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Method for preparing methyl methacrylate through aldol condensation of methyl propionate and formaldehyde

A technology of methyl methacrylate and methyl propionate, which is applied in the field of methyl methacrylate condensation between methyl propionate and formaldehyde aldol, can solve the problems of catalyst carbon deposition and deactivation, and achieve the enhancement of reaction regeneration process, The effect of convenient operation and simple equipment

Active Publication Date: 2019-02-01
SOUTHWEST RES & DESIGN INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention is to provide a kind of method for producing methyl methacrylate through aldol condensation of methyl propionate and formaldehyde, utilize internal circulating fluidized bed reactor to produce methyl methacrylate through aldol condensation, effectively solve the problem of propionic acid The problem of rapid carbon deposition and deactivation of the catalyst during the aldol condensation of methyl ester and formaldehyde, the production process is continuous and stable, the equipment is simple, and it is economical and efficient

Method used

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  • Method for preparing methyl methacrylate through aldol condensation of methyl propionate and formaldehyde
  • Method for preparing methyl methacrylate through aldol condensation of methyl propionate and formaldehyde
  • Method for preparing methyl methacrylate through aldol condensation of methyl propionate and formaldehyde

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Embodiment 1

[0028] The catalyst in this example is a silica carrier loaded with cesium and zirconium, the cesium loading is 10wt%, and the zirconium loading is 1wt%. Loaded on a silica carrier by the method, dried at 105°C for 5 hours, and calcined at 550°C for 5 hours to obtain a catalyst with a particle size of 0.10-0.15mm.

[0029] Experimental process: Catalyst performance evaluation was carried out in an internal circulating fluidized bed reactor. The diameter of the fluidized bed reactor was 25mm, the height was 500mm, and the catalyst loading was 10g. The thermocouple was extended to the middle of the fluidized bed material to monitor the reaction temperature in real time. The distributor distributes the air evenly. Feedstock flow rate 0.4mL / min, containing 44wt% methyl propionate, 43wt% methanol, 10wt% formaldehyde and 3wt% water, oxygen-containing fluidizing gas containing 2wt% O 2 N 2 +O 2 Mixed gas, the flow rate is 50L / h, the reaction temperature is 360°C, and the operation...

Embodiment 2

[0035] The catalyst in this example is a silica carrier loaded with cesium and zirconium, the cesium loading is 10wt%, and the zirconium loading is 1wt%. Loaded on a silica carrier by method, dried at 105°C for 5h, and calcined at 550°C for 5h to obtain a catalyst with a particle size of 0.38-0.83mm.

[0036] Experimental process: Catalyst performance evaluation was carried out in a fixed-bed tubular reactor. The inner diameter of the reaction tube was 25mm, and the catalyst loading was 10g. It was used after dilution. The thermocouple was extended to the middle of the catalyst bed to monitor the reaction temperature in real time. The raw material flow rate is 0.4mL / min, including 44wt% methyl propionate, 43wt% methanol, 10wt% formaldehyde and 3wt% water, the flow rate of carrier gas N2 is 5L / h, the reaction temperature is 360°C, and the operation is under normal pressure. During the experiment, the raw material was preheated at 250°C and then entered the catalytic bed with th...

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Abstract

The invention provides a method for preparing methyl methacrylate through aldol condensation of methyl propionate and formaldehyde, and belongs to the technical field of synthesis of methyl methacrylate. According to the method, methyl propionate, a formaldehyde source, methanol, water and oxygen-containing fluidized gas enter a fluidized bed reactor after pre-heating, and the oxygen in the oxygen-containing fluidized gas reacts with the carbon deposit on the surface of a catalyst so as to be consumed, such that an upper poor-oxygen zone and a lower oxygen-containing zone are formed; in the upper poor-oxygen zone, the methyl propionate reacts with the formaldehyde to form MMA, and carbon deposit is formed on the surface of the catalyst; in the lower oxygen-containing zone, the catalyst contacts the oxygen to burn off the carbon deposit on the surface; the catalyst continuously and cyclically flows in the fluidized bed; and the catalyst regenerated in the lower oxygen-containing zone cyclically returns to the upper poor-oxygen zone through the bed material so as to stably provide the fresh catalytic surface for the aldol condensation process, the carbon deposition catalyst returns to the lower oxygen-containing zone to start the next cycle, and the gas phase product is delivered to a subsequent separation unit. With the method of the present invention, the problem of rapid carbon deposition deactivation of the catalyst during the aldol condensation of methyl propionate and formaldehyde can be effectively solved.

Description

technical field [0001] The invention belongs to the technical field of methyl methacrylate synthesis, in particular to a method for preparing methyl methacrylate through aldol condensation of methyl propionate and formaldehyde. Background technique [0002] Methyl methacrylate (MMA) is an important organic chemical raw material, widely used in the production of organic glass (PMMA), PVC additives, coatings and other fields. The traditional industrial production technology of MMA is the acetone cyanohydrin method (ACH method). This route uses highly toxic hydrocyanic acid as a raw material, and is mostly produced with acrylonitrile equipment. The reaction process consumes a large amount of sulfuric acid, which requires high equipment materials and side effects. A large amount of ammonium bisulfate is produced, the process is long, and the pressure on environmental protection is high. At present, the newly developed MMA synthesis technology includes isobutylene method, ethyle...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/54C07C67/343B01J23/04
CPCB01J23/002B01J23/04B01J2523/00C07C67/343C07C69/54B01J2523/15B01J2523/41B01J2523/48Y02P20/584
Inventor 王光永毛震波贾绘如周拥华赵国强康仲良
Owner SOUTHWEST RES & DESIGN INST OF CHEM IND
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