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Production process and reaction equipment for synthesizing vanillin from 4-methyl guaiacol

A technology of methylguaiacol and production process, which is applied in the direction of bulk chemical production, condensation preparation of carbonyl compounds, organic compound/hydride/coordination complex catalyst, etc. Low yield and other problems, to achieve high yield, good selectivity, continuous separation and circulation effect

Pending Publication Date: 2020-10-09
KUNSHAN YAXIANG SPICEL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The existing vanillin preparation process uses 2-methoxy-4-methylphenol to prepare vanillin. The process is not complicated, but the yield is low and there are many wastes. It takes 20 tons of water to produce one ton of vanillin , can no longer meet the needs of process production

Method used

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  • Production process and reaction equipment for synthesizing vanillin from 4-methyl guaiacol
  • Production process and reaction equipment for synthesizing vanillin from 4-methyl guaiacol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] 4-methylguaiacol synthetic vanillin production technology, comprises the following steps:

[0044] S1. Prepare the raw material solution of 4-methylguaiacol and nitrosodimethylaniline in the mixing reactor 1, and supplement the catalyst in the mixing reactor 1;

[0045] The catalyst uses cobalt and iron as active components and honeycomb-shaped thermoplastic polyurethane elastic particles as carriers;

[0046] S2. Move the mixture in step S1 to the reactor 2, and at the same time, input high-pressure oxygen into the reactor 2 through the high-pressure oxygen pipe 3, and carry out catalytic oxidation reaction with the mixture in step S1 at 0.3 MPa and 80° C. for 1 hour;

[0047] S3, the product of step S2 is transported to the supercritical fluid extraction equipment 4 to extract the product, the extracted liquid phase is the obtained vanillin, the extracted filtrate is filtered, and the gas is separated through the separation tank 5 at the same time The liquid is separ...

Embodiment 2

[0056] 4-methylguaiacol synthetic vanillin production technology, comprises the following steps:

[0057] S1. Prepare the raw material solution of 4-methylguaiacol and nitrosodimethylaniline in the mixing reactor 1, and supplement the catalyst in the mixing reactor 1;

[0058] The catalyst uses cobalt and iron as active components and honeycomb-shaped thermoplastic polyurethane elastic particles as carriers;

[0059] S2. Move the mixture in step S1 to the reactor 2, and at the same time, input high-pressure oxygen into the reactor 2 through the high-pressure oxygen pipe 3, and carry out catalytic oxidation reaction with the mixture in step S1 at 0.4 MPa and 90° C. for 2 hours;

[0060] S3, the product of step S2 is transported to the supercritical fluid extraction equipment 4 to extract the product, the extracted liquid phase is the obtained vanillin, the extracted filtrate is filtered, and the gas is separated through the separation tank 5 at the same time The liquid is sepa...

Embodiment 3

[0069] 4-methylguaiacol synthetic vanillin production technology, comprises the following steps:

[0070] S1. Prepare the raw material solution of 4-methylguaiacol and nitrosodimethylaniline in the mixing reactor 1, and supplement the catalyst in the mixing reactor 1;

[0071] The catalyst uses cobalt and iron as active components and honeycomb-shaped thermoplastic polyurethane elastic particles as carriers;

[0072] S2. Move the mixture in step S1 to reactor 2, and at the same time, input high-pressure oxygen into reactor 2 through high-pressure oxygen pipe 3, and carry out catalytic oxidation reaction with the mixture in step S1 at 0.5 MPa and 100° C. for 3 hours;

[0073] S3, the product of step S2 is transported to the supercritical fluid extraction equipment 4 to extract the product, the extracted liquid phase is the obtained vanillin, the extracted filtrate is filtered, and the gas is separated through the separation tank 5 at the same time The liquid is separated, the ...

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Abstract

The invention relates to a production process for synthesizing vanillin from 4-methyl guaiacol. The process comprises the following steps of: S1, preparing a raw material solution of 4-methyl guaiacoland nitrosodimethylaniline in a mixed reaction kettle (1), and supplementing a catalyst in the mixed reaction kettle (1); wherein the catalyst adopts cobalt and iron as active components, and takes honeycomb thermoplastic polyurethane elastic particles as the carrier; S2, moving the mixture of S1 to a reactor (2), meanwhile, inputting high-pressure oxygen to the reactor (2) through a high-pressure oxygen pipe (3), and carrying out catalytic oxidation reaction with the mixture of S1 under a pressure of 0.3-0.5MPa and a temperature of 80-100DEG C for 1-3h; S3, conveying the product obtained inS2 into supercritical fluid extraction equipment (4) to extract the product, thus obtaining the extracted liquid phase, i.e. vanillin, filtering the extracted filtrate, separating the gas and the liquid through a separation tank (5), recovering the filtered catalyst to be used in S1, and recovering the filtered gas into a storage tank (6).

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a production process and reaction equipment for synthesizing vanillin through methylguaiacol. Background technique [0002] Vanillin is commonly known as vanilla powder, vanillin, vanilla powder, vanilla extract, vanillin. Extracted from the Rutaceae vanilla bean. White to light yellow crystal or crystalline powder, slightly sweet. Soluble in hot water, glycerin and alcohol, not easily soluble in cold water and vegetable oil. The aroma is stable and not easy to volatilize at higher temperature. It is easy to oxidize in the air, and it is easy to change color when it encounters alkaline substances. The chemical name is 3-methoxy-4-hydroxybenzaldehyde. It has vanilla bean aroma and strong milky aroma. It acts as an aroma enhancer and fixer. It is widely used in cosmetics, tobacco, cakes, candies, and baked goods, etc. The industry is one of the largest synthetic fragrance vari...

Claims

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Application Information

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IPC IPC(8): C07C47/58C07C45/45B01J31/28
CPCC07C45/45B01J31/28C07C47/58Y02P20/54
Inventor 陈清周军学强剑康汤建刚黎信业汤化雪刘天进
Owner KUNSHAN YAXIANG SPICEL CO LTD
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