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Preparation method of high-purity longifolene

A longifolene, high-purity technology, applied in chemical instruments and methods, distillation purification/separation, hydrocarbon purification/separation, etc., can solve the problem of low content of longifolene products

Inactive Publication Date: 2013-12-18
WUZHOU SONGHUA AROMATIC CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The invention provides a method for preparing high-purity longifolene to solve the problem that the content of longifolene obtained in the existing longifolene production is not high

Method used

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  • Preparation method of high-purity longifolene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] The small-scale test method of this high-purity longifolene, enters 100 grams of 65% longifolene primary products in a 250-gram three-necked flask with a thermometer, a stirrer and a spherical condenser as a raw material, and then adds 10 grams of high-efficiency solid acid D113 is used as a catalyst, i.e. macroporous weakly acidic acrylic cation exchange resin D113, then start the agitator to start heating, the reaction temperature is controlled at 60°C°, and the caryophyllene content is sampled and analyzed after 3 hours, and the sample is taken every 0.5-1 hour , until the content of caryophyllene is less than 3%, stop adding and start to cool down, lower the temperature to below 40 degrees, then filter in turn, recover the catalyst, and finally obtain the analysis results of the crude product of longifolene: the content of longifolene is 68.755%, and the content of caryophyllene is 2.2% %. The longifolene crude product is distilled and rectified, and the longifolene...

Embodiment 2

[0013] Expanded test of this high-purity longifolene: add 10,000 grams of 60% longifolene in a 20L reactor with condensation and stirring device, and then add 1000 grams of high-efficiency solid acid D113 as a catalyst, that is, macroporous weakly acidic Acrylic cation exchange resin D113, then start the agitator to start heating, control the reaction temperature to 90°C, take samples and analyze the caryophyllene content after 3 hours, take a sample every 0.5-1 hour, stop until the caryophyllene content is less than 3% After adding, the temperature was lowered, and the temperature was lowered to below 40 degrees, followed by filtration and catalyst recovery. Finally, the analysis results of the crude longifolene were obtained: the content of longifolene was 62.245%, and the content of caryophyllene was 2.3%. The longifolene crude product is distilled and rectified, and the longifolene with the required content (more than 80%, 85% or 90%) is intercepted according to the custome...

Embodiment 3

[0016] The pilot test implementation of this high-purity longifolene is as follows: add 63% longifolene 100kg longifolene / pot in the pilot test reactor, and then add 10kg high-efficiency solid acid D113 as a catalyst, that is, macroporous weakly acidic acrylic acid It is cation exchange resin D113, then start the agitator to start heating, control the reaction temperature to 110°C, take a sample to analyze the caryophyllene content after 3 hours, take a sample every 0.5-1 hour, stop adding until the caryophyllene content is less than 3%. Lower the temperature to below 40 degrees, then filter and recover the catalyst in sequence, and finally obtain the analysis results of the crude longifolene: the content of longifolene is 63.135%, and the content of caryophyllene is 2.5%. The longifolene crude product is distilled and rectified, and the longifolene with the required content (more than 80%, 85% or 90%) is intercepted according to the customer's index requirements, which is the ...

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Abstract

The invention discloses a preparation method of high-purity longifolene. The preparation method comprises the following steps: placing mixture of 65-70 percent by weight of longifolene and 10-30 percent by weight of caryophyllene into a reaction container; adding a catalyst to perform caryophyllene polymerization reaction, wherein the reaction heating temperature is 80-110 DEG C and the reaction time is 3-6 hours; filtering; recovering the catalyst; performing reduced pressure distillation; rectifying to obtain the longifolene finished product with content of 85-95 percent, wherein the catalyst is macroporous weakly acidic acrylic acid cation exchange resin D113; the weight ratio of the mixture to the catalyst is 1:0.05-0.1. Compared with the prior art, the preparation method has the advantage that the problems of difficulty in separation of the high-purity longifolene and high production cost existing in the prior art can be solved.

Description

technical field [0001] The invention relates to the technical field of chemical pine resin deep processing, in particular to a preparation method that can relatively easily obtain high-content longifolene. Background technique [0002] At present, the purification of longifolene in turpentine heavy oil is generally achieved by vacuum distillation, but it is difficult to purify longifolene to more than 80% by vacuum distillation, because the heavy oil contains a caryophyllene component, caryophyllene The boiling point and physical properties of caryophyllene are very close to those of longifolene. The content ratio of caryophyllene to longifolene is between 1:3 and 4 according to different tree species. It is difficult to separate the two by fractional distillation, so without The treated turpentine heavy oil can only be distilled to obtain longifolene with a content of 65% to 70%. In order to meet customer requirements and increase the content of longifolene, new technologi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C13/605C07C7/00C07C7/148C07C7/04
CPCY02P20/584
Inventor 陈键泉陈伟强孔仕才车乾池黄宇平杨振洲梁利诚苏炳连李战
Owner WUZHOU SONGHUA AROMATIC CHEM
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