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Method for continuously recovering PGMEA (propylene glycol methyl ether acetate) from PGMEA/aqueous solution by utilizing azeotropic distillation

A technology of azeotropic distillation and azeotropic distillation column, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as inability to separate and purify, low azeotrope, etc., to reduce production costs, Reduced pressure, the effect of reducing the content of organic matter

Inactive Publication Date: 2018-06-08
淄博高新技术产业开发区精细化工和高分子材料研究院 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to provide a method for continuously recovering high-purity PGMEA from PGMEA / water solution by azeotropic distillation, which can solve the problem that PGMEA and water form the lowest azeotrope and cannot be separated and purified by ordinary rectification.

Method used

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  • Method for continuously recovering PGMEA (propylene glycol methyl ether acetate) from PGMEA/aqueous solution by utilizing azeotropic distillation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Such as figure 1 Shown, the massfraction of PGMEA in the PGMEA / water solution 2 to be treated is 1%, and feed flow rate is 300kg / h, and the circulating flow rate of entrainer cyclohexane 1 is 891kg / h, and now entrainer consumption is 3 times the quality of water. The above-mentioned materials are continuously fed into the azeotropic rectification tower A containing 20 theoretical plates, the PGMEA / water solution to be treated is continuously fed from the 10th theoretical plate of the azeotropic rectification tower, and the entrainer cyclohexane is fed from the top of the tower Continuous feeding, the material is heated and vaporized in the bottom of the azeotropic distillation column, and then enters the gas phase condenser B at the top of the azeotropic distillation column, the gas phase is condensed into liquid in the condenser, and the gas phase condensate at the top of the azeotropic distillation column 4 and fresh entrainer 5 enter the phase separation tank C, and...

Embodiment 2

[0025] The difference between the present embodiment and embodiment one is: the massfraction of PGMEA in the PGMEA / water solution is 50%, the feed flow rate is 100kg / h, and the circulation flow rate of entrainer hexanaphthene is 250kg / h. When the amount of entrainer is 5 times of water quality. The above-mentioned materials are continuously fed to an azeotropic rectification tower containing 15 theoretical plates, the PGMEA / water solution to be treated is continuously fed from the 10th theoretical plate of the azeotropic rectification tower, and the entrainer cyclohexane is continuously fed from the top of the tower. Feed, the material is heated and vaporized in the bottom of the azeotropic distillation column and enters the condenser upwards, the gas phase is condensed into a liquid in the condenser, the condensate and fresh entrainer enter the phase separation tank, water and cyclohexane in the condensate The mass fractions were 16.7%, 83.3%, respectively. The flow rate of ...

Embodiment 3

[0028] The difference between this embodiment and embodiment two is: the mass fraction of PGMEA in the PGMEA / water solution is 99%, the feed flow rate is 500kg / h, and the recirculation flow rate of entrainer hexanaphthene is 35kg / h, this When the amount of entrainer is 7 times of water quality. The above-mentioned materials are continuously fed to an azeotropic rectification tower containing 30 theoretical plates, the PGMEA / water solution to be treated is continuously fed from the 16th theoretical plate of the azeotropic rectification tower, and the entrainer cyclohexane is continuously fed from the top of the tower. Feed, the material is heated and vaporized in the bottom of the azeotropic distillation column and enters the condenser upwards, the gas phase is condensed into a liquid in the condenser, the condensate and fresh entrainer enter the phase separation tank, water and cyclohexane in the condensate The mass fractions were 12.5%, 87.5%, respectively. The flow rate of ...

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Abstract

The invention discloses a method for continuously recovering high-purity PGMEA (propylene glycol methyl ether acetate) from PGMEA / aqueous solution by utilizing azeotropic distillation. The method is characterized by comprising the following steps: (1) feeding the PGMEA / aqueous solution and an azeotrope agent into an azeotropic distillation tower respectively and continuously, continuously extracting a PGMEA product with the mass percentage more than 99.9 percent from a tower kettle, continuously extracting the mixed steam of the azeotrope agent and water from the top of the tower, cooling through a heat exchanger, and enabling the obtained condensed liquid into a split phase tank; and (2) performing split phase on the mixed liquid of the azeotrope agent and water obtained in the step (1) in a split phase tank, enabling the water to be on the lower layer and the azeotrope agent to be on the upper layer after split phase, returning to the azeotropic distillation tower, recycling, simplytreating the extracted waste water and discharging. Azeotropy of the PGMEA and the water is broken through the addition of the azeotrope agent hexamethylene, and a high-purity PGMEA product is obtained through the tower kettle of the azeotropic distillation tower; furthermore, the organic matter content of the discharged waste water is reduced to extremely low concentration, discharging can be conducted through simple treatment, the treatment quantity of the organic matter-containing waste water is reduced, the organic matter concentration of the waste water is reduced and the environmental pollution is greatly reduced.

Description

technical field [0001] The invention relates to a method for continuous dehydration of a PGMEA aqueous solution, which obtains a PGMEA product with a purity of more than 99.9% through an azeotropic rectification operation. Background technique [0002] PGMEA (Propylene Glycol Methyl Ether Acetate) is a high-grade industrial solvent with excellent performance and low toxicity. It has strong solubility for polar and non-polar substances. PGMEA is usually used as the main component of cleaning solvents, suitable for adding to various polymers such as high-grade coatings and inks, and can be used to dissolve urethane, vinyl, polyester, cellulose acetate, acrylic resin, epoxy resin And nitrocellulose, novolac resin, etc. As a cleaning solvent, PGMEA will inevitably form a mixed solution with water. From the perspective of economy and environmental protection, the recovery of PGMEA from PGMEA waste liquid has huge economic and social value. [0003] Considering the nature of the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/16C07C67/54
CPCC07C67/54C07C69/16
Inventor 吕灵娟杜振江刘宁那平白鹏
Owner 淄博高新技术产业开发区精细化工和高分子材料研究院
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