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Production method of isolongifolene

A production method and isofolene technology, applied in the production field of isofolene, can solve the problems of insufficient purity, affecting the purity of isofolene products, etc., and achieve the effect of high product purity

Inactive Publication Date: 2016-10-26
WUZHOU SONGHUA AROMATIC CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] When purifying longifolene from heavy turpentine, the longifolene product usually contains 10% to 12% caryophyllene due to the close boiling point of longifolene and caryophyllene in heavy turpentine oil, making the purity of longifolene insufficient 70%; and the existing isolongifolene is all longifolene with lower purity as raw material, which undoubtedly affects the purity of isolongifolene products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] The production method of isolongifolene in this example includes the following steps: adding diatomaceous earth 5A molecular sieve into the sodium salt solution, raising the temperature to 50° C. to 60° C., and keeping it warm for 2 hours to make spherical particles with a diameter of 2 mm. ℃~180℃, dry for 2 hours, and then calcine at 450℃~455℃ for 1.5 hours; put the longifolene crude product into the reaction kettle, add sodium zeolite molecular sieve, mix well, heat up to 109℃~113℃, heat preservation reaction for 30 minutes, filter to remove sodium zeolite molecular sieve, then add concentrated sulfuric acid, heat up to 120°C-123°C, heat preservation reaction for 30 minutes, add alkali solution to adjust the pH of the solution to neutral; vacuum distillation, discharge, to obtain High-purity longifolene; add macroporous ion exchange resin, add acetic acid solution, heat up to 60°C-70°C, perform isomerization reaction for 60 minutes, and filter to remove macroporous ion...

Embodiment 2

[0015] The production method of isolongifolene in this example includes the following steps: adding diatomaceous earth 5A molecular sieve into the sodium salt solution, raising the temperature to 60° C. to 65° C., and keeping it warm for 2 hours to make spherical particles with a diameter of 2 mm. ℃~180℃, dry for 2 hours, and then calcined at 462℃~472℃ for 2 hours; put the crude longifolene into the reaction kettle, add sodium zeolite molecular sieve, mix well, heat up to 100℃~105℃, Insulate and react for 40 minutes, filter to remove sodium-type zeolite molecular sieves, then add concentrated sulfuric acid, heat up to 127°C to 130°C, insulate for 35 minutes, add alkali solution to adjust the pH of the solution to neutral; distill under reduced pressure, and discharge to obtain High-purity longifolene; add macroporous ion exchange resin, add acetic acid solution, heat up to 60°C-70°C, perform isomerization reaction for 50 minutes, and filter to remove macroporous ion exchange re...

Embodiment 3

[0017] The production method of isolongifolene in this example includes the following steps: adding diatomaceous earth 5A molecular sieve into the sodium salt solution, raising the temperature to 67° C. to 70° C., and keeping it warm for 2 hours to make spherical particles with a diameter of 2 mm. ℃~180℃, dry for 2 hours, and then calcine at 489℃~493℃ for 1 hour; put the longifolin crude product into the reaction kettle, add sodium zeolite molecular sieve, mix well, and heat up to 115℃~120℃, Insulate and react for 1 hour, filter to remove sodium zeolite molecular sieve, then add concentrated sulfuric acid, raise the temperature to 120°C to 125°C, heat for 40 minutes, add alkali solution to adjust the pH of the solution to neutral; distill under reduced pressure, and discharge to obtain High-purity longifolene; add macroporous ion exchange resin, add acetic acid solution, heat up to 60°C to 70°C, perform isomerization reaction for 40 minutes, and filter to remove macroporous ion...

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PUM

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Abstract

The invention discloses a production method of isolongifolene, relating to the technical field of turpentine deep processing. The method comprises the following steps: by using longifolene as a raw material, carrying out isomerization reaction to remove caryophyllene in the longifolene so as to obtain high-purity longifolene, adding a macroporous ion-exchange resin, and carrying out isomerization reaction to obtain the isolongifolene product with higher purity.

Description

technical field [0001] The invention relates to the technical field of turpentine deep processing, in particular to a production method of isolongifolene. Background technique [0002] Isolongifolene is a product obtained by catalytic isomerization of longifolene in heavy turpentine oil. Like longifolene, it is also a sesquiterpene. It is a new type of raw material in the synthetic perfume industry. It can synthesize isolongifolene alkanone, isolongifolenone, isolongifolenol, isolongifolyl acetate, hydroxymethylisolongifene and other fragrances; it has a woody aroma, so it is widely used in the modern synthetic fragrance industry application. [0003] When purifying longifolene from heavy turpentine, the longifolene product usually contains 10% to 12% caryophyllene due to the close boiling point of longifolene and caryophyllene in heavy turpentine oil, making the purity of longifolene insufficient 70%; and the existing isolongifolene is all longifolene with lower purity as...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C13/72C07C5/29C07C13/605
CPCC07C5/29C07C2529/70C07C13/72C07C13/605
Inventor 陈键泉陈伟强车乾池黄宇平
Owner WUZHOU SONGHUA AROMATIC CHEM