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Preparation method of catalyst for synthesizing methacrylic acid

A methacrylic acid and catalyst technology, which is applied in the preparation of organic compounds, the preparation of carboxylate, chemical instruments and methods, etc., can solve the problems of difficult industrial application, shortened service life of catalysts, and expensive ceramic whiskers.

Active Publication Date: 2012-07-11
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

There are some patents, such as patents CN1274619, CN1461236, etc., by introducing arsenic into the catalyst composition to improve its activity and selectivity, but the service life of the catalyst is shortened due to the sublimation of arsenic
Catalysts based on phosphomolybdovanadium heteropolyacids and their salts still have the disadvantages of low mechanical strength and poor thermal stability. Some patents improve this. For example, in patent JP55079340, metal sulfate is added to the catalyst to improve the mechanical strength. It has a certain effect, but the catalyst does not show good catalytic activity. The patent JP59183832 adds ceramic whiskers such as silicon carbide to the catalyst to improve the mechanical strength, but it is difficult to industrialize the application due to the high price of ceramic whiskers.

Method used

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  • Preparation method of catalyst for synthesizing methacrylic acid
  • Preparation method of catalyst for synthesizing methacrylic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add 158.334 grams of molybdenum trioxide and 9.1 grams of vanadium pentoxide into 1500 grams of distilled water, heat to 80°C and stir for 2 hours, then add 86.47 grams of 17% phosphoric acid, and reflux for 36 hours under stirring to obtain solution A. Dissolve 8.768 grams of 1-butyl-3-methylimidazole in 300 grams of distilled water to obtain solution B, add B to A under stirring at 60°C, and age at a constant temperature for 2 hours, take 19.491 grams of cesium nitrate, nitric acid trihydrate 7.248 grams of copper, 12.12 grams of ferric nitrate nonahydrate, and 4.3425 grams of cerium nitrate hexahydrate were dissolved in 700 grams of distilled water to obtain solution C. Under stirring at 60 ° C, C was added to the mixed solution formed by B and A, and aged at a constant temperature for 6 hours , then evaporate the water to concentrate the slurry to obtain a solid, dry it at 110°C for 12 hours, press it into a cylinder with a diameter of 5mm and a height of 4.5mm, calc...

Embodiment 2

[0024] Add 158.334 grams of molybdenum trioxide and 11.698 grams of ammonium metavanadate into 1500 grams of distilled water, heat to 80°C and stir for 2 hours, then add 69.176 grams of 17% phosphoric acid, and reflux for 6 hours under stirring to obtain solution A. Dissolve 4.384 grams of 1-butyl-3-methylimidazole in 300 grams of distilled water to obtain solution B, add B to A under stirring at 60°C, and age at a constant temperature for 2 hours, take 19.491 grams of cesium nitrate, nitric acid trihydrate 12.08 grams of copper, 8.08 grams of iron nitrate nonahydrate, and 4.3425 grams of cerium nitrate hexahydrate were dissolved in 700 grams of distilled water to obtain solution C. Under stirring at 60 ° C, C was added to the mixed solution formed by B and A, and aged at constant temperature for 6 hours , then evaporate the water to concentrate the slurry to obtain a solid, dry it at 110°C for 12 hours, press it into a cylinder with a diameter of 5mm and a height of 4.5mm, cal...

Embodiment 3

[0036] Except that 4.024 g of 1-butyl-3-methylimidazole nitrate was used to replace 4.384 g of 1-butyl-3-methylimidazole bromide when preparing solution B, other preparation steps were the same as in Example 2.

[0037] Under the same conditions as in Example 1, the catalyst was used for the gas-phase oxidation of methacrolein to methacrylic acid, and the results are listed in Table 1.

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Abstract

The invention relates to a preparation method of a catalyst for synthesizing methacrylic acid. The preparation method comprises the following steps: preparing a heteropoly compound catalyst by adopting an ionic liquid and metal salt step-by-step precipitation method; performing a reaction on a molybdenum-containing compound, a vanadium-containing compound and phosphoric acid to obtain solution orslurry A; preparing imidazolium ionic liquid into solution B; preparing alkali metal nitrate, transition metal nitrate and lanthanide nitrate into mixed aqueous solution C; adding the B and the C into the A in a step-by-step precipitation and aging mode; and then obtaining the catalyst by concentrating, drying, forming and roasting. The catalyst prepared by the method has high activity and high selectivity for the reaction of preparing methacrylic acid by carrying out gas-phase oxidation on methylacrolein and has high mechanical strength and high thermochemical stability.

Description

technical field [0001] The invention relates to a method for preparing a catalyst for synthesizing methacrylic acid. The heteropolyacid compound catalyst is prepared by adopting the ionic liquid and metal salt step-by-step precipitation method, which improves the conversion rate of methacrolein and the selectivity of methacrylic acid, and improves the mechanical strength and stability of the shaped catalyst. Background technique [0002] Methyl methacrylate (MMA) is a widely used polymerization monomer, mainly used in the production of organic glass, coatings, adhesives, PVC modifiers, etc. The traditional process is the acetone cyanohydrin method using acetone and hydrocyanic acid as raw materials. This technical route has many by-products, poor atom economy, and the waste gas, waste water and waste residues discharged during production threaten the ecological environment and human safety. Friendly process route to replace, wherein the technology route from C4 derivatives ...

Claims

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Application Information

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IPC IPC(8): B01J27/199C07C57/055C07C51/235
Inventor 张锁江张恒闫瑞一杨丽刁琰琰王蕾李增喜
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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