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Reactive rectification method and device for separating ethylene glycol, propylene glycol and butylene glycol

A reactive distillation tower, ethylene glycol technology, applied in chemical instruments and methods, separation/purification of hydroxyl compounds, preparation of organic compounds, etc., can solve the problem that propylene glycol and butanediol are not recycled, azeotroped or extracted The problems of high energy consumption and low separation energy consumption in rectification separation can achieve the effect of reducing energy consumption, less side reactions and better separation effect.

Active Publication Date: 2016-05-04
TIANJIN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The purpose of the present invention is to provide a reactive distillation separation method and device for ethylene glycol, propylene glycol and butanediol, which solves the problem of high energy consumption in the current azeotropic or extractive distillation separation, and that propylene glycol and butanediol are not well recovered Taking advantage of this problem, the method has the advantages of low separation energy consumption, good separation of diol mixture and high recovery rate

Method used

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  • Reactive rectification method and device for separating ethylene glycol, propylene glycol and butylene glycol
  • Reactive rectification method and device for separating ethylene glycol, propylene glycol and butylene glycol
  • Reactive rectification method and device for separating ethylene glycol, propylene glycol and butylene glycol

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Embodiment 1

[0047] use figure 1 Shown flow process, raw material S01 (the mass fraction of ethylene glycol is 47.4%, the mass fraction of 1,2-propanediol is 21.2%, the mass fraction of 1,2-butanediol is 31.4%) and reactant acetaldehyde S02 Respectively enter from the upper part of the reaction section of the reactive distillation tower T11 and the bottom of the tower, the total number of theoretical plates of the reactive distillation tower is 21, the operating pressure is 0.5atm in terms of absolute pressure, the reflux ratio is 0.14, and the catalyst uses NKC-9 macroporous acidic cations Resin, the feeding amount of acetaldehyde and the total molar ratio of diol are 1.2:1, and the content of diol is controlled at the top of the tower. The stream S07 produced from the top of the reactive distillation tower enters the acetaldehyde recovery tower T12, the tower operating pressure is 2 atm in absolute pressure, the total number of theoretical plates is 20, the reflux ratio is 1.7, and unrea...

Embodiment 2

[0052] use figure 1 Shown flow process, raw material S01 (the mass fraction of ethylene glycol is 61.9%, the mass fraction of 1,2-propanediol is 22.3%, the mass fraction of 2,3-butanediol is 15.8%) and reactant acetaldehyde S02 Respectively enter from the upper part of the reaction section of the reactive distillation tower T11 and the bottom of the tower, the total number of theoretical plates of the reactive distillation tower is 21, the operating pressure is 0.5atm in terms of absolute pressure, the reflux ratio is 0.14, and the catalyst uses NKC-9 macroporous acidic cations Resin, the feeding amount of acetaldehyde and the total molar ratio of diol are 1.2:1, and the content of diol is controlled at the top of the tower. The stream S07 produced from the top of the reactive distillation tower enters the acetaldehyde recovery tower T12, the tower operating pressure is 2 atm in absolute pressure, the total number of theoretical plates is 20, the reflux ratio is 1.7, and unrea...

Embodiment 3

[0056] use figure 1The flow process shown, raw material S01 (the mass fraction of ethylene glycol is 84.7%, the mass fraction of 1,3-propanediol is 8.3%, the mass fraction of 1,3-butanediol is 7.0%) and reactant propionaldehyde S02 Respectively enter from the upper part of the reactive distillation column T11 reaction section and the bottom of the tower, the total number of theoretical plates of the reactive distillation column is 20, the operating pressure is 0.5atm in terms of absolute pressure, the reflux ratio is 0.12, and the catalyst uses NKC-9 macroporous acidic cationic resin , the feeding amount of propionaldehyde and the total molar ratio of diol are 1.5:1, and the content of diol is controlled at the top of the tower. The stream S07 produced from the top of the reactive distillation tower enters the propionaldehyde recovery tower T12. The operating pressure of the tower is 1.5 atm in terms of absolute pressure, the total number of theoretical plates is 22, and the r...

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Abstract

The invention relates to a separation method and device for a mixture of ethylene glycol, propylene glycol and butylene glycol, and mainly aims to solve the problems that ethylene glycol, propylene glycol and butylene glycol are difficult to separate, the energy consumption is high and a high-purity glycol product is difficult to obtain at present. According to the method and device provided by the invention, by adoption of acetal or ketal reversible reaction, a glycol mixture reacts with a reactant namely aldehyde / ketone in a reaction rectification tower T11 to generate an acetal / ketone mixture S07 at first, and then separation is carried out sequentially by virtue of a rectification method to obtain unreacted aldehyde / ketone S12, a mixture S19 of an ethylene glycol acetal / ketone product and water, a mixture S26 of a propylene glycol acetal / ketone product and water, and a mixture S27 of a butylene glycol acetal / ketone product and water. The invention has the advantages that a method of reactive rectification is adopted to change a difficult problem of separating glycol mixtures with close boiling points to produce an azeotrope and having relatively small relative volatility into a problem of separating acetal / ketone products which are relatively easy to separate, and an effect of effectively separating the glycol mixtures is achieved.

Description

technical field [0001] The invention belongs to the field of chemical distillation and separation, and relates to a method for reactive distillation and separation of ethylene glycol, propylene glycol and butanediol. Background technique [0002] As an important basic organic chemical raw material, ethylene glycol is mainly used in the production of polyester fibers, antifreeze, unsaturated polyester resins, lubricants, plasticizers, nonionic surfactants and explosives. In addition, ethylene glycol Alcohol can also be used in coatings, photographic developer, brake fluid, and ink industries, as a solvent and medium for ammonium perborate, and for the production of special solvents such as glycol ether, etc., with a wide range of uses. Moreover, studies have pointed out that ethylene glycol has great potential for development in the field of liquid fuel cells in the future. [0003] At present, large-scale ethylene glycol production at home and abroad adopts direct hydration...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/20C07C29/88C07C29/74
CPCC07C29/74C07C29/88C07C31/202C07C31/205C07C31/207Y02P20/10
Inventor 高鑫李鑫钢李洪黄伟进许长春
Owner TIANJIN UNIV
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