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Method for separating methyl-acrolein in methyl-methyl acrylate

A technology of methyl methacrylate and methacrolein, which is applied in the field of absorption and separation of volatile polymerized monomers, can solve the problems that cannot meet the requirements of the second-step oxidative esterification reaction, MAL separation is difficult, and can not meet the requirements, so as to reduce the Equipment investment and operating costs, the effect of solving high water content and easy operation

Active Publication Date: 2006-08-16
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This makes the separation of MAL in the reaction product of the first step more difficult.
The method proposed by U.S.Pat.No.3,957,880 is to absorb with ethanol, then carry out extractive distillation with water as extractant, what obtains like this is the azeotrope of water and methacrolein, can not satisfy the second step oxidative esterification reaction Require
The method proposed by U.S.Pat.No.2,514,966 is to absorb with water, but the obtained MAL cannot meet the requirements of the second step oxidative esterification reaction
U.S.Pat.No.5,969,178 reported that the four-column combination of water washing, methanol drying, methanol absorption and rectification recovery has been industrialized, but the process is complex

Method used

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  • Method for separating methyl-acrolein in methyl-methyl acrylate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0006] Embodiment 1: a kind of technological operation parameter of MAL separation and purification in the product gas mixture

[0007] The reaction product gas stream is flowed into the water absorption tower, and the number of trays is 10, operated at normal pressure, 110 ° C of the inlet product gas temperature, and the gas composition is 0.22% of IB (isobutylene), O 2 1.51%, N 2 68.11%, H 2 O 12.30%, CO 2 4.25%, CO 1.77%, MAL 10.97%, MAA 0.50%, C 3 h 6 O 0.1%, mass flow rate is 15.44kg / h, absorbing with 2°C water 42.00kg / h, tower bottom temperature 44.6°C, tower top temperature 2.3°C. The composition of the overhead gas after absorption is IB 0.03%, O 2 1.96%, N 2 89.6%, H 2 O 0.5%, CO 2 5.5%, CO 2.32%, MAL trace, C 3 h 6 O trace.

[0008] Put the MAL aqueous solution and methanol into the rectification tower. The rectification tower has 25 plates. It operates under normal pressure. The feeding position is 13 plates. The temperature of the inlet material i...

Embodiment 2

[0009] Embodiment 2: another kind of technological operation parameter of MAL separation and purification in the product gas mixture

[0010] The gas flow of the reaction product flows into the water absorption tower, the number of trays is 10, the normal pressure is operated, the inlet product gas temperature is 130°C, and the gas composition is IB 0.22%, O 2 1.51%, N 2 68.11%, H 2 O 12.30%, CO 2 4.25%, CO 1.77%, MAL 10.97%, MAA 0.50%, C 3 h 6 O 0.1%, the mass flow rate is 15.44kg / h, absorbing with 20°C water 48.00kg / h, the temperature of the bottom of the tower is 52.0°C, and the temperature of the top of the tower is 22.3°C. The composition of the overhead gas after absorption is IB 0.20%, O 2 1.97%, N 2 85.20%, H 2 O 1.7%, CO 2 5.21%, CO2.12%, MAL 3.4%, C 3 h 6 O trace.

[0011] Put the MAL aqueous solution and methanol into the rectification tower. The rectification tower has 25 plates. It operates under normal pressure. The feeding position is 13 plates. ...

Embodiment 3

[0012] Embodiment 3: the third process operation parameter of MAL separation and purification in product gas mixture

[0013] The gas flow of the reaction product flows into the water absorption tower, the number of trays is 10, the operating pressure is 2atm, the inlet product gas temperature is 120°C, and the gas composition is IB 0.22%, O 2 1.51%, N 2 68.11%, H 2 O 12.30%, CO 2 4.25%, CO 1.77%, MAL 10.97%, MAA 0.50%, C 3 h 6 O 0.1%, the mass flow rate is 15.44kg / h, absorbing with 42.00kg / h of water at 10°C, the temperature of the bottom of the tower is 52.2°C, and the temperature of the top of the tower is 10.5°C. The tower top gas composition after absorbing is IB trace, O 2 2%, N 2 90.00%, H 2 O 0.4%, CO 2 5.21%, CO 2.30%, MAL 0.23%, C 3 h 6 O 0.004%.

[0014] Put the MAL aqueous solution and methanol into the rectification tower, the rectification tower has 25 plates, operates under normal pressure, the feed position is 10 plates, the inlet material temp...

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Abstract

Separation of methylacrolein in methyl methacrylate production is carried out by reacting to obtain mixed gas containing MAL, cooling and absorbing for MAL by 0~60 degrees C water, azeotropic rectifying with methanol as azeotropic agent, and separating MAL from mixed gas to obtain azeotropic mixture of MAL and methanol with water content lower 500pp. It is simple.

Description

Technical field: [0001] The invention belongs to the technical field of absorption and separation of volatile polymerized monomers, and in particular relates to the technology and method of separating methacrolein to synthesize methyl methacrylate. Background technique: [0002] Methyl methacrylate (MMA) is widely used in national defense, construction and fine chemicals, such as the production of plexiglass, plastic modification, production of advanced coatings and adhesives, etc. Although the traditional acetone cyanohydrin method for producing MMA has a mature process, the price of raw materials is relatively high, and the use of highly toxic drugs and strong acids has caused serious problems such as environmental pollution and human poisoning. In recent years, various countries have launched researches on new process routes for MMA production, among which C 4 The process route of producing MMA from distillate as raw material is attractive in terms of environmental prote...

Claims

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Application Information

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IPC IPC(8): C07C45/84C07C47/22C07C67/00C07C69/54
Inventor 张香平闫瑞一张锁江成卫国王蕾
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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