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High-purity Delta terpilenol separation and purification method

An extraction method and technology for terpineol, which are applied in the field of separation and extraction of high-purity delta-terpineol, can solve the problems of low purity of delta-terpineol and difficulty in rectification, and achieve the effect of improving the purity

Active Publication Date: 2014-09-17
宜宾石平香料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The present invention aims to solve the problems of difficult rectification and low purity of δ-terpineol in the prior art, and proposes a separation and extraction method of high-purity δ-terpineol, which can make the purity of δ-terpineol reach 99% %above

Method used

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  • High-purity Delta terpilenol separation and purification method

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Effect test

Embodiment 1

[0020] A method for separating and extracting high-purity delta terpineol, comprising the following steps:

[0021] A. Rectification: Add 3000kg of δ-terpineol raw material into the packed rectification tower, the heating temperature of the tower kettle is 210°C, the temperature of the tower top is 80~150°C, the vacuum degree of the rectification tower is 750mmHg~760 mmHg, heat The final steam keeps rising, and through the cycle process of rectification, condensation, reflux and rectification for many times, according to the different boiling points of the main components in camphor oil (among them, β-caryophyllene 130°C, camphor 204°C, δ-pine oleyl alcohol at 210°C, terpinene-4-ol at 212°C and a-terpineol at 219°C) and collected separately, the reflux ratio was controlled to 800:1, and the fraction at 210±1°C was collected to obtain 500kg of crude δ-pine Oleyl alcohol, the content of δ-terpineol after analysis is 85%;

[0022] B, crystallization: After heating and meltin...

Embodiment 2

[0025] A method for separating and extracting high-purity delta terpineol, comprising the following steps:

[0026] A, rectification: 3000kgδ-terpineol raw material is added in the packed rectification tower, and tower kettle heating temperature is 215 ℃, and the temperature of tower top is 80~150 ℃, and the vacuum degree of rectification tower is 750mmHg~760 mmHg, will The reflux ratio was controlled at 850:1, and the fraction at 210±1°C was collected to obtain 550kg of crude δ-terpineol. After analysis, the content of δ-terpineol was 82.5%;

[0027] B, crystallization: after heating and melting the crude δ-terpineol obtained in step A, mix with ethanol with a concentration of 98% at a mass ratio of 2:5, and crystallize at 8° C. for 4 days after mixing;

[0028] C, centrifugation: add the material after the crystallization is completed in the centrifuge, the centrifuge speed is 1800r / min, let it stand after centrifuging for 10min, collect the crystallization product, repeat s...

Embodiment 3

[0031] A method for separating and extracting high-purity delta terpineol, comprising the following steps:

[0032] A. Rectification: Add 3500kg of δ-terpineol raw material into the packed rectification tower, the heating temperature of the tower kettle is 218°C, the temperature at the top of the tower is 80-150°C, the vacuum degree of the rectification tower is 750mmHg-760 mmHg, heat The final steam rises continuously, and is collected separately according to the boiling points of the main components in the camphor oil through repeated rectification, condensation, reflux, and rectification cycles. The cut of ℃ obtains the thick δ-terpineol of 506kg, and the content of δ-terpineol is 90% after analysis;

[0033] B, crystallization: After heating and melting the crude δ-terpineol obtained in step A, mix it with 90% ethanol at a mass ratio of 1:5, and crystallize at 10° C. for 2 days after mixing;

[0034] C. Centrifugal separation: add the material obtained after crystallizati...

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Abstract

The invention discloses a high-purity Delta terpilenol separation and purification method, which comprises the following steps: A, rectification, namely adding a Delta-terpilenol raw material to a rectifying tower, controlling the reflux ratio to be (800-1000) to 1, and collecting fractions of 210+ / -1 DEG C to obtain crude Delta-terpilenol, wherein the heating temperature of the tower is 210-220 DEG C, the tower top temperature is 80-150 DEG C, the vacuum degree of the rectifying tower is 750mmHg to 760mmHg; B, crystallization, namely heating the crude Delta-terpilenol to a molten state, mixing the molten crude Delta-terpilenol with 90-98% ethanol according to a mass ratio f 1 to (2.5-5), and crystalizing for 1-5 days at 5-10 DEG C; and C, centrifugal separation, namely adding the crystallized material to a centrifugal machine, centrifuging for 10-30 minutes and then standing, and collecting the crystallized product, wherein the rotation speed of the centrifugal machine is 1500-2000r / min. Due to the adoption of the method, the Delta-terpilenol with the purity being above 99 percent can be obtained by separation.

Description

technical field [0001] The invention relates to a method for purifying chemical products, in particular to a method for separating and extracting high-purity delta terpineol. Background technique [0002] Terpineol, also known as terpineol, refers to at least four monocyclic terpineol compounds with molecular formula C10H18O, namely α-terpineol, β-terpineol, γ-terpineol and δ-terpineol, Has a lilac scent. It has a wide range of applications, mainly used in the preparation of flavors, medicine, pesticides, plastics, soap, and ink industries, and can also be used as a solvent for colors on glassware. The melting points of α-terpineol, β-terpineol, γ-terpineol and δ-terpineol increase in order from small to large, and the difficulty in the rectification process is also increasing. The most common α-terpineol The melting point of alcohol is about 30°C, the rectification and purification is relatively simple, and the product purity is high, while the melting point of δ-terpineo...

Claims

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Application Information

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IPC IPC(8): C07C33/14C07C29/76C07C29/80
CPCC07C29/76C07C29/78C07C29/80C07C2601/16C07C33/14
Inventor 江石平
Owner 宜宾石平香料有限公司
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