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Preparation method of isovanillin

A technology of isovanillin and ethyl vanillin, which is applied in the field of preparation of isovanillin, can solve the problems of process by-products polluting the environment, etc.

Inactive Publication Date: 2018-05-29
CHONGQING THRIVE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in many chemical synthesis methods, the raw materials themselves are expensive drug intermediates in the reaction process, and many process by-products pollute the environment

Method used

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  • Preparation method of isovanillin
  • Preparation method of isovanillin
  • Preparation method of isovanillin

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Experimental program
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Effect test

Embodiment 1

[0050] A preparation method of isovanillin, comprising the steps of:

[0051] (1) Dimethyl sulfate and ethyl vanillin solution were reacted for 6 hours in an alkaline environment at a temperature of 20° C., filtered, and the filter residue was taken to obtain an intermediate.

[0052] (2) The intermediate and concentrated sulfuric acid were reacted for 5 hours in an inert gas atmosphere at a temperature of 50°C and under negative pressure conditions.

Embodiment 2

[0054] A preparation method of isovanillin, comprising the steps of:

[0055] (1) Adding ethyl vanillin to a potassium hydroxide solution with a pH of 12 to obtain an ethyl vanillin solution.

[0056] (2) Dimethyl sulfate and ethyl vanillin solution were reacted in an alkaline environment at a temperature of 30° C. for 6 hours, filtered, washed and dried to obtain an intermediate. Wherein, the mass ratio of ethyl vanillin to dimethyl sulfate is 1:1.

[0057] (3) Put the intermediate into an enamel reaction kettle, and add concentrated sulfuric acid with a mass concentration of 92% after passing through nitrogen, and react at a temperature of 60°C and a pressure of -92Kpa for 3 hours to obtain crude isovanillin. Among them, the mass ratio of the intermediate to the concentrated sulfuric acid is 1:2.

[0058] (4), transfer the reacted isovanillin crude product into water to dilute and then extract with ethyl acetate to obtain isovanillin, wherein the mass ratio of concentrated...

Embodiment 3

[0060] A preparation method of isovanillin, comprising the steps of:

[0061] (1) Adding ethyl vanillin to sodium hydroxide solution with a mass concentration of 8% to obtain ethyl vanillin solution.

[0062] (2) Dimethyl sulfate and ethyl vanillin solution were reacted in an alkaline environment at a temperature of 5° C. for 4 hours, filtered, washed and dried to obtain an intermediate. Among them, the mass ratio of ethyl vanillin to dimethyl sulfate is 1:0.8.

[0063] (3) Add the intermediate to an enamel reaction kettle, and add concentrated sulfuric acid with a mass concentration of 90% after passing through nitrogen, and react at a temperature of 40°C and a pressure of -90Kpa for 2 hours to obtain crude isovanillin. Among them, the mass ratio of the intermediate to the concentrated sulfuric acid is 1:1.5.

[0064] (4) Transfer the reacted crude isovanillin into ice water for dilution, extract with ethyl acetate, and distill under reduced pressure to obtain pure isovanil...

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Abstract

The invention provides a preparation method of isovanillin, and belongs to the technical field of isovanillin production. The preparation method of isovanillin comprises the following steps: dimethylsulfate and an ethyl vanillin solution are subjected to reaction in an alkaline environment at temperature of 5-40 DEG C for 4-8h, filtering is performed, filter residues are taken, and an intermediate is obtained; the intermediate and concentrated sulfuric acid are subjected to reaction for 2-7 hours in an inert gas atmosphere at temperature of 40-70 DEG C and under negative pressure. According to the preparation method, ethyl vanillin, dimethyl sulfate, concentrated sulfuric acid and the like are used as raw materials and are easily available and low in cost, the process is simple to controland easy to operate, industrial production is easy to realize, the yield is high, little waste water is produced, and the method is environmentally friendly.

Description

technical field [0001] The invention relates to the technical field of isovanillin production, in particular to a preparation method of isovanillin. Background technique [0002] Isovanillin is also called isovanillin or isovanillin, and its chemical name is 3-hydroxy-4-methoxybenzaldehyde. Isovaillin has an olive-like aroma and rich milky aroma. It is an important raw material in the food additive industry. It is used as a flavor enhancer and sweetener, and is widely used in sugar, popsicles, beverages, desserts, tobacco and alcohol class industry. Isvanillin is also an important product in the fine chemical industry, and is widely used to regulate plant growth, as an additive in cosmetics and skin care products, etc. Isvanillin has a unique property: its fragrance also changes with the change of ambient temperature, so it is especially suitable for some special fragrances and flavor industries, and can also be used as deodorant for soap, toothpaste, rubber, plastic and o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/64C07C47/575
CPCC07C45/64C07C47/575
Inventor 兰军马学兵赵华文唐凌
Owner CHONGQING THRIVE CHEM
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