Carbon dioxide supercritical continuous extraction of vanillic aldehyde and derivates thereof from acidic water solution

An acidic aqueous solution, carbon dioxide technology, applied in the separation/purification of carbonyl compounds, bulk chemical production, organic chemistry, etc. The effect of continuous feeding

Active Publication Date: 2009-03-18
BC P INC CHINA NAT PETROLEUM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the disadvantages of high energy consumption, large amount of solvent, and water pollution.
[0006] Early foreign patents introduced the method of using carbon dioxide supercritical extraction of lignin in oxidized wood pulp to obtain vanillin. This process emphasizes the change of extraction pressure and temperature. The extracted vanillin contains acetylguaiacol, guaiac Wood phenol and other impurities, the purity is only about 90%, which affects the subsequent purification process

Method used

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  • Carbon dioxide supercritical continuous extraction of vanillic aldehyde and derivates thereof from acidic water solution
  • Carbon dioxide supercritical continuous extraction of vanillic aldehyde and derivates thereof from acidic water solution
  • Carbon dioxide supercritical continuous extraction of vanillic aldehyde and derivates thereof from acidic water solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] The carbon dioxide gas with a purity of 99.5% is pressed in from the bottom of the extraction column through a high-pressure plunger pump at a flow rate of 15kg / h, and the extraction pressure is controlled to 24MPa and the extraction temperature is 55°C. Then start the liquid high-pressure plunger pump, and press the 3.3% vanillin acid aqueous solution from the storage tank into the top of the extraction column. The liquid flow rate is 4.0Kg / h, so that the two fluids are in countercurrent continuous contact in the extraction column. The carbon dioxide fluid with vanillin passes through the top of the extraction column to the separation tank 1 for decompression. The separation tank 1 has a control pressure of 6.0MPa and a temperature of 55°C. After decompression, the vanillin remains at the bottom of the separation tank and the carbon dioxide gas Enter the separation tank 2 for decompression, control the pressure at 5.3MPa, and control the temperature at 32°C. The separated ...

Embodiment 2

[0026] Proceed as in Example 1. The carbon dioxide gas with a purity of 99.5% is pressed in from the bottom of the extraction column through a high-pressure plunger pump at a flow rate of 20kg / h, and the extraction pressure is controlled to 22MPa and the extraction temperature is 60°C. Then the liquid high-pressure plunger pump is started, and a 3.3% acidic aqueous solution of vanillin dissolved in the storage tank is pressed into the top of the extraction column, and the liquid flow rate is 3.8Kg / h. The carbon dioxide fluid with vanillin passes through the top of the extraction column to the separation tank 1 for decompression. The separation tank 1 has a control pressure of 5.7MPa and a temperature of 55°C. After decompression, the vanillin remains at the bottom of the separation tank and the carbon dioxide gas Enter the separation tank 2 for decompression, control the pressure at 5.0 MPa, control the temperature at 30°C, and run for 18 hours dynamically, stop the extraction, an...

Embodiment 3

[0028] Proceed as in Example 1. The carbon dioxide gas with a purity of 99.5% is forced in from the bottom of the extraction column through a high-pressure plunger pump at a flow rate of 20kg / h, the extraction pressure is controlled to 30MPa, the extraction temperature is 45°C, and the liquid flow rate is 3.0Kg / h. Control the pressure of separation tank 1 to 6.0MPa and control the temperature to 45℃. After decompression, the vanillin stays at the bottom of the separation tank, and the carbon dioxide gas enters the separation tank 2 for decompression. The control pressure is 5.0MPa, the control temperature is 30℃, and the dynamic operation is 18 hour. The vanillin content in the separation tank 1 was analyzed by high performance liquid chromatography to be 92.87%, the vanillin content in the water phase was 0.063%, and the extraction efficiency was 94.6%.

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Abstract

The invention provides a carbon dioxide supercritical method for continuously extracting vanillin and derivatives thereof in acidic aqueous solution. The method is characterized in that glyoxylic acid and phenolic compounds are used as raw materials, condensed and oxidized so as to obtain an acidic aqueous solution containing 2 to 7 percent of the vanillin and the derivatives thereof; the acidic aqueous solution and carbon dioxide supercritical fluid are continuously and reversely mixed in an extraction column, enter separation tanks, and are decompressed and separated so as to obtain a product; the liquid flow rate of the acidic aqueous solution is between 2 and 6 Kg/h; the flow rate of the carbon dioxide fluid is between 10 and 25 Kg/h; the pressure is between 20 and 35 MPa; the temperature is between 40 and 65 DEG C; the separation pressures of the two separation tanks are between 5.5 and 7.0 MPa and between 4.5 and 5.5 MPa respectively; the temperatures of the two separation tanks are between 50 and 65 DEG C and between 30 and 45 DEG C respectively; and the method is simple to operate, improves product content, has the extraction efficiency over 95 percent, has the product content more than 95 percent, realizes the continuous feeding of supercritical extraction, and has good industrialization prospect.

Description

Technical field [0001] The invention relates to a supercritical continuous countercurrent extraction of carbon dioxide using glyoxylic acid and phenolic compounds as raw materials, condensation and oxidation to obtain vanillin and vanillin in an acidic aqueous solution containing 2 to 7% vanillin and its derivatives Derivative method. Background technique [0002] Vanillin (vanillin), whose chemical name is 3-methoxy-4-hydroxybenzaldehyde, is the world’s largest production of synthetic fragrances and an important chemical intermediate. It is widely used in food, daily chemical, and pharmaceutical synthesis. etc. In addition, vanillin is used as a brightening agent in the electroplating industry and as a ripening agent in agriculture. [0003] The production of vanillin and its derivatives from glyoxylic acid and guaiacol (or 2-ethoxyphenol or catechol) through the condensation-oxidation route is currently an advanced synthesis process at home and abroad. The process has the advan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/58C07C45/80
CPCY02P20/54
Inventor 魏国峰刘宇
Owner BC P INC CHINA NAT PETROLEUM CORP
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