A kind of supported oxidative esterification catalyst and its preparation method and application

A technology of oxidative esterification and catalyst, which is applied in the direction of metal/metal oxide/metal hydroxide catalyst, physical/chemical process catalyst, carboxylate preparation, etc., which can solve the problem of high palladium content, failure to meet market demand, and low efficiency and other issues, to achieve the effects of structural stability, good cycle stability, catalytic activity and high selectivity

Active Publication Date: 2019-11-22
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But these methods, the main active component palladium content of catalyzer is high, and efficiency is lower
In addition, Asahi Kasei Company CN103097296 reported a series of silica-based materials and its impregnation method to support noble metal Au for one-step oxidative esterification to prepare methyl methacrylate, with a conversion rate of 40-60% and a selectivity of about 91%, but due to technical Monopolies cannot meet market demand

Method used

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  • A kind of supported oxidative esterification catalyst and its preparation method and application
  • A kind of supported oxidative esterification catalyst and its preparation method and application
  • A kind of supported oxidative esterification catalyst and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Preparation of catalyst:

[0037] Mix 3g of 200-300 mesh column chromatography silica gel, 3.0g of aluminum nitrate, 1.96g of magnesium hydroxide, 3g of concentrated nitric acid with a concentration of 65%, and 60mL of deionized water at 25°C, and keep the mixture at 50°C for 24h with stirring to obtain The homogeneous solid solution suspension was evaporated to remove water, and dried under vacuum at 80°C to obtain a white powdery solid. The solid was placed in a tube furnace and roasted under a nitrogen gas temperature program. Starting at 30°C, the temperature was raised to 300°C at a rate of 2.25°C / min, kept at 300°C for 4 hours, and then started at 300°C, and the temperature was raised at a rate of 2.5°C / min. To 600°C, keep at 600°C for 4h. SiO obtained after natural cooling 2 -MgO-Al 2 o 3 Metal composite oxide carrier, in which magnesium oxide, silicon oxide and aluminum oxide in the composite oxide carrier combine to form a solid solution, which improves the...

Embodiment 2

[0042] Mix 3g of 200-300 mesh column chromatography silica gel, 3.0g of calcium nitrate, 1.96g of magnesium hydroxide, 3g of concentrated nitric acid with a concentration of 80%, and 60mL of deionized water at 25°C, and keep the mixture at 50°C for 24h with stirring to obtain The homogeneous solid solution suspension was evaporated to remove water, and dried under vacuum at 80°C to obtain a white powdery solid. Put the solid in a tube furnace, and roast it under nitrogen with programmed temperature rise, heating at 30-300°C for 3 hours (heating rate 1.5°C / min), keeping at 300°C for 4 hours, heating at 300-600°C for 3 hours (heating rate 1.7°C / min) , keep at 600°C for 4h. SiO obtained after natural cooling 2 - MgO-CaO metal composite oxide support.

[0043] Add 1 g of SiO to the reactor sequentially 2 -MgO-CaO carrier, 1.6g of hexamethyltetramine, 63.5mg of chloroauric acid, 0.18g of cobalt nitrate, 0.050g of cerium nitrate, and 200mL of deionized water were mixed evenly, st...

Embodiment 3

[0046] Mix 3g of 200-300 mesh column chromatography silica gel, 5g of magnesium nitrate, 3g of concentrated nitric acid with a mass concentration of 60%, and 80mL of deionized water, and keep the mixture at 50°C for 24 hours with stirring to obtain a uniform solid solution suspension. °C and dried under vacuum to obtain a white powdery solid. Put the solid in a tube furnace, and roast it under nitrogen with programmed temperature rise, heating at 30-300°C for 3 hours (heating rate 1.5°C / min), keeping at 300°C for 4 hours, heating at 300-600°C for 3 hours (heating rate 1.7°C / min) , keep at 600°C for 4h. SiO obtained after natural cooling 2 - MgO metal composite oxide support.

[0047] Add 1 g of SiO to the reactor sequentially 2 - MgO carrier, 2.0g hexamethyltetramine, 63.5mg chloroauric acid, 0.18g cobalt nitrate, 0.03g ytterbium nitrate, 70mL deionized water were mixed evenly, stirred and reacted at 80°C for 4h, after the mixture was cooled to room temperature, Press filt...

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Abstract

The object of the present invention is to provide a supported oxidative esterification catalyst and its preparation method and application, wherein the supported oxidative esterification catalyst is made of Al 2 O 3 , one or two or three oxides of MgO, CaO and SiO 2 The composite oxide prepared as a raw material is used as a carrier, gold (Au) and cobalt (Co) are used as active components, and lanthanide elements are supported. The method is to support active components and the like on a carrier through a chemical uniform precipitation method to prepare an efficient and stable oxidative esterification catalyst. In addition to the advantages of high conversion rate and good selectivity, the method also has the characteristics of low consumption of precious metals, high utilization rate and good stability. The catalyst is used for the catalytic synthesis of methyl methacrylate, and its catalytic activity and selectivity exceed those of the existing catalysts. The conversion rate of methacrolein is up to 100%, and the selectivity of methyl methacrylate is up to 97%. The post-treatment cost of other by-products acetal and carboxylic acid. The catalyst has good cycle stability.

Description

technical field [0001] The invention belongs to the field of oxidative esterification catalysts, and in particular relates to a supported oxidative esterification catalyst and its preparation method and application. Under the conditions of the catalyst of the present invention, methacrolein and methanol are used as raw materials in the presence of an oxidant Direct oxidative esterification produces methyl methacrylate. Background technique [0002] Methyl methacrylate is an important organic chemical raw material with a wide range of uses. It is mainly used as a polymerized monomer to produce its polymers and copolymers, and can also be used to produce high-carbon methacrylate through transesterification. Its polymer is a plastic material with excellent transparency, so it is often called plexiglass, and has excellent characteristics such as excellent weather resistance. It is also used in the production of acrylic resin, molding compound, acrylic paint, PVC additives, Adh...

Claims

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Application Information

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IPC IPC(8): B01J23/89C07C67/39C07C69/54
CPCB01J23/002B01J23/894B01J2523/00C07C67/39B01J2523/19B01J2523/22B01J2523/31B01J2523/3706B01J2523/41B01J2523/845B01J2523/23B01J2523/3712B01J2523/3787B01J2523/14C07C69/54
Inventor 高爽王连月李国松王闯李文双袁龙
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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