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A method for reducing isomerization of beta-ionone in a rectification process

A technology of ionone and rectification process, applied in the separation/purification of carbonyl compounds, organic chemistry and other directions, can solve the problems of high yield, low purity and high operating costs

Inactive Publication Date: 2021-11-19
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] 1. General vacuum degree (10-15mmHg), high distillation temperature (above 300°C), the result is low yield (generally less than 60%), low purity, serious isomerization in the rectification process, and the main isomerization is very large Difficult to separate α-ionone (boiling point is only 2°C different from β-ionone), up to 35%
[0004] 2. High vacuum (below 1mmHg), medium distillation temperature (about 250°C), high yield (generally less than 70%), average purity, serious isomerization in the rectification process, the main isomerization is difficult Isolated α-ionone (boiling point is only 2°C different from β-ionone), up to 20%, and high operating costs
[0005] As a pharmaceutical intermediate for the preparation of vitamin A, the purity of β-ionone must reach more than 94%, otherwise it can only be scrapped or used as a spice raw material with a much lower price, which will cause great losses

Method used

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  • A method for reducing isomerization of beta-ionone in a rectification process
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  • A method for reducing isomerization of beta-ionone in a rectification process

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Embodiment 1-1

[0022] A method for reducing isomerization of β-ionone in a rectification process, the specific steps are:

[0023] Grind the purchased chemically pure magnesia into 100 mesh powder (if the product is powdery, it is not necessary to grind again). Dry the powdered magnesia in an oven at 120°C for 3 hours for later use, and put it in a desiccator for later use if not used in time. Add the baked magnesium oxide powder into the crude product of β-ionone to be rectified while stirring. Use a vacuum pump to draw the β-ionone crude product to be rectified with magnesium peroxide powder into the rectification tower for rectification. The distillate is in a boiling state to ensure that the magnesium oxide does not sink to the bottom of the rectification tower. Then gradually increase the temperature for fractionation, the heating rate is about 5°C / min, there is a slip-out, and after the top of the refining tower reaches 70-80°C (related to the vacuum degree, the vacuum degree is abou...

Embodiment 1-2

[0025] A method for reducing isomerization of β-ionone in the rectification process, the specific steps are as follows.

[0026] Grind the purchased chemically pure magnesia into 100 mesh powder (if the product is powdery, it is not necessary to grind again). Dry the powdered magnesia in an oven at 120°C for 3 hours for later use, and put it in a desiccator for later use if not used in time. Add the baked magnesium oxide powder into the crude product of β-ionone to be rectified while stirring. Use a vacuum pump to draw the β-ionone crude product to be rectified with magnesium peroxide powder into the rectification tower for rectification. The distillate is in a boiling state to ensure that the magnesium oxide does not sink to the bottom of the rectification tower. Then gradually increase the temperature for fractionation, the heating rate is about 5°C / min, there is a slip-out, and after the top of the refining tower reaches 70-80°C (related to the vacuum degree, the vacuum d...

Embodiment 1-3

[0028] A method for reducing isomerization of β-ionone in the rectification process, the specific steps are as follows.

[0029] Grind the purchased chemically pure magnesia into 100 mesh powder (if the product is powdery, it is not necessary to grind again). Dry the powdered magnesia in an oven at 120°C for 3 hours for later use, and put it in a desiccator for later use if not used in time. Add the baked magnesium oxide powder into the crude product of β-ionone to be rectified while stirring. Use a vacuum pump to draw the β-ionone crude product to be rectified with magnesium peroxide powder into the rectification tower for rectification. The distillate is in a boiling state to ensure that the magnesium oxide does not sink to the bottom of the rectification tower. Then gradually increase the temperature for fractionation, the heating rate is about 5°C / min, there is a slip-out, and after the top of the refining tower reaches 70-80°C (related to the vacuum degree, the vacuum d...

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Abstract

The invention provides a method for reducing the isomerization of β-ionone in the rectification process, which is characterized in that, comprising: adding metal oxide or metal carbonate powder to the crude product of β-ionone to be rectified, Carry out rectification in the rectification tower. During the rectification process, the product to be rectified is boiled so that the metal oxide or metal carbonate powder does not sink to the bottom of the rectification tower. The present invention can preferably reduce the proportion of β-ionone isomerized into α-ionone that is difficult to separate in the heating and rectifying process, and increase the product yield to 72.5% (according to the purity of qualified products higher than 94%) β-ionone ‑Ionone, which meets the requirements as a raw material for the preparation of vitamin A.

Description

technical field [0001] The invention belongs to the field of chemical industry, and relates to the technology of reducing the isomerization of organic matter which is easy to isomerize in the heating process, especially the pharmaceutical intermediate which requires high purity, such as β-ionone. Background technique [0002] At present, there are several methods for rectifying β-ionone: [0003] 1. General vacuum degree (10-15mmHg), high distillation temperature (above 300°C), the result is low yield (generally less than 60%), low purity, serious isomerization in the rectification process, and the main isomerization is very large Difficult to separate α-ionone (boiling point is only 2°C different from β-ionone), up to 35%. [0004] 2. High vacuum (below 1mmHg), medium distillation temperature (about 250°C), high yield (generally less than 70%), average purity, serious isomerization in the rectification process, the main isomerization is difficult The isolated α-ionone (bo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/82C07C45/86C07C49/21
CPCC07C45/82C07C45/86C07C2601/16C07C49/21
Inventor 周祖新王爱民何卫平
Owner SHANGHAI INST OF TECH