Preparation method of catalyst for preparing methacrylic acid through oxidation of methylacrolein

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

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

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Problems solved by technology

However, these publicly reported catalysts have disadvantage...

Method used

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  • Preparation method of catalyst for preparing methacrylic acid through oxidation of methylacrolein
  • Preparation method of catalyst for preparing methacrylic acid through oxidation of methylacrolein
  • Preparation method of catalyst for preparing methacrylic acid through oxidation of methylacrolein

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1 kg MoO 3 Add 15L of deionized water, stir for 30 minutes until uniform, and slowly add 283ml of phosphoric acid with a mass fraction of 17%. The temperature was raised to 105° C., condensed and refluxed for 3 hours, and the slurry turned into a yellow transparent solution A. After cooling to room temperature, unreacted solid particles were filtered off.

[0027] The above clear solution was warmed up to 85°C, and 52.6gV was added 2 o 5 , condensed to reflux, stirred for 2h, then added 23.2gCuO, 4.7gFe 2 o 3 , 9.4gZnO, condensed and refluxed, stirred for 2h. Finally add 225.7gCsNO 3 , Condensed to reflux, stirred for 3h. Stop condensation and reflux at 85°C, carry out concentrated drying, stop stirring when the viscosity of the slurry increases significantly, take out the semi-solid slurry, and place it in a blast drying oven at 80°C for 24 hours. The expression for the catalyst (ignoring hydrogen and oxygen) is:

[0028] PMo 12 V 1 Cs 2 Cu 0.5 Fe 0.1 Zn ...

Embodiment 2

[0032] The preparation method of solution A and V 2 o 5 The addition amount is as embodiment 1, adds 23.2gCuO, 5.0gMnO in the slurry after reaction 2 , 2.3gTiO 2 And 9.4gZnO, reflux condensation at 85°C for 2h. Finally add 282.1gCsNO 3 , Condensed to reflux, stirred for 3h. The expression of the catalyst is:

[0033] PMo 12 Cs 2.5 VCu 0.5 mn 0.1 Ti 0.05 Zn 0.1

[0034] The processing method of catalyst in subsequent steps is as embodiment 1. The evaluation method of the catalyst is as in Example 1, the conversion rate of MAL is 83.2%, and the selectivity of MAA is 80.5%.

Embodiment 3

[0036] The preparation method of solution A is as embodiment 1, in the filtered solution A, add V 2 o 5 78.9g, reflux condensed at 85°C, stirred for 2h, added CuO13.9g, 17.3gNiO, 2.2gCoO, refluxed condensed at 85°C, stirred for 2h, finally added 225.7gCsNO 3 , Reaction 3h. The expression of the catalyst is:

[0037] PMo 12 Cs 2 V 1.5 Cu 0.3 Ni 0.4 co 0.05

[0038] Catalyst follow-up treatment step is as embodiment 1, and the evaluation method of catalyzer is as embodiment 1, and the filling of catalyst is that the volume ratio of catalyst particle and quartz sand is 4:1, and the transformation rate of MAL is 80.7%, and the selectivity of MAA is 87.5% %.

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Abstract

The invention discloses a heteropolyacid and oxide compound catalyst for preparing methacrylic acid through oxidation of methylacrolein. The preparation method of the catalyst comprises the following steps: mixing phosphomolybdic acid and metallic oxide (such as vanadium pentoxide, ferric oxide, cupric oxide, nickel oxide, manganese dioxide, cobaltous oxide, titanium dioxide and zinc oxide) in a liquid phase step by step so as to form relatively large amount of active sites on the surface of heteropolyanion; adding caesium to obtain the catalyst. The catalyst has high catalytic activity for preparing methacrylic acid through oxidation of methylacrolein and has a long catalyst service life.

Description

technical field [0001] The invention relates to a method for preparing a composite catalyst of a heteropolyacid salt and an oxide. The prepared catalyst can be used for the oxidation of methacrolein to methacrylic acid, and has a high conversion rate of methacrolein and a high yield of methacrylic acid. selective. Background technique [0002] Methyl methacrylate (MMA) is an important chemical intermediate. At present, it has a huge market demand. The total production capacity of MMA in the world is more than 3.26 million tons per year, and the operating rate of factories producing MMA in the world is more than 80%. The Asian market is the main market that consumes MMA, among which China, Japan, South Korea and Taiwan have the largest demand, and the annual growth rate is about 5%. Therefore, new factories have been put into construction in recent years. [0003] MMA is mainly used in the production of plexiglass, and can also be polymerized with other monomers to form co...

Claims

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Application Information

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IPC IPC(8): B01J31/18C07C57/055C07C51/235
Inventor 张锁江周理龙王蕾闫瑞一韩军兴刁琰琰郑艳霞
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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