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Method for continuously recycling PGMEA from PGMEA/water solution through extractive rectification

A technology of extractive distillation and extractive distillation column is applied in the field of continuous dehydration of PGMEA/aqueous solution to achieve good social and economic benefits and simple process flow.

Active Publication Date: 2018-07-20
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

AI Technical Summary

Problems solved by technology

[0005] In order to overcome the problems existing in the prior art, the present invention provides a method for continuously recovering PGMEA from PGMEA / water solution by extractive distillation, which can solve the problem that PGMEA and water form the lowest azeotrope and cannot be separated and purified by ordinary rectification operations

Method used

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  • Method for continuously recycling PGMEA from PGMEA/water solution through extractive rectification

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Such as figure 1 As shown, the PGMEA / water solution 2 to be treated and the extractant 1 are continuously fed to the extractive distillation column A respectively. Extractant adopts ethyl benzyl ether, and the massfraction of PGMEA in PGMEA / water solution is 10%, and feed flow rate is 200kg / h, and the circulating flow rate of extractant ethyl benzyl ether is 200kg / h, and now ethyl Benzyl ether is 10 times the mass of PGMEA. The extractive distillation column A contains 31 theoretical plates, the PGMEA / water solution to be treated is continuously fed from the 14th theoretical plate of the extractive distillation column A, and the extractant ethyl benzyl ether is continuously fed from the second theoretical plate of the extractive distillation column A Feed, the material is heated into steam in the tower kettle, and enters the extractive distillation tower condenser B and the extractive distillation tower catcher C to condense, and the condensate enters the extractive di...

Embodiment 2

[0026] The difference between this embodiment and embodiment one is: the massfraction of PGMEA in PGMEA / water solution 2 is 50%, the feed flow rate is 50kg / h, and the extraction agent adopts ethyl benzyl ether, the content of ethyl benzyl ether The circulating flow rate is 100kg / h, and at this time, the ethyl benzyl ether is 4 times the mass of PGMEA. The extractive distillation column A contains 40 theoretical plates, the PGMEA / water solution to be treated is continuously fed from the 21st theoretical plate of the extractive distillation column A, and the extraction agent ethyl benzyl ether is continuously fed from the second theoretical plate of the extractive distillation column A Feed, the material is heated into steam in the tower kettle, and enters the extractive distillation tower condenser B and the extractive distillation tower catcher C to condense, and the condensate enters the extractive distillation tower reflux tank D, and the extractive distillation tower reflux ...

Embodiment 3

[0030]The difference between the present embodiment and embodiment two is: the massfraction of PGMEA in the PGMEA / water solution is 95%, the feed flow rate is 100kg / h, and the circulation flow rate of the extractant ethyl benzyl ether is 190kg / h, At this time, the ethyl benzyl ether is twice the mass of PGMEA. The extractive distillation column A contains 20 theoretical plates, the PGMEA / water solution to be treated is continuously fed from the 12th theoretical plate of the extractive distillation column A, and the extraction agent ethyl benzyl ether is continuously fed from the second theoretical plate of the extractive distillation column A Feed, the material is heated into steam in the tower kettle, and enters the extractive distillation tower condenser B and the extractive distillation tower catcher C to condense, and the condensate enters the extractive distillation tower reflux tank D, and the extractive distillation tower reflux ratio is 1, the flow rate of the overhead...

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Abstract

The invention discloses a method for continuously recycling high-purity PGMEA from a PGMEA / water solution through extractive rectification. Through addition of ethyl benzyl ether as an extractant, anazeotrope of PGMEA and water is destroyed, the extractant extracts the PGMEA from mixed liquid, mixed liquid of water, the PGMEA and the extractant is obtained at the top of a tower, wastewater is removed from a water phase after phase separation, and an organic phase returns to a temporary extractant storage tank and re-enters an extractive rectification tower; mixed liquid of the PGMEA and the extractant is taken out from a tower kettle of the extractive rectification tower, enters a reduced pressure rectification tower for separation, a PGMEA product is obtained in the tower top of the reduced pressure rectification tower, and an azeotrope agent is recycled in the tower kettle. By the method, the content of organic matters in the discharged wastewater is reduced to very low concentration, the wastewater can be discharged after simple treatment, the treatment amount of the organic matter-containing wastewater is reduced, the concentration of the organic matters in the wastewater is reduced, and the environment pollution is greatly reduced.

Description

technical field [0001] The invention relates to a method for continuous dehydration of PGMEA / water solution. 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 PGMEA / water system, PGMEA and water will form the lowest azeotrope with an azeotropic point of 96.8°C, and the co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/54C07C69/16
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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