Method for recycling solvent, namely isopropanol, during production of carvone

A technology of recovery and treatment of isopropanol, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as inability to produce carvone, unfavorable industrial production, long production cycle, etc., and achieve enhanced international Market competitiveness, cost saving, less side effects

Inactive Publication Date: 2012-07-04
HUAIAN WAN BANG SPICE IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the commonly used treatment methods are as follows: one is fractional distillation after adding quicklime to reflux, and calcium hydride, magnesium strips, barium oxide, calcium sulfate and molecular sieves can also be used for dehydration. In the production of carvone, the circulation of isopropanol is large. This water removal method is not conducive to industrial production; the second is to add solid sodium hydroxide to absorb water, separa...

Method used

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  • Method for recycling solvent, namely isopropanol, during production of carvone
  • Method for recycling solvent, namely isopropanol, during production of carvone

Examples

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Effect test

Embodiment 1

[0020] Take the theoretical plate number of the extractive distillation column as 70 (the plate number is counted from bottom to top), select the ethylene glycol mixed solution containing potassium acetate mass fraction as 20% as the salt-added extraction agent, and start from the 65th theoretical plate Add, flow rate is 1500kg / hour, water content is the isopropanol aqueous solution of 15% to add from the 20th theoretical plate, flow rate is 500 kg / hour. Operate under normal pressure, the reflux ratio at the top of the tower is 0.3, the temperature at the top of the tower is controlled at 82-83°C, and the temperature at the bottom of the tower is controlled at 130-135°C. Analyze the isopropanol that tower top obtains, water content is 5%.

[0021] The water, salt, and solvent mixture in the tower kettle enter the regeneration tower. In this embodiment, the regeneration tower selects 50 theoretical plates, the feeding position is the 20th theoretical plate, and the operating ...

Embodiment 2

[0023] The number of theoretical plates of the extractive distillation column is selected as 80 (the number of plates is counted from bottom to top), and the ethylene glycol mixture containing sodium acetate with a mass fraction of 15% is selected as the salt-added extraction agent. From the 72nd theoretical plate Adding, the flow rate is 1300kg / hour, and the isopropanol solution with a water content of 14% is added from the 20th theoretical plate, and the flow rate is 500 kg / hour. Operate under normal pressure, the reflux ratio at the top of the tower is 0.5, the temperature at the top of the tower is controlled at 82-83°C, and the temperature at the bottom of the tower is controlled at 130-135°C. The isopropanol obtained at the top of the tower is analyzed with a water content of 0.4%.

[0024] The water, salt, and solvent mixture in the tower kettle enter the regeneration tower. In this embodiment, the regeneration tower uses 40 theoretical plates, the feed position is at th...

Embodiment 3

[0026] The number of theoretical plates of the extractive distillation column is 90 (the number of plates is counted from the bottom to the top), and the propylene glycol mixture containing sodium propionate with a mass fraction of 18% is selected as the salt-added extraction agent, and the salt is added from the 79th theoretical plate. , the flow rate is 1300 kg / hour, and the isopropanol solution with a water content of 13% is added from the 20th theoretical plate, and the flow rate is 500 kg / hour. Operate under normal pressure, the reflux ratio at the top of the tower is 0.6, the temperature at the top of the tower is controlled at 82-83°C, the temperature at the bottom of the tower is controlled at 130-135°C, and the water content of the isopropanol obtained at the top of the tower is 0.45%. All the other implementations are as in embodiment 1 or 2.

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Abstract

The invention discloses a method for recycling a solvent, namely isopropanol, during production of carvone. The method comprises the following steps: respectively adding a salt extracting agent and an isopropanol water solution obtained by distillation and separation during the production of the carvone into a rectifying tower under normal pressure so as to get isopropanol with the water content of not more than 5% at the top of the tower, and enabling a water-salt-solvent mixture obtained in a tower kettle to enter into a regeneration tower for recycling and reutilization, wherein the flow ratio of the isopropanol solution to the salt extracting agent solution is 1:(2-5), the temperature at the top of the tower is 80-85 DEG C, the temperature in a tower kettle is 130-135 DEG C, the salt extracting agent is a mixture of carboxylate and the organic polar solvent, and the percentage by weight of the salt in the salt extracting agent is 15-35%.

Description

technical field [0001] The invention relates to a method for recovering, treating and recycling solvents for synthesis of fragrance compounds, in particular to a method for recovering and treating solvent isopropanol in carvone production. Background technique [0002] The solvent isopropanol used in the production of carvone requires that its water content should be 0.5% or below to meet the production requirements, while the water content of the isopropanol solution obtained by distillation and separation of carvone in the production process is 12-20%. 20%, it is necessary to further reduce the water content to below 0.5% before it can be used in production. At present, the commonly used treatment methods are as follows: one is fractional distillation after adding quicklime to reflux, and calcium hydride, magnesium strips, barium oxide, calcium sulfate and molecular sieves can also be used for dehydration. In the production of carvone, the circulation of isopropanol is lar...

Claims

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Application Information

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IPC IPC(8): C07C31/10C07C29/80C07C49/647C07C45/00
Inventor 林祥陈兆刚陈文昌
Owner HUAIAN WAN BANG SPICE IND CO LTD
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