Unlock instant, AI-driven research and patent intelligence for your innovation.

Isovanillin centrifugal extraction method

A technology of isovanillin and centrifugal extractor, which is applied in the field of organic extraction, can solve the problems of large volume of extraction tower, low extraction efficiency, and large amount of solvent, so as to shorten the operation period, improve the separation efficiency, and simplify the process.

Active Publication Date: 2016-06-29
PETROCHINA CO LTD
View PDF4 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0017] The technical solution of the present invention is to overcome the separation of isovanillin by means of step-by-step separation in the prior art, which has a long process and complicated procedures; the extraction tower used in the extraction is bulky, the amount of solvent used is large, and the extraction efficiency is low. Insufficient such as separation difficulties, and the shortcomings of the need for acidification and neutralization before entering the extraction tower, and provide a centrifugal extraction method for isovanillin, which involves the use of 3,4-dihydroxybenzaldehyde selective methylation reaction synthesis The isovanillin crude product aqueous solution, the method that adopts centrifugal extractor to separate isovanillin

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Isovanillin centrifugal extraction method
  • Isovanillin centrifugal extraction method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Such as figure 1 Shown, use 1 # The content of the 3,4-dihydroxybenzaldehyde selective methylation reaction synthesized by the metering pump 3 is 91.3% by weight of the crude isovanillin liquid at 1.2m 3 / h flow, same as 0.4m 3 / h of extracted benzene, injected into the light phase inlet of the first centrifugal extractor 4 together with 2 # Metering pump 5 will flow 9.6m 3 / h 30~32wt% sodium hydroxide solution is injected into the heavy phase inlet, and the centrifuge is extracted and separated at 18°C. The centrifuge drum speed is controlled to 2800r / min, and the light phase outlet flows out the veratraldehyde-rich benzene phase , Distilled in the first benzene boiler 1 to obtain veratraldehyde and solvent benzene, and solvent benzene is recovered to 1 # Benzene storage tank 2, use 1 # Metering pump 3 will 1 # The solvent benzene in the benzene storage tank 2 is recycled to the first centrifugal extractor 4, and the water phase rich in isovanillin and vanillin from the h...

Embodiment 2

[0053] According to the operation steps of Example 1, the crude isovanillin content was changed, and the remaining process conditions were the same as in Example 1.

[0054] 1) The content of crude isovanillin liquid: 92.6% by weight;

[0055] 2) Isovanillin crude liquid content: 93.0wt%.

[0056] The test conditions and results are shown in the attached table below.

Embodiment 3

[0058] According to the operating steps of Example 1, change the flow of crude isovanillin and the flow of extraction of benzene, sodium hydroxide, and sulfuric acid, and the remaining process conditions are the same as in Example 1.

[0059] Isovanillin crude liquid flow rate

[0060] 1) Isovanillin crude liquid flow rate: 1.3m 3 / h;

[0061] 2) Isovanillin crude liquid flow rate: 1.4m 3 / h;

[0062] 3) Isovanillin crude liquid flow rate: 1.5m 3 / h.

[0063] Extraction benzene flow

[0064] 1) Extraction benzene flow rate: 0.43m 3 / h;

[0065] 2) Extraction benzene flow rate: 0.47m 3 / h;

[0066] 3) Extraction benzene flow rate: 0.3m 3 / h.

[0067] Sodium hydroxide flow

[0068] 1) Sodium hydroxide flow rate: 10.4m 3 / h;

[0069] 2) Sodium hydroxide flow: 11.4m 3 / h;

[0070] 3) Sodium hydroxide flow rate: 12.3m 3 / h.

[0071] Sulfuric acid flow

[0072] 1) Sulfuric acid flow rate: 0.26m 3 / h;

[0073] 2) Sulfuric acid flow rate: 0.30m 3 / h;

[0074] 3) Sulfuric acid flow rate: 0.33m 3 / h.

[0075...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
melting pointaaaaaaaaaa
Login to View More

Abstract

The invention belongs to the technical field of organic extraction, and discloses an isovanillin centrifugal extraction method. 3,4-dihydroxyl benzaldehyde carries out selective methylation reactionsto obtain a coarse liquid product of isovanillin with an isovanillin content of 91 to 93 wt%; the coarse product also comprises 5 to 6 wt% of vanillin, and 2 to 3 wt% of veratraldehyde. According to the extraction method, the coarse liquid product of isovanillin with a flow rate of 1.2 to 1.5 m<3> / h and extracting benzene with a flow rate of 0.4 to 0.5 m<3> / h are injected into the light phase inlet of a centrifugal extractor together, a sodium hydroxide solution (30 to 32 wt%) is injected into the heavy phase inlet; after centrifugal extraction and separation, a benzene phase, which is rich inveratraldehyde and flows from the light phase outlet, is distilled to obtain veratraldehyde and benzene (the solvent); a water phase, which is rich in isovanillin and vanillin and flows from the heavy phase outlet, and a solvent (benzene) are injected into the light phase inlet of another centrifugal extractor, a sulfuric acid solution (30 to 32 wt%) is injected into the heavy phase inlet, aftercentrifugal extraction and separation, a benzene phase, which is rich in isovanillin and flows from the light phase outlet, is distilled to obtain an isovanillin product, and the isovanillin product is purified to obtain the final product.

Description

Technical field: [0001] The invention belongs to the technical field of organic extraction, and relates to a centrifugal extraction method for isovanillin, that is, it relates to a crude isovanillin aqueous solution synthesized by a selective methylation reaction of 3,4-dihydroxybenzaldehyde, and a centrifugal extractor is used to separate isovanillin Vegetarian method. Background technique: [0002] The chemical name of isovanillin is 3-hydroxy-4-methoxybenzaldehyde. It is mainly used in fragrances, essences, food and cosmetic additives, plant growth regulators, etc. It is also an important pharmaceutical intermediate. As a pharmaceutical intermediate, it is mainly used to synthesize 2-bromo-isovanillin, and then synthesize anti-cancer, radiation and chemotherapy sensitizers such as kangbotide and phenanthrenequinone. [0003] At present, the "green process" for synthesizing isovanillin is mainly to use catechol as the starting material and condense with glyoxylic acid to synthes...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/575C07C45/78
Inventor 杨雨富刘宇刘长清张宏宇王淑娟
Owner PETROCHINA CO LTD