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A method for recovering veratraldehyde from veratraldehyde rectification raffinate

A technology of veratroaldehyde and rectification, which is applied in the preparation of alkali metal sulfites, the separation/purification of carbonyl compounds, organic chemistry and other directions, can solve problems such as increasing the disposal burden of enterprises, waste of useful substances, etc., and achieves easy industrialization. , Improve the added value, the effect that is conducive to environmental protection

Active Publication Date: 2021-11-16
武汉青江化工黄冈有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the bottoms of veratraldehyde distillation are treated as hazardous waste, which not only wastes a large amount of useful substances with high added value, but also increases the burden of disposal for enterprises

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Hydrolysis and sulfonation: 1M 3 The 3,4-dimethoxybenzaldehyde distillation kettle liquid is pumped into the hydrolysis kettle, and the temperature of the material in the hydrolysis kettle is controlled at 85~90°C to maintain a certain fluidity of the material. Add 2.0M 3 The saturated sodium bisulfite solution hydrolysis sulfonation kettle, 60-65 ℃ heat preservation hydrolysis sulfonation time is about 3 to 4 hours. After the hydrolysis is completed, keep the heat preservation and stand still for 1 hour, and separate the phases. The upper layer is a brown oil phase, and the lower layer is an aqueous phase with crystalline material, which is pumped into the alkalization kettle.

[0023] Alkalinization and phase separation: add 30% liquid caustic soda dropwise to the water phase of the alkalization kettle to adjust the pH to 10~11, control the temperature within 45~50°C, add 500 L of toluene, keep stirring for 3 hours, and stand still for 1 hour. Layering, the lower wat...

Embodiment 2

[0026] Hydrolysis and sulfonation: 1m 3 The 3,4-dimethoxybenzaldehyde distillation kettle liquid is pumped into the hydrolysis kettle, and the temperature of the material in the hydrolysis kettle is controlled at 80~90°C to maintain a certain fluidity of the material. Add 2.4 M 3 In the saturated sodium bisulfite solution hydrolysis kettle, the hydrolysis and sulfonation time is about 3 to 4 hours at 80-85 °C. After the hydrolysis is completed, stir for 1 hour, keep the temperature and stand still for 1 hour, and separate the phases. The upper layer is the brown oil phase, and the lower layer is the water phase with crystal material, which is pumped into the alkalization kettle.

[0027] Alkalinization and phase separation: Add 5% liquid caustic soda dropwise to the water phase of the alkalization kettle to adjust the pH to 9.5~10, control the temperature within 45~50°C, add 500 L of toluene, and keep stirring for 3 hours. Stand still for 1 hour, separate layers, the lower wa...

Embodiment 3

[0030] Hydrolysis and sulfonation: 1M 3 The veratraldehyde still liquor was pumped into the hydrolysis kettle, and the temperature of the material in the hydrolysis kettle was controlled at 85-90°C to maintain a certain fluidity of the material. Add 3.0 M 3 In the saturated sodium bisulfite solution hydrolysis kettle, the hydrolysis and sulfonation time is about 3 to 4 hours at 80~85°C. After the hydrolysis is completed, stir for 1 hour, keep the heat for 1 hour, and separate the phases. The upper layer is the brown oil phase, and the lower layer is the water phase with crystal material, which is pumped into the alkalization kettle.

[0031]Alkalinization and phase separation: add 5% soda ash solution dropwise to the water phase in the alkalization kettle to adjust the pH to 10~11, control the temperature at 45~50°C, add 500 L of toluene, keep stirring for 3 hours, stand still for 1 hour, divide The water phase in the lower layer goes to the water phase collection tank and en...

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PUM

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Abstract

The invention discloses a method for recovering veratraldehyde from veratraldehyde rectification raffinate, which solves the problems of waste disposal hazards and waste of useful substances in the prior art, and is characterized in that: rectification with veratraldehyde The raffinate is used as a raw material, and the sulfonated electrophile made of sodium bisulfite reacts with veratraldehyde to generate hydroxysulfonate, and the hydroxysulfonate insoluble in saturated sodium bisulfite is analyzed in the form of yellow crystals. Then separate the hydroxysulfonate from the saturated sodium bisulfite solution, add a dilute alkali solution to the separated hydroxysulfonate system to adjust the pH to 9.5-11.5, add an organic extraction solvent at the same time, and keep it warm at 60-90°C 3 to 5 hours, 45 to 50 ° C static phase separation, the oil phase enters the desolventization tower to recover the solvent to obtain the target product veratraldehyde. It has the advantages of advanced technology, simple operation, high aldehyde recovery rate, and easy industrial treatment, which is beneficial to environmental protection and increases the added value of resources. It provides a new organic synthesis method for recovering useful aldehydes from aldehyde distillation bottom liquid.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis production, in particular to a method for recovering veratraldehyde from veratraldehyde rectification raffinate. [0002] technical background [0003] The scientific name of veratraldehyde is 3,4-dimethoxybenzaldehyde, also known as methyl vanillin, pyrocatechin dimethyl ether, green veratraldehyde, vanillin methyl ether, methyl vanillin; white or light yellow Flaky crystal; easily soluble in ethanol and ether, sensitive to air; the solution can be oxidized to 3,4-dimethoxybenzoic acid under the influence of light. It is a synthetic spice with a vanilla-like aroma, and it is also a pharmaceutical intermediate with many uses. It can be used in the synthesis of antibiotics, such as the synthesis of verazin, methyldopa, methyldopa ethyl ester, carby Dopa, and diaminoveratridine and so on. There are many techniques for synthesizing veratraldehyde in the prior art. There are mainly vanilli...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/78C07C45/85C07C45/80C07C45/81C07C45/82C07C45/42C07C47/575C07C303/32C07C309/24C01D5/14
CPCC01D5/14C07C45/42C07C45/78C07C45/80C07C45/81C07C45/82C07C45/85C07C303/32C07C47/575C07C309/24
Inventor 欧阳兆辉赵敏张淑珍陈建超周建锋陈扬张恒明
Owner 武汉青江化工黄冈有限公司
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