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Longifolene purification method

A purification method, the technology of longifolene, applied in the direction of chemical change purification/separation, etc., can solve the problems of harsh reaction conditions, unsatisfactory longifolene purification effect, complicated purification process, etc., and achieve mild reaction conditions, low cost, and process and the effect of simple process

Inactive Publication Date: 2015-09-16
WUZHOU CAYIN GUM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem solved by the present invention is to provide a purification method of longifolene, which can solve the problems of unsatisfactory purification effect of longifolene, complicated purification process and harsh reaction conditions.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] This embodiment includes the following steps:

[0015] A. Under the condition of stirring, put 1000g of longifolene to be treated into the reactor, firstly heat it to 40°C, then add 120g of acetic acid solution with a concentration of 1mol / L and 60g of p-phenylene preheated to 40°C in sequence. Diphenol and 80g p-toluenesulfonic acid were stirred, and the stirring was stopped after 6 hours, and the material layer was separated by standing, and then the obtained material was washed with water and rectified to obtain the crude longifolene;

[0016] B. Put the crude longifolene obtained after the treatment in step A into another reactor, use 10 g of solid phosphoric acid as a catalyst, react at 120° C. for 3 hours, then stop the reaction, and distill under reduced pressure to obtain the finished longifolene.

[0017] The content of longifolene in the longifolene product treated in this embodiment is increased to 90%.

Embodiment 2

[0019] This embodiment includes the following steps:

[0020] A. Under stirring conditions, put 1000g of longifolene to be treated into the reactor, first heat it to 60°C, and then add 150g of acetic acid solution with a concentration of 1mol / L and 40g of p-phenylene preheated to 60°C in sequence. Diphenol and 90g p-toluenesulfonic acid were stirred, and the stirring was stopped after 10 hours, and the material layer was separated by standing, and then the obtained material was washed with water and rectified to obtain the longifolene crude product;

[0021] B. Put the crude longifolene obtained after the treatment in step A into another reactor, use 50 g of solid phosphoric acid as a catalyst, react at 125° C. for 2 hours, then stop the reaction, and distill under reduced pressure to obtain the finished longifolene.

[0022] The content of longifolene in the longifolene product treated in this embodiment is increased to 91%.

Embodiment 3

[0024] This embodiment includes the following steps:

[0025] A. Under the condition of stirring, put 1000g of longifolene to be treated into the reactor, firstly heat it to 50°C, then add 130g of acetic acid solution with a concentration of 1mol / L and 50g of p-phenylene preheated to 50°C in sequence. Diphenol and 100g p-toluenesulfonic acid were stirred, and the stirring was stopped after 8 hours, and the material layer was separated by standing, and then the obtained material was washed with water and then rectified to obtain the longifolene crude product;

[0026] B. Put the crude longifolene obtained after the treatment in step A into another reactor, use 30 g of solid phosphoric acid as a catalyst, react at 135° C. for 1 hour, then stop the reaction, and distill under reduced pressure to obtain the finished longifolene.

[0027] The content of longifolene in the longifolene product treated in this embodiment is increased to 90.5%.

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PUM

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Abstract

The present invention discloses a longifolene purification method, and belongs to the technical field of turpentine deep processing. The longifolene purification method comprises: stirring longifolene to be treated, an acetic acid solution, hydroquinone and p-toluenesulfonic acid, carrying out standing separation to obtain a material layer after stopping the stirring, sequentially carrying out water washing and rectification on the obtained material, transferring into another reactor, carrying out a reaction of the material and a solid phosphoric acid catalyst, and carrying out pressure reducing distillation on the substance obtained from the reaction. According to the present invention, the longifolene purification method has advantages of mild reaction condition, simple process and simple procedure, less equipment, and low cost; and with the longifolene purification method, the longifolene product purity can achieve more than or equal to 90%.

Description

technical field [0001] The invention belongs to the technical field of turpentine deep processing, and in particular relates to a method for purifying longifolene. Background technique [0002] Longifolene is a natural spice extracted from heavy turpentine oil. It has special chemical activity and is a raw material for synthetic resins, synthetic fragrances, flotation agents and organic synthesis. Longifolene can be used to produce isolongifolene, isolongifolene Longifolene and other products can be used in the formulation of flavors to replace some expensive spices. [0003] During the preparation of longifolene, since the boiling point of longifolene is close to that of caryophyllene in heavy turpentine, the longifolene product usually contains 10% to 12% caryophyllene, so that the purity of longifolene is only 65% to 68%, which greatly reduces the use value of longifolene. At this time, physical and chemical methods are generally used to try to eliminate the caryophylle...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C13/605C07C7/148
Inventor 黄宇平岑潮锋杨韶平刘娟娟黄蕾陈键泉
Owner WUZHOU CAYIN GUM
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