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Process for preparing methyl methacrylate according to aldol condensation method

A technology for the preparation of methyl methacrylate and aldol condensation, which is applied in the field of aldol condensation to prepare methyl methacrylate, can solve the problems of short catalyst life, loss, easy carbonization and deactivation, etc., and improve the single cycle Long service life, ensure online regeneration, and reduce the effect of carbon shrinkage

Active Publication Date: 2017-05-17
PUJING CHEM IND SHA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the alkali metal catalyst used in aldol condensation is prone to carbon formation and deactivation under high temperature conditions, thus resulting in a short service life of the catalyst. Under this condition, only the fluidized bed process application of Risun Chemical, such as CN102775302A, CN104513163A, is expected Catalyst activity recovery by continuous regeneration
However, compared with the fixed bed, the conversion rate of the fluidized bed is relatively low, and the strength of the catalyst is high, which is easy to cause catalyst pulverization and loss, and the solid particle catalyst will seriously wear the pipe and container.
At the same time, because formaldehyde is prone to side reactions and the effective utilization rate is not high, how to effectively improve the process conditions, prolong the service life of the catalyst, and increase the effective utilization rate of formaldehyde has become an important factor affecting production costs in the industrial scale-up process

Method used

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  • Process for preparing methyl methacrylate according to aldol condensation method
  • Process for preparing methyl methacrylate according to aldol condensation method
  • Process for preparing methyl methacrylate according to aldol condensation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Such as figure 1 As shown, both the X series and the Y series have three reactors, that is, n=3, therefore, the formaldehyde source is equally divided into 3 feeds. In this embodiment, methyl propionate and formaldehyde are used as raw materials, which are realized by connecting multiple reactors in series and in parallel, specifically including the following steps:

[0025] The X series reactors are put into reaction, and the Y series reactors are waiting to be put into use.

[0026] Methyl propionate 1 and the first strand of formaldehyde 2 are heated together by the heat exchanger HA1 and enter the first reactor A1 of the X series. The reaction temperature is 330°C, the reaction pressure is 0.6MPa, and the molar ratio of methyl propionate to formaldehyde is 10:1, the liquid hourly space velocity is 1.8 / h; the material reacted in the first reactor A1 of the X series is cooled by the heat exchanger EA1, and enters the second reactor A2 of the X series together with th...

Embodiment 2

[0043] As a comparison, the single-cycle service life of the catalyst after formaldehyde is not fed in stages, that is, the case of n=1, was investigated. The effect is as follows.

[0044] Reactor operating conditions are shown in the table below.

[0045] temperature reflex reaction pressure liquid hourly space velocity Ester-aldehyde ratio A1 reactor 345℃ 0.6MPa 0.6 / h 3.33:1

[0046] The results of the reactor reaction operation are shown in the table below.

[0047]

[0048] Note: Y MMA is the space-time yield of methyl methacrylate, g / (Kg.cat.h);

[0049] x HCHO is the effective conversion rate of formaldehyde, %.

[0050] The experimental results of embodiment 1 and embodiment 2 show, reduce catalyst load to original 1 / 3 (cluster 1.8 / h reduces to 0.6 / h), ester-aldehyde ratio reduces to 3.33:1 from 10:1, promptly guarantees that this reactor The unit processing capacity of the catalyst is consistent with the unit processing capacit...

Embodiment 3

[0052] Considering the case of n=5, the catalyst position is 20% Cs / SiO2.

[0053] The reaction operating conditions of each reactor of the X and Y series are shown in the table below.

[0054] A series temperature reflex reaction pressure liquid hourly space velocity Ester-aldehyde ratio A1 reactor 330℃ 0.6MPa 2.5 / h 15:1 A2 reactor 340℃ 0.5MPa 2.5 / h 14:1 A3 reactor 360℃ 0.4MPa 2.5 / h 13:1 A4 reactor 380℃ 0.3MPa 2.5 / h 12:1 A5 reactor 400℃ 0.2MPa 2.5 / h 11:1 B1 reactor 330℃ 0.6MPa 2.5 / h 15:1 B2 reactor 340℃ 0.5MPa 2.5 / h 14:1 B3 reactor 360℃ 0.4MPa 2.5 / h 13:1 B4 reactor 380℃ 0.3MPa 2.5 / h 12:1 B5 reactor 400℃ 0.2MPa 2.5 / h 11:1

[0055] Regeneration conditions are similar to Example 1.

[0056] According to above-mentioned conditions, the reaction result of each reactor is as follows:

[0057]

[0058]

[0059] Note: C MMA is the space-time yield of methy...

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Abstract

The invention relates to production of methyl methacrylate, in particular to a process for preparing methyl methacrylate according to an aldol condensation method, wherein the process is realized by connecting multiple reactors in series and in parallel. According to the process, the multiple reactors are connected in series, and a methyl propionate stream and multiple formaldehyde streams are fed, so that the effective conversion rate of a raw material formaldehyde can be well increased, and the single-cycle service life of a catalyst can be prolonged; the reactors of two series are connected in parallel, so that regeneration operation over the catalyst which is deactivated is realized without shutdown, and the whole system can run normally. Compared with the prior art, the process has the advantages that unfavorable factors such as the short service life of the aldol condensation catalyst and the high requirement on the catalyst during use of a fluidized bed are well eliminated, and the process has high application value and good economic benefits.

Description

technical field [0001] The invention relates to a production process of methyl methacrylate, in particular to a process for preparing methyl methacrylate by an aldol condensation method with long catalyst service life and high raw material utilization rate. Background technique [0002] Methyl methacrylate (MMA) is an important organic chemical raw material, mainly used in the production of plexiglass (PMMA), and also widely used in the production of resins, plastics, coatings, adhesives and various industrial additives. From 2009 to 2013, the production capacity and demand of my country's MMA industry both increased rapidly, and the production capacity increased from 420,000 tons / year to 590,000 tons / year, with an average annual compound growth rate of 7.0%; the demand increased from 470,000 tons / year to 690,000 tons / year, with an average annual compound growth rate of 8.0%. Domestically, demand is higher than production capacity growth. Driven by the downstream industry, ...

Claims

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Application Information

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IPC IPC(8): C07C67/343C07C69/54
CPCC07C67/343C07C69/54Y02P20/584
Inventor 骆念军贺俊陈长军
Owner PUJING CHEM IND SHA
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