Method of manufacturing high purity alpha-terpineol

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...

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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 resin is used as a catalyst, using a fixed bed process, which improves the yield, simplifies the process, and basically solves the problems of equipment corrosion and environmental pollution. However, some harmful substances such as copper, titanium, cobalt, and iron will inevitably be introduced into the product. Metal ions may make the product not meet the requirements for use in food additives, medicine and cosmetics industries

(3) There are also some other literature reports that use such as mixed acid method, heterogeneous catalysis method, chloroacetic acid catalytic hydration method, etc. to synthesize α-terpineol. Although the reaction speed is fast, the product contains more acid. Separation and purification tougher

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