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Gold-based catalyst, and preparation method and application thereof

A catalyst and gold-based technology, which is applied to the gold-based catalyst for preparing methacrolein dimethyl acetal and the field of preparation thereof, can solve the problem of low selectivity of MDA, low conversion rate of methacrolein, and inability to realize methyl acrolein at the same time. Problems such as high conversion of acrolein and high selectivity of MDA

Active Publication Date: 2020-11-10
XIAMEN UNIV
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  • Abstract
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  • Claims
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AI Technical Summary

Problems solved by technology

[0004] At present, the reaction of methacrolein and methanol to prepare MDA is mainly carried out under the action of Au catalyst, but the selectivity of MDA is generally not high or the conversion rate of methacrolein is very low, and the high conversion rate of methacrolein cannot be achieved at the same time. and high selectivity of MDA
For example, Yuchao Li et al. (oxidative esterification of methacrolein tomethyl methacrylate over supported gold catalysts prepared by colloiddeposition) reported a kind of Au / CeO 2 catalyst, the conversion rate of methacrolein is only 13%; Jun Gao et al. (Oxidative Esterification of Methacrolein to Methyl Methacrylate over Gold Nanoparticles on Hydroxyapatite) prepared a high-performance Au / N-HAP catalyst, which can only be achieved at a low conversion rate Higher MDA selectivity, the highest yield is only 32.3% (MAL conversion rate 34%, MDA selectivity 95%)

Method used

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  • Gold-based catalyst, and preparation method and application thereof
  • Gold-based catalyst, and preparation method and application thereof
  • Gold-based catalyst, and preparation method and application thereof

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preparation example Construction

[0033] The invention provides a kind of preparation method of gold-based catalyst, comprises the following steps:

[0034] S1: Dissolve the iron salt and protective agent in the solvent, stir evenly, then add the precipitant and stir evenly to obtain the first suspension. In the present invention, the iron salt is ferric nitrate, ferrous nitrate, ferric sulfate and ferrous sulfate One or more of them, using a precipitant to precipitate the iron ions in the iron salt in the form of hydroxide;

[0035] S2: Add reducing agent solution and carrier to the first suspension, stir evenly and transfer to a reaction kettle for reaction, the reaction temperature is 10-40°C, the reaction time is 8-36h, and the second suspension is obtained, wherein The carrier is aluminum hydroxide; in the presence of a reducing agent, iron ions are reduced to exist as a part of elemental iron;

[0036] S3: washing, filtering, and drying the second suspension to obtain a first solid powder. At this time,...

Embodiment 1-1

[0053] Weigh 0.469g Fe(NO 3 ) 3 9H 2 O and 0.50g protective agent were added to a 250mL Erlenmeyer flask, and dissolved in a mixed solvent of 82.5mL deionized water and 12.5mL ethanol, and magnetically stirred for 10min; then 12.5mL of 0.1mol / L NaOH precipitant solution was added to the above Stir in the solution for 10 minutes to obtain the first suspension. In the present invention, the precipitating agent precipitates the iron ions in the iron salt in the form of hydroxide.

[0054] Use a pipette to pipette 25 mL of hydrazine hydrate solution, add it to the above-mentioned first suspension and stir for 10 min; weigh 1 g of carrier AlOOH in a conical flask (the carrier AlOOH contains almost no chlorine in this example), and continue stirring for 10 min. Transfer the solution in the Erlenmeyer flask to the reaction kettle for stirring reaction, the reaction temperature is 25°C, and the reaction time is 18h. After the reaction is completed, the second suspension is obtained,...

Embodiment 1-2

[0060] The difference between this embodiment 1-2 and embodiment 1-1 is that the carrier is α-Al 2 o 3 , other preparation processes are the same as in Example 1-1.

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Abstract

The invention provides a gold-based catalyst and a preparation method thereof, and the application of the gold-based catalyst in MDA preparation reactions. The gold-based catalyst is characterized inthat the gold-based catalyst comprises a carrier, and an active component and an auxiliary agent which are loaded on the carrier, wherein the carrier is hydroxide of aluminum; the active component isgold, and the content of the active component is 0.1-10 wt.%; and the auxiliary agent is iron, or iron and iron oxide. With the gold-based catalyst, in the process of preparing methylacrolein dimethylacetal from methanol, methylacrolein and oxygen as raw materials, the conversion rate of methylacrolein can reach 80% or above, and MDA selectivity is up to 90% or above; and compared with the priorart, the yield of MDA is greatly increased, and large-scale industrial preparation of MDA is realized.

Description

technical field [0001] The invention relates to the technical field of catalysts, in particular to a gold-based catalyst for preparing methacrolein dimethyl acetal and a preparation method thereof. Background technique [0002] Acetal compounds are important spices and important intermediates in organic synthesis reactions. Acetals have good stability and will not react with oxidizing reagents, Grignard reagents, brominating reagents, metal hydrides, etc. Acetal compounds According to the synthesis route, it can be generally divided into three categories, one is single alcohol acetal, which is produced by condensation reaction of aldehyde and monohydric alcohol; the other is mixed acetal, which is produced by condensation reaction of aldehyde and two different monohydric alcohols; Acetals are formed by the condensation of aldehydes and diols. The preparation method of acetal compounds mainly includes direct condensation method, orthoformyl (silicate) ester condensation meth...

Claims

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Application Information

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IPC IPC(8): B01J23/89C07C41/56C07C43/303
CPCB01J23/8906C07C41/56C07C43/303
Inventor 陈秉辉王明亮郑进保吴钊男谢建榕张诺伟
Owner XIAMEN UNIV
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