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Process for preparing unsaturated esters proceeding from aldehydes by direct oxidative esterification

A technology of oxidative esterification and methacrolein, applied in chemical instruments and methods, preparation of carboxylic acid esters, preparation of organic compounds, etc., can solve the problems of catalyst short life, achieve catalyst service life, improve yield, The effect of suppressing side effects

Active Publication Date: 2016-06-29
ROHM G M B H
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  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

[0018] - Catalyst leaching and the resulting relatively short lifetime

Method used

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  • Process for preparing unsaturated esters proceeding from aldehydes by direct oxidative esterification
  • Process for preparing unsaturated esters proceeding from aldehydes by direct oxidative esterification

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0058] Catalyst preparation

[0059] Catalyst 1 (on SiO 2 -Al 2 o 3 -0.9%Au-1.1%NiO on MgO, 1.16-2.36mm balls)

[0060] A solution of 37.5g of aluminum nitrate nonahydrate, 25.6g of magnesium nitrate hexahydrate and 5.4g of 60% nitric acid in 100ml of water was mixed with 108g of SiO at room temperature. 2The carrier (FujiSilicia, CariactQ-10, 1.16-2.36 mm balls) was mixed. The mixture was stirred at 50°C for 24 hours, then cooled to room temperature, dried at 130°C and calcined at 300 to 600°C for a total of 10 hours. 30g of this SiO 2 -Al 2 o 3 - The MgO carrier is mixed with 100ml of water and heated to 90°C. After 15 minutes, 1.64 g of nickel nitrate hexahydrate and 530 mg of gold acid (HAuCl 4 ) in 100 ml of water was added to the mixture at 90° C. within 30 minutes. After stirring for a further 30 minutes at 90° C., the mixture was cooled and the solid separated, then stirred three times at 20° C. with 100 ml of fresh water for 5 minutes each and filtered. The...

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Abstract

The present invention relates to a process for preparing methyl methacrylate by a direct oxidative esterification of methacrolein with oxygen and methanol, which is conducted in the liquid phase at a pressure of 2 to 100 bar with a gold catalyst. According to the invention, the liquid phase is withdrawn continuously from the reactor and optionally enriched with oxygenous gas, the pH, after the withdrawal, is adjusted to a pH between 5 and 9 by means of addition of a basic solution and this liquid phase is conducted back into the reactor again to an extent of at least 50%.

Description

technical field [0001] The present invention relates to a process for the preparation of methyl methacrylate by direct oxidative esterification of methacrolein. [0002] Methyl methacrylate is used extensively in the preparation of polymers and copolymers with other polymerizable compounds. In addition, methyl methacrylate is an important synthetic unit for a number of specialty esters based on methacrylic acid (MAS), which can be prepared by transesterification with appropriate alcohols. [0003] This has led to great interest in the simplest possible, economically feasible and environmentally friendly preparation methods for this starting material. Background technique [0004] Methyl methacrylate (MMA) is currently mainly prepared starting from hydrogen cyanide and acetone via acetone cyanohydrin (ACH) formed as a core intermediate. The disadvantage of this method is that very large quantities of ammonium sulfate are obtained, the workup of which involves very high cost...

Claims

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Application Information

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IPC IPC(8): C07C67/39
CPCY02P20/582C07C67/39C07C69/54B01J8/008B01J23/52C07C2523/52B01J35/40C07C67/42B01J35/19B01J35/23B01J23/02B01J23/892
Inventor S·克里尔A·黎金T·巴尔杜弗R·波格哈德特A·泰普瑞斯M·格勒姆平
Owner ROHM G M B H
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