Catalyst for synthesizing vanillin and derivative and preparation

A catalyst and derivative technology, applied in the field of supported catalysts and preparation, can solve the problems of difficult source of glyoxylic acid raw materials, complicated separation process, low reaction efficiency, etc., and achieve strong industrial application value, high product purity, and high selectivity. Effect

Inactive Publication Date: 2008-08-06
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the source of glyoxylic acid raw materials is difficult and expensive
At present, the nitrosation method of guaiacol is mainly used in China to produce vanillin. This method has a long process route, serious discharge of three wastes, la...

Method used

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  • Catalyst for synthesizing vanillin and derivative and preparation
  • Catalyst for synthesizing vanillin and derivative and preparation
  • Catalyst for synthesizing vanillin and derivative and preparation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Weigh 1.20g Co(NO 3 ) 2 ·6H 2 O, 1.30g Cu(NO 3 ) 2 ·3H 2 O, 0.05g Fe(NO 3 ) 3 9H 2 O, 0.02gCe(NO 3 ) 3 ·6H 2 O Add water to a beaker to make 12mL impregnating liquid, mix 10g γ-Al 2 o 3 The carrier was added to the impregnating solution, stirred evenly, and after standing still for 24 hours, it was dried at 120°C, calcined in a muffle furnace at 600°C for 2 hours, and after cooling, it was finely ground to obtain Catalyst 1#, which was evaluated using Scheme 1, with air as the oxidant. The reaction results are shown in Table 1.

Embodiment 2

[0032] Weigh 3.69g Co(NO 3 ) 2 ·6H 2 O, 2.75g Cu(NO 3 ) 2 ·3H 2 O, 0.41g Fe(NO 3 ) 3 9H 2 O, 0.09gMn(CH 3 COO) 2 4H 2 O, 0.257g Ni(NO 3 ) 2 ·6H2 O, 0.020gCe(NO 3 ) 3 ·6H 2 O, add water to a beaker to make 12mL impregnation solution, put 10g TiO 2 The carrier was added to the impregnating solution, stirred evenly, and after standing still for 24 hours, it was dried at 120°C, roasted in a muffle furnace at 600°C for 2 hours, and after cooling, it was pulverized to obtain Catalyst 2#, which was evaluated using Scheme 1, with air as the oxidant. The reaction results are shown in Table 1.

Embodiment 3

[0034] Weigh 1.4g Co(NO 3 ) 2 ·6H 2 O, 1.89g Cu(NO 3 ) 2 ·3H 2 O, 0.02g Fe(NO 3 ) 3 9H 2 O, 0.02gMn(CH 3 COO) 2 4H 2 O, 0.068g Zn(NO 3 ) 2 ·6H 2 O, 0.13g Ce(NO 3 ) 3 ·6H 2 O was prepared in a beaker to make 12mL impregnating solution, and 5g γ-Al 2 o 3 and 5g TiO 2 The composite carrier was added into the impregnating solution, stirred evenly, and after standing still for 24 hours, it was dried at 120°C, roasted in a muffle furnace at 600°C for 3 hours, and after cooling, it was finely ground to obtain Catalyst 3#, which was evaluated using Scheme 1, with air as the oxidant. The reaction results are shown in Table 1.

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Abstract

The invention relates to a catalyst which is used for selecting hydroxymethyl in catalytic phenolic compound to be oxidized into aldehyde group and the preparation method thereof, in particular to a supported catalyst used in vanillin (3-methoxy-4-hydroxy benzaldehyde) compounded by 3-methoxy-4-hydroxy benzalcohol and 3-ethoxy-4-hydroxy benzalcohol and ethyl vanillin (3-methoxy-4-hydroxy benzaldehyde) and the preparation method thereof. The catalyst of the invention with one or more transition metal oxides as active components, which comprises cobalt, molybdenum, aluminum, silver, iron, copper, manganese, nickel, zinc and other oxides; one or more rare earth elements are added to be cocatalysts which comprise praseodymium, lanthanum, scandium, cerium, neodymium, etc., one or more composite materials among alumina, silicon dioxide, titanium dioxide, activated carbon are as carriers. Under the function of the catalyst, 3-methoxy-4-hydroxy benzalcohol can choose to be oxidized into vanillin. After 3-methoxy-4-hydroxy benzalcohol reacts under a temperature of 70 DEG C for 4h, the conversion rate of the 3-methoxy-4-hydroxy benzalcohol is up to 95.4 percent, and the yield rate of vanillin is 83.0 percent. The catalyst has the advantages of low cost, easy separation and recycling use after reaction, simple post-processing, low amount of by-products, friendly environment and wide prospect of industrialization application.

Description

technical field [0001] The invention relates to a catalyst and preparation method for catalyzing the selective oxidation of methylol groups on phenolic compounds into aldehyde groups, especially phenolic compounds with methylol groups on the 2, 3, and 4 positions of the benzene ring . More specifically refers to the synthesis of "vanillin" (3-methoxy-4-hydroxybenzaldehyde) and " A supported catalyst and preparation method of "ethyl vanillin" (3-ethoxy-4-hydroxybenzaldehyde). technical background [0002] Vanillin, also known as vanillin and methyl vanillin, has a scientific name of 3-methoxy-4-hydroxybenzaldehyde and has a unique sweet aroma of vanilla. It is one of the most widely used spices at present, with elegant and refreshing aroma, and can be widely used in industries such as fixatives, flavor enhancers, coordinating agents, cosmetics, soaps, blended spices, cigarettes, pastries, candies, and baked foods. It can also be used as a plant growth promoter, fungicide, ...

Claims

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Application Information

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IPC IPC(8): B01J23/83C07C47/58C07C45/27B01J37/02
Inventor 王筠松杨维成卢冠忠郭杨龙郭耘李海娟张志刚王艳芹刘晓晖
Owner EAST CHINA UNIV OF SCI & TECH
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