative density (water=1): 1.089. Relative vapor density (air=1): 2.9. And vapor pressure (kPa, 20°C): 1.05. Critical temperature (°C): 310. Critical pressure (MPa): 5.47. Octanol / water partition coefficient: -0.39. Flash point (°C): 34. Ignition temperature (°C): 275. Explosive upper limit (%): 11.7. Lower explosion limit (%): 2 [0003] Diketene has a strong reaction ability and can be derived from a variety of products. It is a raw material for fine chemicals such as ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D305/12
CPCC07D305/12
Inventor 丁彩峰庆九朱小刚刘芳姚俊生王健华
Owner NANTONG ACETIC ACID CHEM