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Production of methyl a-methacrylate with methanal as raw material

A technology of methyl methacrylate and methacrolein, which is applied in the field of preparation of methyl methacrylate, can solve the problems of high reaction temperature, complicated process, and easy deactivation of catalysts, and achieve high conversion rate, environmental friendliness, Inexpensive to prepare

Inactive Publication Date: 2007-11-21
TIANJIN UNIV
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  • Description
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AI Technical Summary

Problems solved by technology

However, in the isobutene method, the oxidation of isobutene to methacrolein has the disadvantages of high reaction temperature, complicated process, and easy deactivation of the catalyst.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] Weigh the specific surface area of ​​500m 2 / g, 20g of styrene-divinylbenzene copolymer resin with an average pore diameter of 18nm (the resin was purchased from Nankai University Chemical Plant), immersed in ethanol for 4 hours at 25°C, filtered and placed in an oven at 60°C Dry and set aside. Dissolve 1.00g of palladium chloride, 0.462g of bismuth chloride, 0.192g of lead nitrate, and 0.866g of iron nitrate in 60ml of N.N-dimethylformamide at 70°C. Then pour the solution into the styrene-divinylbenzene copolymer carrier, stir to make the carrier impregnated evenly, after impregnating for 6 hours, place it in an oven at 90° C. for 6 hours to dry. After drying, immerse in 60ml of 0.01g / ml NaOH methanol solution for 4 hours, and dry completely under the same condition of 90°C. Finally place in hydrogen reducer, hydrogen flow rate 40ml / min, reduce 10 hours under the condition of 200 ℃, the catalyst that obtains contains Pd3%, Bi1.5%, Pb0.6%, Fe0.6% (relative carrier mas...

Embodiment 2

[0013] The preparation of methacrolein and catalyst is the same as in Example 1.

[0014] Add 2.0g of the catalyst prepared above, 3.28g of methacrolein and 60g of methanol into a reactor equipped with a reflux condenser, the oxygen flow rate of the reactor is 10mL / min, and react at 50°C for 4 hours, the conversion rate of methacrolein The selectivity to methyl methacrylate was 90.5%, and the selectivity to methyl methacrylate was 98.2%.

Embodiment 3

[0016] The preparation of methacrolein and catalyst is the same as in Example 1.

[0017] Add 2.5g of the catalyst prepared above, 3.28g of methacrolein and 60g of methanol into a reactor equipped with a reflux condenser, the oxygen flow rate of the reactor is 10mL / min, react at 50°C for 6 hours, the conversion of methacrolein The selectivity to methyl methacrylate was 96.9%, and the selectivity to methyl methacrylate was 97.3%.

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PUM

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Abstract

Production of methyl-methyl acrylate from methanal is carried out by reacting methanal with propanal in diethylamine muriate solution at 40-45 degree to obtain methyl-acryl, mixing methyl-acryl with methanol in proportion of 30-50:1, adding them into reactor, adding into 2.0-4.0% catalyst, inducing into oxygen at 40-60 degree and flow 10 ml / min, reacting for 4-6 hrs and synthesizing to obtain final product. The catalyst carrier is styrene-divinylbenzene polymer organic resin, which consists of palladium 2-5 wt%, bismuth 0-3 wt%, lead 0.3-1 wt% and iron 0.3-1 wt%. It's cheap, has friendly reactive environment, better selectivity and conversion rate.

Description

technical field [0001] The invention belongs to the preparation technology of methyl methacrylate, in particular to a method for preparing methyl methacrylate with formaldehyde as raw material. Background technique [0002] At present, the methods for producing methyl methacrylate mainly include acetone cyanohydrin method and isobutylene method. Because the acetone cyanohydrin method uses highly toxic hydrocyanic acid as a raw material, and excessive concentrated sulfuric acid is used in the production process, it has the disadvantages of high requirements for equipment materials and a large investment in environmental protection equipment. The isobutylene method is an environmentally friendly preparation method. The method generally consists of three or two-step reactions. The three-step reaction is to first oxidize isobutene to methacrolein, and then oxidize methacrolein to produce methacrylic acid, formaldehyde Acrylic acid is esterified with methanol to obtain methyl me...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/44C07C69/54C07C47/22
Inventor 汪宝和李云丽井欣张宗礼张德立朱璟吉鹏举
Owner TIANJIN UNIV
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