Method for synthesizing vanillin

A technology of vanillin and materials, which is applied in the field of safety technology, can solve the problems of poor control of reaction pressure, large explosion hazards, and explosion hazards, and achieve the effects of accelerating oxidation reaction speed, reducing the amount of hydrochloric acid, and short reaction time

Inactive Publication Date: 2011-04-27
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI +2
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Problems solved by technology

The disadvantages of this process are: the reaction temperature is too high / long time leads to serious deep oxidation of the target product, and the product yield is low; the reaction pressure is not easy to control, and it is difficult to avoid the wide explosion limit of methanol-oxygen, so the risk of explosion is great
Because the tank-type oxidation process technology that also uses methanol as the reaction solvent cannot avoid the extremely wide explosion limit of methanol-oxygen, so this process also has serious explosion hazards

Method used

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  • Method for synthesizing vanillin
  • Method for synthesizing vanillin

Examples

Experimental program
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Effect test

Embodiment 1

[0031] In 300 liters of pressure reactors, add 12 kilograms of sodium hydroxide, 50 kilograms of ethylene glycol monomethyl ethers, 15 kilograms of 4-methyl-2-methoxyphenols of artificial chemical synthesis, stir (rotating speed 130 rev / mins) After 10 minutes, 135 grams of cobalt dichloride hexahydrate as a catalyst and 0.7 grams of manganese acetate tetrahydrate as a cocatalyst were added, the kettle was sealed, and the mixture was stirred at 120° C. for 10-15 minutes by raising the temperature. Stop heating, and when the temperature drops to about 70°C, the reaction materials are introduced into a loop-type slurry reactor.

[0032]The temperature of the reaction material is controlled at 70° C., oxygen is introduced to start the oxidation reaction, and the pressure in the reactor is controlled at 0.3-0.5 MPa. Oxygen is fed intermittently to maintain the temperature of the reaction mass at 75-80°C. When the reaction almost no longer absorbs oxygen (reaction ends in about 5 h...

Embodiment 2

[0034] Using recovered ethylene glycol monomethyl ether as a solvent, repeating the operation of Example 1, the yield of vanillin product was 81%.

Embodiment 3

[0036] Use ethylene glycol monoethyl ether as solvent, repeat the operation of Example 1, and the yield of vanillin product is 85%.

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Abstract

The invention relates to a method for synthesizing vanillin, comprising the following steps of: carrying out material thermal pretreatment by adopting a pressured reaction axe, and then pouring the materials into a cannular slurry reactor for vanillin synthetic oxidation reaction; and by using 4-methyl-2-metoxyphenol as a raw material, using ethylene glycol monomethyl ether or ethylene glycol monoethyl ether as a solvent and using oxygen as an oxidant, carrying out the oxidation reaction for synthesizing vanillin in a way of intermittently feeding oxygen. The conversion rate of the 4-methyl-2-metoxyphenol as the raw material reaches more than 99%, the selectivity of the vanillin reaches more than 93%, and the separation yield reaches about 82%. The oxidation test carried out in the cannular slurry reactor proves that the oxidation reaction of the 4-methyl-2-metoxyphenol can be successfully carried out in the reactor under a milder condition to synthesize vanillin, and the method avoids a danger of easy explosion of the traditional axe type oxidation technology process for synthesizing vanillin by using methanol as the reaction solvent and has the advantages of environmental-protection process and high efficiency.

Description

technical field [0001] The invention relates to the synthesis of vanillin, in particular to a safe process technology suitable for industrial production that uses 4-methyl-2-methoxyphenol as a raw material to synthesize vanillin through oxidation. Background technique [0002] The methods for synthesizing vanillin mainly include eugenol method, guaiacol method, sassafras oil method and lignin method. The raw materials used in these methods are difficult to obtain, the price is high, and the synthetic routes are complicated. Although the glyoxylic acid method has been successfully developed to produce vanillin, the synthesis process discharges a large amount of phenolic wastewater, which is likely to cause serious environmental pollution problems. The Chinese patent CN1167750A published on December 17, 1997 reported a process for the synthesis of vanillin by a one-step oxidation method successfully developed by the Dalian Institute of Chemical Physics, Chinese Academy of Sci...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/58C07C45/36B01J31/04
Inventor 余正坤阎圣刚刘衡
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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