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Method for producing coumarin intermediate through microreactor in pilot-plant-scale manner

A technology of microreactor and coumarin, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of many side reactions and low yield, and achieve good product quality, low energy consumption, The effect of high operational safety

Inactive Publication Date: 2015-05-27
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to provide a method for large-scale production of coumarin intermediates in a microreactor pilot scale to solve the problems of many side reactions and low yields in the prior art

Method used

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  • Method for producing coumarin intermediate through microreactor in pilot-plant-scale manner
  • Method for producing coumarin intermediate through microreactor in pilot-plant-scale manner
  • Method for producing coumarin intermediate through microreactor in pilot-plant-scale manner

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] In the micro-reaction device, the diameter of the connecting pipe is 1cm, the length of the inlet pipe is 2m, the length of the connecting pipe between the T-shaped valve and the microchannel reactor is 3m, and the length of the connecting pipe between the microreactor and the outlet is 3m; The volume of the microchannel reactor is 250L.

[0026] Weigh 40kg of salicylaldehyde and add it into container A; weigh 42kg and 5kg of acetic anhydride and acetic acid into container B, then weigh 1.9kg of potassium acetate and heat and stir until homogeneous. The two materials are mixed and pumped into the microchannel reactor through the T-valve. The reaction fluid of pump A flows through the microreactor at 10L / min, and the fluid of pump B flows through the microreactor at 15L / min. The reaction time is 10min, the temperature of the reactor is 160°C, and the crude product is collected through cooling at the outlet; the conversion is calculated by HPLC rate, the conversion rate ...

Embodiment 2

[0028] The micro-reaction device is basically the same as in Example 1, except that the diameter of the pipeline of this microchannel reactor is 1cm, the length of the liquid inlet pipe is 2m, and the length of the connecting pipe between the inlet and the microreactor is 3m , the length of the connecting pipe between the microreactor and the outlet is 3m; the volume of the microchannel reactor is 250L.

[0029] Weigh 40kg of salicylaldehyde and add it into container A; weigh 42kg and 5kg of acetic anhydride and acetic acid into container B, then weigh 1.9kg of potassium acetate and heat and stir until homogeneous. The two materials are mixed and pumped into the microchannel reactor through the T-valve. The reaction fluid of pump A flows through the microreactor at 20L / min, and the fluid of pump B flows through the microreactor at 30L / min. The reaction time is 5min, the temperature of the reactor is 140°C, and the crude product is collected after cooling at the outlet; the con...

Embodiment 3

[0031] The micro-reaction device is basically the same as in Example 1, except that the diameter of the pipeline of this microchannel reactor is 1cm, the length of the liquid inlet pipe is 2m, and the length of the connecting pipe between the inlet and the microreactor is 3m , the length of the connecting pipe between the microreactor and the outlet is 3m; the volume of the microchannel reactor is 250L.

[0032] Weigh 40kg of salicylaldehyde and add it into container A; weigh 42kg and 5kg of acetic anhydride and acetic acid into container B, then weigh 1.9kg of potassium acetate and heat and stir until it is homogeneous. The two materials are mixed and pumped into the microchannel reactor through the T-valve. The reaction liquid fluid of pump A flows through the microreactor at 13L / min, and the reaction liquid fluid of pump B flows through the microreactor at 20L / min. The reaction time is 7.6min, the reactor temperature is 140°C, and the crude product is collected after coolin...

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Abstract

The invention discloses a method for producing coumarin intermediate through microreactor in a pilot-plant-scale manner. The method comprises the following steps: preparing potassium acetate, acetic anhydride and acetic acid into homogenous solution, pumping salicylaldehyde into a microreaction device, and reacting to obtain the coumarin intermediate. Compared with the prior art, the method is simple in technology, can conduct continuous production, has higher operation safety and high selectivity, the reaction is small, the time is short, the catalyst can be repeatedly utilized, and the corrosion to equipment is small; in addition, by utilizing the high-efficiency heat mass transfer capability and easily direct amplification of the micro-channel reactor, the conversion rate is up to more than 99%, the coumarin intermediate is good in quality, low in energy consumption, and thus the method is a green, environment-friendly and high-efficiency method for synthesizing the courmarin intermediate.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a method for producing a coumarin intermediate in a microreactor pilot scale. Background technique [0002] Coumarin (coumarin, C 9 h 6 o 2 ), also known as 1,2-benzopyrone, is a lactone compound that exists in nature and is widely distributed in higher plants, especially Rutaceae and Umbelliferae. It is also widely found in plants, and a few are found in animals and microorganisms. Coumarin has a variety of physiological activities, and has dual physiological activities on plants. It is a plant hormone at low concentrations, but it can inhibit plant growth at high concentrations; it has anti-AIDS, anti-tumor, anti-oxidation, and anti-microbial effects on the human body. , antihypertensive, anti-radiation and many other physiological activities. In addition, coumarin is also commonly used in scented daily cosmetics such as violet, Suxinlan, sunflower, orchid, so...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/157
CPCC07C67/08C07C69/157Y02P20/584
Inventor 郭凯黄玲玲李昕陈安邦张锴
Owner NANJING UNIV OF TECH
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