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Heliotropin rectification method

A technology of piperonal and rectification, applied in the field of medicine and chemical industry

Inactive Publication Date: 2017-09-15
江西科美香料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is no bibliographical report in this respect in the preparation literature of piperonal at present

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] A kind of rectifying method of piperonal, concrete steps are:

[0014] Add 500g piperonal crude product (wherein raw material piperonyl ring contains 10%), 200ml white oil in the 1000ml single-necked flask, connect 10cm rectifying column, fractionation device, receiving bottle;

[0015] Turn on the vacuum, measure the vacuum degree to 30Pa, start to heat up, and perform total reflux at the beginning, and start to accept the previous fraction after half an hour of full reflux. , to obtain 445g of the piperonal rectification product, the content of which is higher than 98%.

[0016] A high vacuum system is used for rectification operation, and the vacuum degree is ≤30PA.

[0017] Heat conduction oil is used to raise the temperature, and the maximum oil temperature is 250°C.

[0018] The rectification collection temperature is 100-180°C, the front fraction collection temperature is ≤150°C, and the main component collection temperature is 150-180°C.

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Abstract

The invention relates to a rectification method of piperonal. The specific steps are as follows: add 500 g of crude piperonal (wherein the raw material piperonyl ring contains 10%), 200 ml of inert solvent, connect a 10 cm rectification column, a fractionation device, and a receiving bottle into a 1000 ml single-necked flask ;Turn on the vacuum, measure the vacuum degree to be 30Pa, start to heat up, carry out total reflux at the beginning, and start to accept the previous fraction after half an hour of total reflux, the acceptance temperature of the former fraction is 100-150°C, higher than 150°C, lower than 180°C is the product pepper Aldehyde, get piperonal aldehyde rectification product 445g, content is higher than 98%. The addition of an inert solvent forms a protective layer on the surface of piperonal, which isolates the oxidation and polymerization of piperonal by a small amount of oxygen, and plays a protective role. It also reduces the risk of explosion and improves the distillation yield. .

Description

technical field [0001] The invention relates to a method for rectifying piperonal, which belongs to the field of medicine and chemical industry. Background technique [0002] Piperonal, also known as jasmonal, is widely used in various daily cosmetic flavors and food flavors, and is also widely used in medicine, pesticides, electroplating and other industries. [0003] In the rectification process of piperonal, due to the easy oxidation of aldehyde and the increase of temperature in the rectification process of piperonal, a trace amount of oxygen will promote the oxidative polymerization of piperonal, and may even cause an explosion hazard. There is no bibliographic report in this respect in the preparation literature of piperonal at present. Contents of the invention [0004] The purpose of this invention is to provide a kind of rectification method of piperonal, the method that piperonal is isolated from air during rectification, avoids piperonal oxidation, polymerizati...

Claims

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Application Information

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IPC IPC(8): C07D317/54
CPCC07D317/54
Inventor 徐兵夏铁红夏铁平夏荣良符庆强陈国勇夏治海
Owner 江西科美香料有限公司
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