Heterogeneous catalyst used in reaction of synthesizing vanillin and preparation method thereof

A heterogeneous catalyst and catalyst technology, applied in the preparation of organic compounds, the preparation of carbon-based compounds, chemical instruments and methods, etc., can solve the problems of non-reusability, complex process, difficult separation, etc., and achieve strong industrial application value, The effect of high product purity and easy purification

Inactive Publication Date: 2011-06-15
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above catalysts are all soluble homogeneous catalysts, which are difficult to separate after the reaction and cannot be reused. Therefore, there are many problems such as complicated process, high cost and serious pollution.

Method used

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  • Heterogeneous catalyst used in reaction of synthesizing vanillin and preparation method thereof
  • Heterogeneous catalyst used in reaction of synthesizing vanillin and preparation method thereof
  • Heterogeneous catalyst used in reaction of synthesizing vanillin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Weigh 1.5gCo(NO 3 ) 2 ·6H 2 O, 1.0gMn(NO 3 ) 2 ·6H 2 O, 0.06gAl(NO 3 ) 3 ·6H 2 O was prepared into a mixed solution with a certain concentration, and 0.5 mol / L NaOH solution was slowly added dropwise to the mixed solution, and titrated to pH = 8 under vigorous stirring, aged for 4 hours, filtered and washed to neutralize the precipitate. Dry at 120°C, bake in a muffle furnace at 400°C for 4 hours, cool and grind to obtain 1# catalyst, and use the implementation plan for evaluation.

Embodiment 2

[0022] Weigh 1.5gCo(NO 3 ) 2 ·6H 2 O, 1.0gMn(NO 3 ) 2 ·6H 2 O, 0.06gAl(NO 3 ) 3 ·6H 2 O is prepared into a mixed solution with a certain concentration, and 0.5mol / L Na 2 CO 3 The solution was added dropwise to the mixed solution, titrated to pH=9 under vigorous stirring, aged for 5 hours, filtered and washed to neutralize the precipitate. Dry at 120°C, bake in a muffle furnace at 500°C for 3 hours, cool and grind to obtain 2# catalyst, and use the implementation plan for evaluation.

Embodiment 3

[0024] Weigh 1.5gCo(NO 3 ) 2 ·6H 2 O, 1.0gMn(NO 3 ) 2 ·6H 2 O, 0.06gAl(NO 3 ) 3 ·6H 2 O is prepared into a mixture of a certain concentration, and a certain amount of NH 4 Add OH dropwise to the mixture, titrate to pH=10 under vigorous stirring, age for 4 hours, filter and wash the precipitate to neutrality. Dry at 120°C, bake in a muffle furnace at 300°C for 7 hours, cool and grind to obtain 3# catalyst, and use the implementation plan to evaluate.

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Abstract

The invention relates to a heterogeneous catalyst used in one-step reaction of synthesizing vanillin through catalytic oxidation of 4-methyl-2-metoxyphenol. A Co(x)Mn(y)M(z)O(1-x-y-x) type heterogeneous catalyst is prepared by adopting cobalt and manganese as active components and adding one or more of elements, such as aluminum, silicon, cerium, zirconium, niobium and the like as cocatalysts, and using an alkaline solution as a precipitator through using a coprecipitation process. Under the action of the catalyst, oxidization is carried out by adopting oxygen or air, the reaction is carried out for 5 hours under a pressurizing condition, the transfer rate of the 4-methyl-2-metoxyphenol can reach 100 percent, and the yield of the vanillin can reach 85 percent. The catalyst has the advantages of simpleness in preparation and low cost, is easy to separate and recycle after the reaction, and is capable of completely replacing homogeneous catalysts of cobalt, copper salts and the like applied to the modern industry. Meanwhile, the catalyst has the advantages of less reaction solution side products after the catalytic oxidation reaction, simpleness in treatment, environment protection performance, and stronger application prospect in the preparation process of the vanillin.

Description

technical field [0001] The present invention provides a recyclable Co(x)Mn(y)M(z ) O(1-x-y-z) type heterogeneous catalyst and its preparation method. technical background [0002] Vanillin, whose scientific name is 3-methoxy-4-hydroxybenzaldehyde, is one of the most widely used spices at present. Cigarette, pastry, candy and baked food industries, can also be used as a plant growth promoter, fungicide, lubricant defoamer, etc. At present, vanillin is mainly obtained by chemical synthesis methods, and its main synthesis methods include guaiacol method, lignin method, safrole method, eugenol method, p-hydroxybenzaldehyde method, 4-methylguaiacol method, p-hydroxybenzaldehyde method, cresol method. The preparation method of the above vanillin is involved at home and abroad at present, but the above method is not long in process route, the three wastes are relatively serious, and the investment in supporting equipment is large, and the separation process of the obtained produ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/889C07C47/58C07C45/36
CPCY02P20/584
Inventor 王筠松赵安锋卢冠忠郭耘郭杨龙詹望成张志刚韩伟王艳芹刘哓晖龚学庆
Owner EAST CHINA UNIV OF SCI & TECH
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