Catalyst for selectively oxidizing methyl acrylic aldehyde to synthesize methyl propenoic acid and its use

A technology for synthesizing methacrylic acid and methacrolein, which is applied in physical/chemical process catalysts, preparation of organic compounds, organic chemistry, etc., and can solve problems such as short service life, low mechanical strength, and poor thermal stability

Active Publication Date: 2005-08-03
SHANGHAI HUAYI NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] There are a large number of reports related to the patents of MAL oxidative synthesis of MAA catalysts. Almost all of the patent reports are heteropolyacids (JP57-171443, CN1483014A and CN1273232A) with P, Mo and alkali metals as main components, but the solid catalyst exists Defects such as poor thermal stability, low mechanical strength, short service life, and poor selectivity to generate MAA
In order to avoid these defects, a large number of patents have improved this, such as adding metal sulfate (JP55-79340 and CN1126718A) or adding organic quaternary ammonium salts (CN1130171A and CN1407961A) to the catalyst composition to improve the catalyst. Although the mechanical strength has been improved, it reduces the reactivity and selectivity of the catalyst; US Pat. Caused the reduction of catalyst mechanical strength; There are also some patents (CN1048540A, CN1274619A and CN1461236A) by adding arsenic to the catalyst composition to achieve the purpose of improving its activity and selectivity, but the service life of the catalyst is caused by the sublimation characteristics of arsenic shorten

Method used

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  • Catalyst for selectively oxidizing methyl acrylic aldehyde to synthesize methyl propenoic acid and its use
  • Catalyst for selectively oxidizing methyl acrylic aldehyde to synthesize methyl propenoic acid and its use

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] One with 85 (Mo 12 P 1.5 K 1.5 Sb 0.5 Cu 0.3 As 0.2 V 0.5 In 0.3 Cs 0.2 Mo 2 ) / 15ZrO 2 The preparation method of the one-stage oxide catalyst (constituting the atomic ratio of the metal element of the active component and the carrier heat-conducting diluent) of expression is as follows:

[0017] 105.9 grams of ammonium paramolybdate, 2.9 grams of ammonium metavanadate, 4.2 grams of potassium hydroxide and 2.0 grams of cesium nitrate were dissolved in 200 grams of distilled water to obtain solution A. 7.4 g of phosphoric acid and 1.4 g of arsenic acid were dissolved in 20 g of water to obtain solution B. Dissolve 5.7 grams of antimony trichloride in 30 grams of 10% by weight of dilute hydrochloric acid aqueous solution, then add 3.6 grams of copper nitrate and 4.5 grams of indium nitrate to obtain solution C. Under stirring, solution B was first added to solution A, and then solution C was added, and the pH of the mixed solution was adjusted to 6 with ammonia ...

Embodiment 2

[0020] Except that 2.9 grams of ammonium metavanadate and 4.5 grams of indium nitrate were replaced by 6.5 grams of ammonium paratungstate and 3.2 grams of germanium tetrachloride. All the other catalysts were prepared in the same manner as in Example 1. The prepared catalyst consists of:

[0021] 85 (Mo 12 P 1.5 K 1.5 Sb 0.5 Cu 0.3 As 0.2 W 0.5 Ge 0.3 Cs 0.2 Mo 2 ) / 15ZrO 2

[0022] The selective oxidation reaction was carried out in the same manner as in Example 1, and the result of the reaction at 320° C. (hot spot temperature) for 80 hours was: the MAL conversion rate was 86.2%, and the MAA selectivity was 87.8%.

Embodiment 3

[0024] Except that 2.9 grams of ammonium metavanadate and 4.5 grams of indium nitrate were replaced with 3.3 grams of niobium pentoxide and 2.5 grams of silicon tetrachloride, all the others were prepared in the same manner as in Example 1. The prepared catalyst consists of:

[0025] 85 (Mo 12 P 1.5 K 1.5 Sb 0.5 Cu 0.3 As 0.2 Nb 0.5 Si 0.3 Cs 0.2 Mo 2 ) / 15ZrO 2

[0026] The selective oxidation reaction was carried out in the same manner as in Example 1, and the result of the reaction at 325° C. (hot spot temperature) for 80 hours was: the MAL conversion rate was 85.2%, and the MAA selectivity was 87.9%.

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Abstract

The present invention provides catalyst for selectively oxidizing methyl acrolein to synthesize methylpropenoic acid and its usage in catalyzing gas phase oxidation of methyl acrolein to synthesize methylpropenoic acid. The catalyst is one heteropoly acid salt containing Mo, P, K, Sb, Cu, As, etc., and has high catalytic activity and stability, long service life, methyl acrolein converting rate higher than 85 % and methylpropenoic acid selectivity over 87 % in the presence of molecular oxygen and diluting gas.

Description

technical field [0001] The invention relates to a heteropolyacid salt catalyst for synthesizing methacrylic acid (MAA) with methacrolein (MAL) through selective oxidation reaction and its application in MAL selective oxidation reaction. Background technique [0002] Methacrylic acid is an important organic synthetic raw material and polymerized monomer, mainly used in the synthesis of plexiglass polymerized monomer methyl methacrylate (MMA) and the synthesis of thermosetting coatings, adhesives, ion exchange resins, fabric treatment agents , leather treatment agents and other fine chemical products. At present, the more advanced process route in the world uses isobutene or tert-butanol as raw material to synthesize through two-step oxidation of MAL intermediate. [0003] There are a large number of reports related to the patents of MAL oxidative synthesis of MAA catalysts. Almost all of the patent reports are heteropolyacids (JP57-171443, CN1483014A and CN1273232A) with P, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/057B01J27/14C07C51/235C07C57/055
Inventor 张培璋张春雷温新庄岩马建学
Owner SHANGHAI HUAYI NEW MATERIAL
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