Method for preparing methyl methacrylate by aldol condensation of methyl acetate and formaldehyde

A technology of methyl methacrylate and methyl acetate, which is applied in the field of methyl methacrylate preparation, can solve the problems of high energy consumption, complex process, large amount of sewage, etc., and achieve enhanced reaction regeneration process, simple equipment, and improved utilization efficiency effect

Active Publication Date: 2019-01-18
SOUTHWEST RES & DESIGN INST OF CHEM IND
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It is also reported that domestic production capacity of polyvinyl alcohol (PVA) will exceed 1.7 million tons in 2018, and nearly 2.8 million tons of methyl acetate will be produced as a by-product. The PVA industry generally adopts the technical scheme of hydrolyzing me

Method used

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  • Method for preparing methyl methacrylate by aldol condensation of methyl acetate and formaldehyde
  • Method for preparing methyl methacrylate by aldol condensation of methyl acetate and formaldehyde
  • Method for preparing methyl methacrylate by aldol condensation of methyl acetate and formaldehyde

Examples

Experimental program
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Embodiment 1

[0031] The aldol condensation catalyst is a silica carrier loaded with cesium and zirconium, the cesium loading is 10wt%, and the zirconium loading is 1wt%. The catalyst was prepared by loading it on a silica carrier, drying at 105°C for 5 hours, and calcining at 550°C for 5 hours. The particle size was 0.10-0.15mm. The hydrogenation catalyst is a strong base anion exchange resin D261 loaded with 0.63wt% palladium. First, 2 g of the carrier is swelled in methanol for 2 hours, and PdCl is added 2 methanol solution, react until the color of the mother liquor becomes colorless, add NaBH 4 Restored for 6 hours, suction filtered, washed and dried for later use.

[0032] Aldol condensation experiment process: Catalyst performance evaluation is carried out in an internal circulating fluidized bed reactor. The diameter of the fluidized bed reactor is 25mm, the height is 500mm, and the catalyst loading is 10g. The thermocouple is extended to the middle of the fluidized bed material to...

Embodiment 2

[0040] The test and analysis methods are the same as in Example 1, only the aldol condensation reaction pressure is changed to 1.0 MPa.

[0041] The experimental results are: the conversion rate of methyl acetate is 21%, the selectivity of methyl acrylate is 90%; the conversion rate of methyl propionate is 32%, and the selectivity of MMA is 91%.

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Abstract

The invention provides a method for preparing methyl methacrylate by aldol condensation of methyl acetate and formaldehyde, and belongs to the technical field of preparation of methyl methacrylate. The method comprises the following steps: preheating methyl acetate, returned methyl propionate, a formaldehyde source, methanol, water and oxygen-containing fluidized gas as materials, enabling the materials to enter a fluidized-bed reactor, under the action of a catalyst bed material in an internal-circulation fluidized bed, generating aldol condensation reaction to produce MMA, and finishing regeneration of a catalyst. The method provided by the invention has the beneficial effects that by utilization of the characteristic of internal-circulation movement of the fluidized-bed material, a little amount of oxygen is introduced at the lower part of the fluidized bed to form a local oxygen-containing area to carry out periodical regeneration on the catalyst bed material, so that the serious side reaction in the presence of a large amount of oxygen and insufficient and non-uniform regeneration of the fluidized-bed material are avoided, regeneration of the catalyst in the aldol condensationreaction is realized, the catalyst can maintain high activity for a long term, and the catalyst utilization efficiency is improved; the problems of inactivation and short service life of a catalyst due to easy carbon deposition in the aldol condensation process of the methyl acetate, the methyl propionate and the formaldehyde are solved.

Description

technical field [0001] The invention belongs to the technical field of methyl methacrylate preparation, in particular to a method for preparing methyl methacrylate through aldol condensation of methyl acetate 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 (C4 meth...

Claims

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Application Information

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IPC IPC(8): C07C67/343C07C69/54
CPCC07C67/343C07C69/54Y02P20/584
Inventor 王光永毛震波李荣王莉李军应理
Owner SOUTHWEST RES & DESIGN INST OF CHEM IND
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