Method for absorbing and refining high-purity methylacrolein

A methacrolein and refining method technology, applied in the field of absorption and refining of high-purity methacrolein, can solve the problems of high loss of methanol, low absorption efficiency, difficult separation, etc., and achieve less loss of absorbent and less loss of absorbent Small size, high process safety effect

Active Publication Date: 2021-12-28
ZHEJIANG HUANGMA TECH +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Patent CN 1817844A uses water as an absorbent to absorb methacrolein, but due to poor mutual solubility between water and methacrolein, a large amount of water is needed for absorption, the absorption efficiency is low, and energy consumption is large
[0005] The patent GP2110031 uses methanol as the absorbent to improve the absorption efficiency, but the boiling point of methanol is too low, and it is easy to vaporize during the absorption process, causing a large amount of methanol to be discharged with the tail gas, resulting in a large loss of methanol and easy to cause safety accidents
[0006] The patent US3957880 uses ethanol and isopropanol as absorbents. Although these absorbents have a higher boiling point than methanol, the existence of a large amount of diluent gas in the oxidation reaction will still cause the absorbent to be taken away, causing losses. The miscibility is good, and the water in the reaction product will also be absorbed, causing separation difficulties
[0007] Patent CN101844973A adopts alcohols with carbon number greater than 4 as absorbent, which reduces the loss of absorbent to a certain extent, but alcohols with larger carbon number basically have a stronger pungent smell (such as butanol has a pungent odor). Odor, can cause coughing), leading to serious air pollution after the exhaust gas is discharged after absorption, and some alcohols have a low flash point, which is unsafe to use
[0008] CN103833537A uses alkanes with 6 to 8 carbons as absorbents, but the boiling points of these alkanes are less different from those of methacrolein, so separation is difficult, and the lower boiling point will also cause more absorbent loss
[0009] Patent CN101020625 uses ionic liquids for absorption, which has high absorption efficiency, but ionic liquids are expensive and difficult to use on a large scale

Method used

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  • Method for absorbing and refining high-purity methylacrolein
  • Method for absorbing and refining high-purity methylacrolein
  • Method for absorbing and refining high-purity methylacrolein

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] The gas phase product after isobutene oxidation is cooled to 15°C and enters the packed absorption tower. Use 5 times the gas mass of phenoxyethanol (15°C) for absorption. The volume content of the gas before and after absorption is shown in Table 1 (the data in the table are volume percentage content).

[0033]

[0034] The content of methacrolein in the heavy phase obtained from the absorption liquid obtained at the bottom of the absorption tower after standing still for 1 hour and separated was 6.4%. In the rectification operation, the temperature at the bottom of the tower was 75° C., and the reflux ratio was 0.5 to obtain the high-purity product methacrolein, the composition of which is shown in Table 2 (the data in the table are percentages by mass).

[0035]

[0036]

Embodiment 2

[0038] The gas phase product after isobutene oxidation is cooled to 15°C and enters the packed absorption tower. Diethylene glycol monophenyl ether (15°C) 5 times the mass of the gas is used for absorption. The volume content of the gas before and after absorption is shown in Table 3 (the data in the table are volume percentage content).

[0039]

[0040] The content of methacrolein in the heavy phase obtained from the absorption liquid obtained at the bottom of the absorption tower after standing for 2 hours and stratified was 6.1%, and the heavy phase was subjected to rectification. In the rectification operation, under the condition that the tower bottom temperature is 80° C. and the reflux ratio is 1.0, a high-purity product methacrolein is obtained, and its composition is shown in Table 4 (the data in the table are mass percentages).

[0041] methacrolein Methacrylate Acetic acid water other 99.43 0.14 0.06 0.20 0.18

Embodiment 3

[0043] The gas phase product after isobutene oxidation is cooled to 15°C and enters the packed absorption tower. A mixture of phenoxyethanol and diethylene glycol monophenyl ether 5 times the mass of the gas is used for absorption. In the mixture, (the mass percent content of phenoxyethanol is 90%, and the temperature is 15° C.). The volume content of the gas before and after absorption is shown in Table 5 (the data in the table are volume percentage content).

[0044]

[0045] The content of methacrolein in the absorption liquid obtained at the bottom of the absorption tower was 6.3%. After standing still for 1.5 hours, the heavy phase was obtained by stratification, and the heavy phase was subjected to rectification. In the rectification operation, under the condition that the tower bottom temperature is 80° C. and the reflux ratio is 0.5, a high-purity product methacrolein is obtained, and its composition is shown in Table 6 (the data in the table are percentages by mass...

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Abstract

The invention belongs to the field of fine chemical engineering, and relates to a method for absorbing and refining high-purity methylacrolein. According to the method, phenoxyethanol, diethylene glycol monophenyl ether or a mixture of the phenoxyethanol and the diethylene glycol monophenyl ether is adopted as an absorbent to absorb the methylacrolein in the mixed gas in the oxidation step, and the methylacrolein with the purity larger than 99% is obtained through standing layering and rectification. The process has the advantages of high absorption efficiency, high product purity, simple and non-toxic absorbent recovery and application, high safety, simple operation and less absorbent loss, and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of fine chemicals, and in particular relates to a method for absorbing and refining high-purity methacrolein. Background technique [0002] Methacrolein is an important chemical raw material. Further oxidation can obtain methacrylic acid, and derivatives such as methyl methacrylate and glycidyl methacrylate; after reduction of methacrolein, methacrylic acid can be obtained Propanol, which is an important raw material for a new generation of high-performance water reducers; in addition, methacrolein can also be used in the manufacture of copolymers and resins. [0003] At present, the method for producing methacrolein is mainly the selective oxidation of isobutylene or tert-butanol, which is environmentally friendly. However, the product obtained by this method is in a gaseous state, which contains a large amount of diluent gas (such as nitrogen, etc.), and the content of methacrolein is relatively low, so it needs to...

Claims

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Application Information

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IPC IPC(8): C07C47/22C07C45/80C07C45/82
CPCC07C45/80C07C45/82C07C47/22Y02P20/10
Inventor 赵炯烽王伟松席蓝萍王胜利秦飞
Owner ZHEJIANG HUANGMA TECH
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