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Catalyst for producing methyl methacrylate by one-step oxidative esterification method and its preparation method and application

A technology of methyl methacrylate and oxidative esterification, applied in the field of catalysis, can solve the problems of many by-products, unsuitable regeneration, gap in catalytic activity, etc., and achieves the effects of mild reaction conditions, simple preparation process and good selectivity

Active Publication Date: 2022-03-29
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Pd is the main active component in the catalyst for the direct oxidative esterification of methacrolein, methanol and molecular oxygen to produce MMA, but the result of single metal catalysis is low conversion rate, many by-products and poor selectivity (US3772381)
Subsequent patents have improved this, such as the Pd-Pb system catalyst proposed in Japanese Patents JP-B-57-35856, JP-A-57-50545 and JP-A-61-243044, Japanese Patent JP-B-61 -Pd-Bi system proposed by -60820, JP-B-62-7902 and JP-A-5-148184, Pd-Te system proposed by Japanese patent JP-A-61-243044, Japanese patent JP-B-57-35860 The proposed Pd-Tl-Hg system, the Pd-alkaline earth-Zn-Cd system proposed by Japanese patent JP-B-57-19090, etc., but the improvement methods disclosed in these Japanese patents are limited to adding many other metal components to improve This defect, and the catalyst preparation process is cumbersome and the reproducibility is poor
Subsequent research on single-metal catalysts, such as the Au-based catalysts proposed in Japanese patents JP-2000154164 and JP-2003192632, has high production costs and is not suitable for regeneration, and the active components are easy to lose. The Pt-based catalysts proposed in Japanese patent JP-57048937 have low activity. High and expensive, the Ru-based catalyst proposed in Japanese patent JP-2003260357 still has a large gap in catalytic activity compared with noble metal catalysts
Thereafter, the direct oxidative esterification of aldols to the corresponding carboxylates has not been much explored for monometallic Pd-catalyzed direct oxidative esterification of aldols

Method used

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  • Catalyst for producing methyl methacrylate by one-step oxidative esterification method and its preparation method and application
  • Catalyst for producing methyl methacrylate by one-step oxidative esterification method and its preparation method and application
  • Catalyst for producing methyl methacrylate by one-step oxidative esterification method and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1 PVA 3 -Pd 5 / MgO 10 -Al 2 o 3 catalyst

[0025] PVA 3 -Pd 5 / MgO 10 -Al 2 o 3 The preparation method of catalyst is as follows:

[0026] (1) 6.4gMg(NO 3 ) 2 ·6H 2 Dissolve O in 200ml deionized water, add carrier 10gγ-Al 2 o 3 , heat and stir until the solvent is evaporated to dryness, dry the obtained solid and grind it into a powder, roast the obtained powder in a nitrogen atmosphere at 350°C to 550°C for 2h to 5h, and then lower it to room temperature to obtain a composite carrier MgO 10 -Al 2 o 3 ;

[0027] (2) Take 0.225g PVA and 0.125g PdCl 2 Dissolve in 9ml deionized water, then add 0.0825g NaCl, stir magnetically at room temperature until completely dissolved, then add 1.5g of MgO prepared in step (1) 10 -Al 2 o 3 Carrier, then stir the resulting mixture and add 10ml of 5wt% NaOH-5wt% HCHO solution for reduction reaction, the reduction reaction temperature is 60°C, and the reduction time is 15min; after the reduction reaction is com...

Embodiment 2

[0029] Example 2 PVA 0.001 -Pd 10 / MgO 1.0 -Al 2 o 3 catalyst

[0030] The preparation method of catalyst adopts the same step as Example 1, and the difference is that the Mg(NO 3 ) 2 ·6H 2 The quality of O is changed to 0.64g, the quality of PVA is changed to 0.00015g, PdCl 2 The quality of NaCl is changed to 0.25g, the quality of NaCl is changed to 0.165g, the consumption of reducing agent 5wt%NaOH-5wt%HCHO is changed to 20ml, and other conditions are the same.

Embodiment 3

[0031] Example 3 PVA 2.5 -Pd 4 / MgO 2.0 -Al 2 o 3 catalyst

[0032] The preparation method of catalyst adopts the same step as Example 1, and the difference is that the Mg(NO 3 ) 2 ·6H 2 The quality of O is changed to 1.28g, the quality of PVA is changed to 0.15g, PdCl 2 The quality of NaCl was changed to 0.1g, the quality of NaCl was changed to 0.066g, the consumption of reducing agent 5wt%NaOH-5wt%HCHO was changed to 8ml, and other conditions were the same.

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Abstract

The invention discloses a catalyst for producing methyl methacrylate by one-step oxidative esterification method and its preparation method and application. The catalyst uses materials containing electron-rich oxides as a composite carrier, metal palladium as an active The metal is the co-active component, and the surfactant is used as the co-agent. Its general chemical formula can be expressed as: X a PD b Y c / M d ‑N, where Pd is palladium, X is a surfactant, Y is one of the rare earth elements scandium, yttrium, lanthanum or cerium, M is an electron-rich oxide, and N is a carrier. The catalyst can be applied to the reaction of methyl methacrylate (MMA) produced by one-step production of methyl methacrylate (MMA) through oxidation of methacrolein and esterification with methanol. The catalyst overcomes some shortcomings of the existing oxidative esterification catalysts by forming a special electron-donating structure between the active component, the carrier and the surfactant, and is applied to the reaction of one-step oxidative esterification to produce MMA in addition to having conversion In addition to the advantages of high yield and good selectivity, it also has the characteristics of simple preparation process and mild reaction conditions.

Description

technical field [0001] The invention belongs to the technical field of catalysis, and in particular relates to a catalyst for producing methyl methacrylate by one-step oxidative esterification and its preparation method and application. Background technique [0002] MMA is an organic chemical raw material widely used in industry. Its synthesis method was mainly based on the acetone cyanohydrin method (ACH method) in the past. The industrial application technology is mature and reliable, but its raw material hydrocyanic acid is highly toxic and reactive. Disadvantages such as refractory by-products, poor atom economy, and limited environmental protection have been gradually replaced by environmentally friendly processes, among which C4 synthesis processes are the main ones. The C4 synthesis process is mainly divided into the following four process routes: three-step oxidation of isobutene (IB) / tert-butanol (TBA), two-step oxidation of isobutene / tert-butanol, direct esterifica...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/63C07C67/39C07C69/54
CPCB01J23/63C07C67/39C07C69/54
Inventor 陈秉辉许梦东郑进保宗子厚吴钊男王明亮
Owner XIAMEN UNIV
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