Catalyst for preparing methacrylic acid by oxidation of methylacrolein and preparation method of catalyst

A technology of methacrylic acid and methacrolein, which is applied in the preparation of organic compounds, catalysts for physical/chemical processes, and preparation of carboxylate, which can solve the problems of short catalytic life and low space-time yield of products

Active Publication Date: 2014-08-27
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the catalysts reported so far still have problems such as low space-time yield of products and short catalytic life, so it is necessary to further improve the catalytic performance.

Method used

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  • Catalyst for preparing methacrylic acid by oxidation of methylacrolein and preparation method of catalyst
  • Catalyst for preparing methacrylic acid by oxidation of methylacrolein and preparation method of catalyst
  • Catalyst for preparing methacrylic acid by oxidation of methylacrolein and preparation method of catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1KgMoO 3 , V 2 o 5 57.4g, 17%H 3 PO 4 364.1 g was added into 15 L of deionized water, stirred, the temperature was raised to 105°C, stirred, condensed and refluxed for about 3 hours until the solution became orange-red solution A. Unreacted solids were filtered off. Take 1 / 3 of filtrate A, namely 5.1L, add CsNO 3 164.1 g, stirred vigorously at room temperature for 2 hours, centrifuged after the reaction was complete, poured out the supernatant, solid precipitate A, washed with deionized water.

[0029] Add the precipitate A to 1 / 3 of the solution A, slowly add 129.6ml of 25% ammonia water dropwise under vigorous stirring, and continue stirring for 2h after the dropwise addition is completed. The resulting solution was then centrifuged to obtain solid precipitate B, which was washed with deionized water.

[0030] Add the precipitate B to the remaining 1 / 3 solution A, raise the temperature to 85°C while stirring, and add 59.4g Cu(NO 3 ) 2 , 25.5gFe(NO 3 ) 3 , 1...

Embodiment 2

[0035] The preparation method of Solution A, Precipitation A and Precipitation B is as in Example 1. Precipitation B is added to the remaining 1 / 3 Solution A, and the temperature is raised to 85°C while stirring, and 59.4g Cu (NO 3 ) 2 , 25.5gFe(NO 3 ) 3 , 38.3gMn(NO 3 ) 4 and 2.5gTiO 2 Add 1.2 L of deionized water to make a solution, slowly drop it into the suspension, react for 2 hours after the dropwise addition, concentrate and dry, and finally obtain the catalyst precursor B. Its composition expression is:

[0036] (Cu 1.5 Fe 0.5 mn 0.6Ti 0.15 PMo 11 VO 40 )[(NH 4 ) 4 PMo 11 VO 40 ](Cs 4 PMo 11 VO 40 )

[0037] Catalyst post-treatment and evaluation methods are as in Example 1. The selectivity was 83.5% for MAL and 88.4% for MAA.

Embodiment 3

[0039] The preparation method of Solution A, Precipitation A and Precipitation B is as in Example 1. Precipitation B is added to the remaining 1 / 3 Solution A, and the temperature is raised to 85°C while stirring, and 59.4g Cu (NO 3 ) 2 , 25.5gFe(NO 3 ) 3 , 23.1gCo(NO 3 ) 2 and 6.0gZn(NO 3 ) 2 Add 1.2 L of deionized water to make a solution, slowly drop it into the suspension, react for 2 hours after the dropwise addition, concentrate and dry, and finally obtain the catalyst precursor B. Its composition expression is:

[0040] (Cu 1.8 Fe 0.6 co 0.6 Zn 0.15 PMo 11 VO 40 )[(NH 4 ) 4 PMo 11 VO 40 ](Cs 4 PMo 11 VO 40 )

[0041] Catalyst post-treatment and evaluation methods are as in Example 1. The selectivity was 82.3% for MAL and 89.7% for MAA.

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Abstract

The invention relates to a heteropolyacid catalyst for preparing methacrylic acid by oxidation of methylacrolein and a preparation method of the catalyst. According to the catalyst, phosphorus molybdenum cesium metavanadate or phosphorus molybdenum ammonium metavanadate with high thermal stability serves as a kernel; phosphorus molybdenum ammonium metavanadate or phosphorus molybdenum cesium metavanadate serves as a secondary outer layer; phosphorus molybdenum vanadate with a catalytic active site coats the outermost layer. The catalyst has high catalytic activity and long catalytic life in preparation of the methacrylic acid by gas-phase oxidation of the methylacrolein.

Description

technical field [0001] The invention relates to a catalyst for the oxidation of methacrolein to methacrylic acid and a preparation method thereof. The catalyst obtained by the method has a core-shell structure, and the prepared catalyst is used for the oxidation of methacrolein to methacrylic acid, and has high The conversion of methacrolein and the selectivity of methacrylic acid. Background technique [0002] Methyl methacrylate (MMA) is an important industrial intermediate, mainly used in the manufacture of plexiglass, coating additives, medical polymer material copolymers, etc. At present, the demand for MMA is still growing, especially in China, Japan, South Korea and Taiwan, where the demand for MMA is growing rapidly at a rate of 5% to 10%. At present, apart from Japan, the production process of MMA in East Asia is mostly based on the acetone cyanohydrin (ACH) method, which requires the use of highly toxic hydrocyanic acid and produces solid waste, which does not mee...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/18C07C57/055C07C51/235
Inventor 张锁江周理龙王蕾闫瑞一刁琰琰韩军兴郑艳霞
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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