Method, process and apparatus for separation of ethylene glycol and 1,2-butanediol

A technology of ethylene glycol and butanediol, applied in chemical instruments and methods, separation/purification of hydroxyl compounds, preparation of organic compounds, etc., can solve problems such as affecting the yield of ethylene glycol, unfavorable energy saving, and poor recovery. , to achieve the effect of high quality recycled products, saving equipment investment and reducing operating costs

Active Publication Date: 2016-06-01
TIANJIN UNIV
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0005] 1. Patent CN101928201 discloses a purification process for the crude product of coal-based ethylene glycol. The purification process is obtained from the crude product of coal-based ethylene glycol through saponification reaction, methanol removal, hydrogenation reaction, three-tower rectification and adsorption treatment. High-purity ethylene glycol products, but 1,2-butanediol is only removed by azeotropy with ethylene glycol, which not only causes the loss of 1,2-butanediol, a high value-added product, but also affects the Yield of diol
[0006] 2. Patent CN102276418 proposes to use a mixture of ethylene glycol and 1,2-butanediol from the process of oxalate hydrogenation to ethylene glycol products, by using at least one of ZSM-5, Y-type zeolite or beta zeolite An adsorbent that absorbs 1,2-butanediol to obtain the purification of ethylene glycol. However, the recovery rate of ethylene glycol is not indicated, and the recovery and utilization of 1,2-butanediol is not involved.
[0007] 3. Patent CN103193594 discloses a method for separating and purifying ethylene glycol from the liquid phase product of oxalate hydrogenation by using a dioxane compound immiscible with ethylene glycol as an entrainer and using azeotropic distillation method, the liquid phase mixture passes through two light removal towers to remove low-boiling compounds such as methanol and methyl glycolate, and then enters the azeotropic rectific

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  • Method, process and apparatus for separation of ethylene glycol and 1,2-butanediol
  • Method, process and apparatus for separation of ethylene glycol and 1,2-butanediol
  • Method, process and apparatus for separation of ethylene glycol and 1,2-butanediol

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Embodiment 1

[0080] The method of the present invention is used for the reaction separation process of ethylene glycol and 1,2-butanediol mixture, such as figure 1As shown, including acetal reactor (R1), aldehyde / ketone recovery column (T11), ethylene glycol acetal / ketone product separation column (T12), butanediol acetal / ketone product separation column (T13), acetal Aldehyde / ketone hydrolysis distillation column (T21, T31), ethylene glycol purification column (T22), 1,2-butanediol purification column (T32), condenser, reboiler, pump and related feed lines and Connect the lines to the above equipment. The diol mixed raw material S02 (the molar ratio of ethylene glycol and 1,2-butanediol: 0.55:0.45) and the reactant acetaldehyde S01 are added to the fully mixed tank reactor (R1). The molar ratio of the total amount of materials was 1, the reaction was carried out at 60° C. and an absolute pressure of 1.5 atm, the reaction residence time was controlled to be 40 minutes, and a macroporous ...

Embodiment 2

[0083] The method of the present invention is used for ethylene glycol and 1,2-butanediol mixture reactive distillation separation process, such as figure 2 As shown, for the improved process of Example 1, it is considered to separate the acetal product of 1,2-butanediol as a product without hydrolysis, including reactor (R1), aldehyde / ketone recovery column (T11), ethyl acetate Glycol acetal / ketone product separation tower (T12), butanediol acetal / ketone product separation tower (T13), ethylene glycol acetal / ketone hydrolysis distillation tower (T21), ethylene glycol refining tower (T22) , 1,2-Butanediol acetal product refining column (T41), phase separator (D1), condenser, reboiler, pump and related feed pipelines and pipelines connecting the above equipment. The other operations of the second embodiment are the same as those of the first embodiment. The overhead draw stream S37 of the butanediol acetal product separation column (T13) enters the 1,2-butanediol acetal produc...

Embodiment 3

[0086] The method of the present invention is used for ethylene glycol and 1,2-butanediol mixture reactive distillation separation process, such as image 3 As shown, it is an improved process of Example 1, and the acetal / ketone product considers the separation method after hydrolysis, and other operations in Example 3 are the same as those in Example 1. Reactors R2 and R3 are both carried out at 75°C and 2 atm absolute pressure, the reaction residence time is controlled to 40 minutes, and a basic ion resin catalyst is used; after hydrolysis, the total number of theoretical plates in the aldehyde recovery tower (T51) is 13, and the operating absolute pressure is 1.3 atm , the reflux ratio is 5; the total number of theoretical plates of the aldehyde recovery tower (T61) after hydrolysis is 13, the absolute operating pressure is 1.3 atm, and the reflux ratio is 5; the total number of theoretical plates of the unhydrolyzed acetal recovery column (T52) is 12, and the absolute opera...

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Abstract

The invention relates to a method, a process and an apparatus for separation of ethylene glycol and 1,2-butanediol. The method includes, (1) subjecting ethylene glycol and 1,2-butanediol to reaction through acetal/ketal to produce acetal/ketal liquid product mixture correspondingly, (2) separating the acetal/ketal liquid product mixture containing ethylene glycol and 1,2-butanediol by a series of rectifying columns, (3) separating different acetal/ketal products by rectifying according to difference of boiling points of acetal or ketal, (4) respectively hydrolyzing the acetal/ketal products to obtain an ethylene glycol primary product and a 1,2-butanediol primary product, and (5) purifying the ethylene glycol primary product and the 1,2-butanediol primary product respectively by rectifying to obtain an ethylene glycol product and a 1,2-butanediol product. The purity of the ethylene glycol product can be up to 99.9% and the recovery thereof can be up to 99.5%; the purity of the 1,2-butanediol product can be up to 98.5%. By a reversible-reaction conversion method, the difficulty in separating ethylene glycol and 1,2-butanediol which are of similar boiling points and low relative volatility and are azeotropic is changed into the problem about separation of acetal/ketal products which are easy to separate relatively.

Description

technical field [0001] The invention belongs to the field of chemical distillation and separation, and relates to a separation method, process and device of ethylene glycol and 1,2-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. Alcohols can also be used in coatings, photographic developers, brake fluids and inks, etc., as solvents and media for ammonium perborate, and in the production of special solvents such as glycol ethers, which are widely used. And some studies have pointed out that ethylene glycol has great development potential in the field of liquid fuel cells in the future. my country is a big consumer of ethylene glycol, and the domestic output of ethylene glycol is far from meeting its own needs. In 2014, my country's ethylene glycol output wa...

Claims

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Application Information

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IPC IPC(8): C07C29/74C07C31/20C07C29/92C07C29/80
CPCC07C29/74C07C29/80C07C29/92C07C31/202C07C31/207C07C31/20
Inventor 李鑫钢高鑫黄伟进李洪
Owner TIANJIN UNIV
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