Preparation method of vanillin

A vanillin and modification technology, applied in the field of vanillin preparation, can solve the problems of low price, high cost, low efficiency, etc., and achieve the effects of less three wastes, lower production costs, and simple operation

Active Publication Date: 2016-12-07
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Vanillin has always been one of the advantageous chemical products of our country to export and earn foreign exchange. However, compared with well-known foreign companies, there is still a big gap between the domestically produced vanillin and the international price. The export of vegeta

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Catalyst preparation

[0019] 1) Preparation of SBA-15. A typical process is as follows: 4.0g of P123 (polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer) is dissolved in 30g of water and 120g, 2mol / L of hydrochloric acid aqueous solution, stirring Then add 8.5g of tetraethyl orthosilicate, react at 35°C for 20h, then stand at 80°C for 12h, wash the obtained solid with water and absolute ethanol until neutral, dry at 100°C for 12h, and place in air at 500°C Calcined for 6h to obtain SBA-15.

[0020] 2) Preparation of modified SBA-15. The typical process is as follows: under the protection of nitrogen, add 2.40g of SBA-15 and 180mL of anhydrous toluene to a three-necked flask equipped with a condenser, and stir at room temperature for 10min. Then a mixture of 1g of 3-aminopropyl-triethoxysilane and 20mL of anhydrous chloroform was added to the reaction system, heated to reflux and stirred for 24h. After cooling, perform suction filtration, w...

Embodiment 2

[0024] Preparation of vanillin: In a 100mL round bottom flask, add 30mg of cat-1, 0.2g of 3-methoxy-4-hydroxybenzyl alcohol and 20ml of water, N 2 Under the atmosphere, the reaction temperature was 80°C, and the reaction was carried out under magnetic stirring and reflux conditions for 5 hours. After the reaction was completed, the catalyst was filtered out, and the organic matter in the filtrate was extracted with ethyl acetate, and the solvent was removed by distillation under reduced pressure to obtain 0.15 g of vanillin, 3- The conversion rate of methoxy-4-hydroxybenzyl alcohol was 76%.

Embodiment 3

[0026] Preparation of vanillin: In a 100mL round bottom flask, add 30mg of cat-1, 0.2g of 3-methoxy-4-hydroxybenzyl alcohol and 20ml of water, N 2 Under the atmosphere, the reaction temperature was 80°C, and the reaction was carried out under magnetic stirring and reflux conditions for 9 hours. After the reaction was completed, the catalyst was filtered out, and the organic matter in the filtrate was extracted with ethyl acetate, and the solvent was removed by distillation under reduced pressure to obtain 0.19 g of vanillin, 3- The conversion rate of methoxy-4-hydroxybenzyl alcohol was 96%.

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PUM

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Abstract

The invention belongs to the technical field of organic chemical industry, and particularly relates to a preparation method of vanillin. The preparation method includes: using 3-methoxy-4-hydroxybenzyl alcohol as a raw material and pure water as a solvent; under action of a Pd modified SBA-15 catalyst, enabling dehydrogenation reaction to obtain vanillin. The preparation method has the advantages that cost is low, and the water which is environment-friendly can be utilized as the solvent, so that using of conventional organic solvents like methylbenzene and benzene is avoided; the solvent is easy to separate and recycle.

Description

technical field [0001] The invention belongs to the technical field of organic chemical industry, and in particular relates to a preparation method of vanillin. Background technique [0002] Vanillin, whose chemical name is 3-methoxy-4-hydroxybenzaldehyde, has a strong milky taste, is one of the earliest spices discovered, and is also the most widely used spice in the world. With the continuous increase of people's demand for vanillin and the continuous development of science and technology, more and more vanillin is synthesized by chemical methods, accounting for about 99% of the total. In the food field, it is mainly used as an aromatic agent in ice cream, chocolate, candy, whiskey, etc. In the cosmetics industry, it is used as a fragrance raw material for perfumes and hand creams. In chemical synthesis, it is mainly used as a defoamer and precursor. With the continuous development of the medical field, vanillin can even be used as a medical masking agent and intermedia...

Claims

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Application Information

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IPC IPC(8): C07C45/00C07C47/58B01J29/035
CPCB01J29/0354C07C45/002C07C47/58
Inventor 李俊付伟许丽岳鲁敏段小刚代士维
Owner SHANGHAI INST OF TECH
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