A kind of gold-based catalyst, its preparation method and application

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 MDA selectivity and inability to achieve high conversion rate of methacrolein and high MDA at the same time. Selectivity, low conversion of methacrolein, etc.

Active Publication Date: 2021-10-01
XIAMEN UNIV
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  • Abstract
  • Description
  • Claims
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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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  • A kind of gold-based catalyst, its preparation method and application
  • A kind of gold-based catalyst, its preparation method and application
  • A kind of gold-based catalyst, its preparation method and application

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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, its preparation method and its application in the preparation of MDA reaction, which is characterized in that it includes a carrier, and active components and auxiliary agents loaded on the carrier; the carrier is aluminum Hydroxide; the active component is gold with a content of 0.1-10wt.%; the additive is iron, or iron and iron oxides. In the process of preparing methacrolein dimethyl acetal with methanol, methacrolein and oxygen as raw materials, the gold-based alloy catalyst obtained in the present invention has a conversion rate of methacrolein of more than 80% and a selectivity of MDA of up to 90%. Above, compared with the prior art, the yield of MDA is greatly improved, and the 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 produced by the condensation of aldehydes and diols. The preparation method of acetal compounds mainly includes direct condensation method, orthoformyl (silicate) ester condensation me...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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