Method of manufacturing high purity alpha-terpineol

A high-purity technology of terpineol, which is applied in the field of preparation of high-purity α-terpineol, can solve the problems of products not meeting the requirements of use, difficulties in separation and purification, troublesome catalyst treatment, etc., and achieve easy purchase and industrial production , easy handling and regenerating effect

Active Publication Date: 2008-01-23
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY +1
View PDF2 Cites 17 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The α-terpineol synthetic method of my country's current report has (1) the patent [ZL 90104026.6] of people such as Xiao Shude [ZL 90104026.6] uses the one-step synthesis method of mordenite catalyst and quaternary ammonium salt emulsifier to have the method for optically active α-terpineol, gained The product is optically active dextrorotatory α-terpineol, and the catalyst treatment of this method is cumbersome, and the reaction time is as long as 30~50h. The product contains about 4% γ-terpineol, and the cost is higher; (2) Huang Kelin et al disclosed in their patent application [03178548.4] [Publication No. CN1482113] the preparation method of L-α-terpineol catalyzed by modified solid superacid. Cationic resi

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method of manufacturing high purity alpha-terpineol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A preparation method of high-purity α-terpineol, comprising the following steps:

[0028]The first step is to synthesize α-terpineol: mix turpentine oil or one of industrial-grade α-pinene or β-pinene, an organic solvent, and water, and mix them with sulfuric acid, phosphoric acid, p-toluenesulfonic acid, and chloroacetic acid. One or two or more mixtures or macroporous cation exchange resins are used as catalysts to generate α-terpineol reaction products in direct hydration reactions. In this process, by controlling turpentine or industrial-grade α-pinene or β- One of the pinene, organic solvent, water ratio and reaction temperature form a transparent homogeneous solution system method to reduce the generation of γ-terpineol, as long as the reactants form a transparent homogeneous solution system, it can effectively inhibit The generation of gamma-terpineol, thereby effectively increases the purity of alpha-terpineol, wherein the quality of catalyst is 1%~20% of turpen...

Embodiment 2

[0038] A preparation method of high-purity α-terpineol, comprising the following steps:

[0039] Step 1: The present invention uses an organic solvent as a reaction medium, water as a reaction reagent, and a macroporous cation exchange resin as a catalyst to generate α-terpineol by direct hydration in a homogeneous solution system. Raw materials can use α-pinene, β-pinene, or turpentine oil with α-pinene and β-pinene as the main components. The turpentine oil can be gum turpentine, sulfate turpentine, wood turpentine; the organic solvent can be C1~C6 Low-carbon fatty alcohols such as ethanol, isopropanol, etc., C1-C6 low-carbon fatty acids (such as acetic acid) and their esters (such as ethyl acetate), etc.; the reagent water can be distilled water, or tap water, etc., no need to carry out Special treatment; within a certain proportion range, turpentine, water, organic solvents, etc. can form a stable and uniform solution system, especially within the reaction temperature rang...

Embodiment 3

[0045] Add calculated amount of turpentine 68g (0.5mol), distilled water 11g (0.61mol) and solvent isopropanol 110g in a round bottom flask equipped with agitator, reflux condenser, and thermometer, and form a transparent homogeneous solution after stirring. All should keep homogeneous solution state in non-heating, heating and reaction process; Add catalyst D-72 macroporous cationic resin 4g (accounting for 5% of raw material quality). Heat the mixture to 90°C, adjust the heating rate to keep the reaction solution at 89-91°C, and react for about 12 hours. During the reaction, samples can be taken for follow-up analysis, and the reaction is generally stopped when the mass fraction of pinene reaches about 8%.

[0046] The mass fractions of main components in the reaction solution obtained after post-treatment are: 35.7% of α-terpineol and 0.9% of γ-terpineol (see accompanying drawing 1 for an example of GC analysis spectrum).

[0047] The mass fraction of the main component α-t...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention discloses a preparation method of the Alpha hyphen Terpinene with high purity, which comprises the following steps: first, synthesizing Alpha hyphen Terpinene: the turpentine oil or one of the Alpha hyphen pinene or Beta hyphen pinene of industrial grade is mixed with the organic solvent and the water and one or two or the mixture of the sulphuric acid, the phosphoric acid, the p-toluene sulfonic acid and the chloroactic acid or the macropore cation exchange resin are used ascatalysts to directly react with water to generate Alpha hyphen Terpinene reaction product; the generation of the Gamma hyphen Terpinene are reduced by the method of controlling the mixture ratio and the reaction temperature of the Terpinene, the organic solvent and the water to form the transparent homogeneous solution system; second, separating the Alpha hyphen Terpinene with high purity. The invention forms the transparent homogeneous solution system through the turpentine oil or one of the Alpha hyphen pinene or Beta hyphen pinene of industrial grade and the organic solvent and water, therefore effectively inhibiting the generation of the main impurity- Gamma hyphen Terpinene.

Description

technical field [0001] The invention relates to a preparation method of terpineol, in particular to a preparation method of high-purity α-terpineol. Background technique [0002] α-Terpineol is a colorless thick liquid, a monocyclic monoterpene alcohol compound, with a density of about 0.931-0.941 at 20°C, a refractive index of 1.4852-1.4850, and a boiling point of 214-224°C. It is soluble in ethanol, etc. Organic solvent, insoluble in water. α-terpineol with a mass fraction of more than 90% (the remaining 10% is basically γ-terpineol and a small amount of other isomer terpineol) has a lilac aroma and is a fine chemical with a wide range of uses. Products are often used as industrial solvents, bactericides, cleaning agents, mineral flotation agents, blending flavors, etc. There are two sources of α-terpineol, (1) it widely exists in nature, and α-terpineol has been found in more than two hundred kinds of natural essential oils. The racemate, natural α-terpineol has abunda...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C07C33/14C07C29/04
Inventor 赵振东李冬梅毕良武赵子牛米世伍王婧古研
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap