Method for converting 2-hydroxyl-3-methoxy-5-aldehyde mandelic acid into vanillin

A technology of aldehyde vanillin and methoxy, which is applied in the field of vanillin preparation to achieve the effect of improving economic benefits

Inactive Publication Date: 2010-05-26
JIAXING ZHONGHUA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There is no related technology to reuse these aromatic compounds

Method used

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  • Method for converting 2-hydroxyl-3-methoxy-5-aldehyde mandelic acid into vanillin

Examples

Experimental program
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Effect test

Embodiment 1

[0039] Embodiment 1 macroporous resin static adsorption

[0040] Weigh 10 grams of D101 macroporous adsorption resin (purchased from Bengbu Liaoyuan New Material Co., Ltd.), put it into a 500ml single-mouth bottle, add 350ml pH3. Cr 6100mg / L, shake in a constant temperature shaking tank at 25-30°C for 1 hour, filter out the resin, and pass the detection of COD Cr Dropped to 985mg / L. Then add 5% (w / v) sodium hydroxide solution 250ml to carry out desorption, obtain the aromatic compound through enrichment, its COD Cr It is 14331mg / L.

Embodiment 2

[0041] Embodiment 2 macroporous resin dynamic adsorption

[0042] In a Add 400ml of XDA-1 macroporous adsorption resin (purchased from Xi’an Electric Power Resin Factory) into the chromatography column, and use electric wire heating method outside the column to keep the temperature inside the column at 35±3°C. First, add a certain amount of Glyoxylate vanillin production wastewater was submerged in the resin, and vanillin production wastewater was added from the top at a rate of 500ml per hour after 60 minutes, and the wastewater after adsorption treatment was collected from the bottom at the same time, and the cumulative amount of wastewater that could be treated reached 10908ml. After testing the COD of wastewater before adding Cr is 5827mg / L, COD of wastewater after adsorption Cr It is 857mg / L. Then add 5% (w / v) sodium hydroxide solution 250ml in 1 hour to carry out desorption, obtain the aromatic compound through enrichment, its COD Cr It is 12509mg / L.

Embodiment 3

[0044] In a 5L autoclave, add 3.5 kilograms of waste water containing 2-hydroxyl-3-methoxyl-5-formyl mandelic acid desorbed from resin, which contains 2-hydroxyl-3-methoxyl-5-formyl almond Acid about 45%. Adjust the pH value to be greater than 11, and then add 150 grams of copper oxide. Seal the autoclave, raise the temperature to 125-150°C for reaction, take a sample and analyze the conversion of 2-hydroxy-3-methoxy-5-formylmandelic acid to over 95%, and then stop the reaction. Cool to below 50°C, filter to obtain a clear liquid containing 2(2-hydroxy-3-methoxy-5-formyl)phenyl-2-oxoacetic acid, and the filtered clear liquid can be directly used for the next decarboxylation reaction.

[0045] Add the above clear liquid into a 5L three-necked flask, add 50% sulfuric acid to adjust the pH value to 4-5, and stir and cool to crystallize. After drying, 129 grams of 5-formyl vanillin were obtained, with a purity of 96.5% and a yield of 102.9% (note: the desorption wastewater itsel...

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Abstract

The invention relates to a method for converting 2-hydroxyl-3-methoxy-5-aldehyde mandelic acid into vanillin, which sequentially comprises the steps of adsorbing by macroporous resin, oxidizing, acidizing, reoxidizing, reacidizing, and the like. The method integrates wastewater treatment and reactant recycling and realizes the wastewater treatment by the macroporous resin. Aromatic compounds in the wastewater are recycled by combining an oxidizing and acidizing process to produce a target product-vanillin. The invention realizes the standard discharge of the wastewater, realizes the recycling of the wastewater generated during producing the vanillin by a glyoxylic acid method, and improves economic benefits.

Description

technical field [0001] The invention relates to a preparation method of vanillin, in particular to a method for converting 2-hydroxy-3-methoxy-5-aldehyde mandelic acid into vanillin. Background technique [0002] Vanillin is an important spice and food additive, which is widely used in flavoring various foods and daily chemical products. Currently, the global annual usage has reached about 17,000 tons. Yuan Hong comprehensively discussed the technology of ethyl vanillin synthesized by glyoxylic acid method in the article "New Technology of Domestic Glyoxylic Acid Synthesis of Ethyl Vanillin and Development Trend" (China Food Additives, z1, 2003). The glyoxylic acid method is also the most commonly used vanillin synthesis method in the world at present. Compared with the traditional nitrosylation method, it has the characteristics of relatively low cost and easy treatment of three wastes. The vanillin obtained by this production Accounting for more than 80% of the global van...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/58C07C45/65C02F9/04C02F1/72C02F1/42
Inventor 陈敏恒夏章健毛海舫
Owner JIAXING ZHONGHUA CHEM
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