Multi-component water-resistant catalyst for preparing carboxylic ester through aldehyde oxidative esterification, preparation and manufacturing of carboxylic ester

A technology of aldehyde oxidation esterification and oxidative esterification, which is applied in the field of new multi-component water-resistant catalysts, can solve the problems of unsatisfactory market demand and technology monopoly, and achieve high mechanical strength and chemical stability, low cost and simple preparation method Effect

Pending Publication Date: 2020-06-05
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] In order to better solve the above problems, foreign companies have conducted a serie...

Method used

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  • Multi-component water-resistant catalyst for preparing carboxylic ester through aldehyde oxidative esterification, preparation and manufacturing of carboxylic ester
  • Multi-component water-resistant catalyst for preparing carboxylic ester through aldehyde oxidative esterification, preparation and manufacturing of carboxylic ester
  • Multi-component water-resistant catalyst for preparing carboxylic ester through aldehyde oxidative esterification, preparation and manufacturing of carboxylic ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038]Mix 10g of 30% silica sol (pH=4.5), 3.0g of aluminum nitrate nonahydrate, 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 stirring and aging After 24 hours, a homogeneous solid solution suspension was obtained, and the water was removed by rotary evaporation, and vacuum-dried 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. After natural cooling, the Si-Mg-Al metal composite oxide carrier is obtained, in which the magnesium oxide, silicon oxide, and aluminum oxide in the composite oxide carrier combine to form a solid solution, which improves the acid and alka...

Embodiment 2

[0040] Mix 10g of 30% silica sol (pH=4.5), 1.8757g of aluminum nitrate nonahydrate, 0.2916g of magnesium hydroxide, 1.7812g of zirconium oxychloride, 2g of concentrated nitric acid with a concentration of 80%, and 60mL of deionized water at 25°C. The mixture was kept at 50° C. for 24 h with stirring to obtain a uniform solid solution suspension, which was evaporated to remove water, and dried in 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. After natural cooling, the Si-Mg-Al-Zr metal composite oxide carrier is obtained.

Embodiment 3

[0042] Mix 10g of 30% silica sol (pH=4.5), 1.8757g of aluminum nitrate nonahydrate, 4.33g of lanthanum nitrate hexahydrate, 3g of concentrated nitric acid with a mass concentration of 60%, and 100mL of deionized water, and keep the mixture at 50°C for 24h with stirring to obtain a uniform The 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. After natural cooling, the Si-La-Al metal composite oxide carrier is obtained.

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Abstract

The invention relates to a novel multi-component water-resistant catalyst for preparing carboxylic ester through aldehyde oxidative esterification, preparation of the novel multi-component water-resistant catalyst and preparation of the carboxylic ester. The catalyst is of a core-shell structure and contains a precious metal, cobalt, nickel, silicon, aluminum and one or more than two of lanthanideseries, actinide series elements, cesium, magnesium, calcium, yttrium, vanadium, scandium, cerium, gallium, zirconium, niobium, manganese, lead, bismuth and antimony. Through use of the catalyst, (methyl)acrolein and primary alcohol are subjected to a one-step oxidative esterification reaction to generate the carboxylic ester under the conditions that the reaction pressure is 2-50 bar, the reaction temperature is 40-160 DEG C, and oxygen sources such as oxygen, air or an oxygen-containing mixed gas exist. Compared with an existing catalyst, the catalyst is good in water resistance, high mechanical strength and chemical stability can still be kept in the long-time reaction process, and the catalyst has the advantages of being simple in preparation method, low in cost and the like.

Description

technical field [0001] The invention provides a novel multi-component water-resistant catalyst for preparing carboxylate by oxidative esterification of aldehyde, and a manufacturing method of using the catalyst as a catalyst for producing unsaturated carboxylate. Background technique [0002] Methyl methacrylate is a widely used chemical raw material. At present, the main processes for industrial production of methyl methacrylate include traditional acetone cyanohydrin method and isobutylene oxidation method. Compared with the acetone cyanohydrin method, the isobutylene oxidation method uses abundant C4 resources in refineries as raw materials, and the by-product is water, which has a high degree of environmental protection and has attracted more and more people's attention. [0003] The advantage of the direct methyl ester method in the isobutene oxidation method is that unsaturated aldehydes can be oxidized and esterified in one step to generate unsaturated carboxylic acid...

Claims

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Application Information

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IPC IPC(8): B01J23/89C07C67/39C07C69/54
CPCB01J23/002B01J23/892B01J23/894B01J23/8946B01J23/898C07C67/39B01J2523/00C07C69/54B01J2523/19B01J2523/22B01J2523/31B01J2523/41B01J2523/845B01J2523/847B01J2523/3706B01J2523/15B01J2523/23B01J2523/35
Inventor 高爽李国松王连月吕迎
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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