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Method for synthesizing terpilenol

A synthesis method and technology of terpineol, applied in the direction of oxidation reaction preparation, etc., can solve the problems of pollution, catalyst breakage and damage, cost increase, etc., and achieve the effects of reducing side reactions, reducing side reactions, and reducing energy consumption.

Inactive Publication Date: 2015-06-10
FUJIAN QINGLIU MINSHAN CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As can be seen from the above studies, more domestic and foreign one-step synthesis of terpineol research all utilizes a stirred tank type scrubber to carry out the synthetic reaction of terpineol, this method generally needs organic acids as auxiliary agents, and requires a large amount of solvent to make The raw materials are fully mixed to promote the reaction, so there are still problems such as complicated separation, equipment corrosion, and serious "three wastes" pollution. More importantly, this method is easy to cause cracking and damage to the catalyst, which seriously reduces the life of the catalyst, so the cost is greatly increased.
Wei Yi et al. have made good progress in the fixed-bed scrubber process. From the effect point of view, the reaction time is still relatively long (5-13h).

Method used

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  • Method for synthesizing terpilenol
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Using turpentine and water as raw materials and isopropanol as a solvent, the mass ratio of turpentine, water and isopropanol is 5:2:3, the temperature of the dirt kettle is set at 135°C, and the temperature of the washing kettle is controlled at 70-80 °C, the porosity of the catalyst bed is 0.2-0.5, the amount of catalyst is 10% of the mass of turpentine, and the reaction time is 4h. After the reaction, the product was simply rectified to remove the solvent, and analyzed by gas chromatography, the conversion rate of α-pinene was calculated to be 91.8%, the yield of terpineol product was 66.7%, and the yield of α-terpineol was 46.7%. .

Embodiment 2

[0029] Using turpentine and water as raw materials and isopropanol as a solvent, the mass ratio of turpentine, water and isopropanol is 5:2:3, the temperature of the dirt kettle is set at 135°C, and the temperature of the washing kettle is controlled at 70-80 °C, the porosity of the catalyst bed is 0.2-0.5, the amount of catalyst is 10% of the mass of turpentine, and the reaction time is 5h. After the reaction, the product was removed by simple rectification to remove the solvent. Through gas chromatography analysis, the conversion rate of α-pinene was calculated to be 91.1%, the yield of terpineol product was 72.8%, and the yield of α-terpineol was 48.4%. .

Embodiment 3

[0031] Using turpentine and water as raw materials and isopropanol as a solvent, the mass ratio of turpentine, water and isopropanol is 5:2:3, the temperature of the dirt kettle is set at 135°C, and the temperature of the washing kettle is controlled at 70-80 °C, the porosity of the catalyst bed is 0.18-0.4, the amount of catalyst is 14% of the mass of turpentine, and the reaction time is 4h. After the reaction, the product was removed by simple rectification to remove the solvent. Through gas chromatography analysis, the calculated conversion rate of α-pinene was 97.4%, the yield of terpineol product was 65.1%, and the yield of α-terpineol was 49.3%. .

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Abstract

A method for synthesizing terpilenol relates to terpilenol. The invention provides a method for synthesizing terpilenol capable of increasing efficiency and reducing the content of byproducts. A solid acid catalyst is filled in a washing kettle; the system is closed; turpentine, water and a solvent are added to a sewage kettle via a valve; a valve between the outlet of a condenser and the inlet of the washing kettle and a valve arranged on a siphon in the vicinity of the top of the sewage kettle are opened, while other valves are closed; the sewage kettle is heated; the liquid condensed reacts through the catalyst bed in the washing kettle; the feed liquid in the washing kettle all flows back to the sewage kettle through the siphon; when the content of turpentine in the material discharged from a valve arranged at the outlet of the condenser is less than 10%, the valve between the outlet of the washing kettle and the inlet of the sewage kettle is opened so as to completely discharge the reactant liquid into the sewage kettle; heating is continued and the condensed material is completely discharged from the valve between the condenser and the washing kettle and stored; heating is stopped until no or few materials are discharged; and the product material is stored and then is separated and purified, so that the product terpilenol is obtained.

Description

technical field [0001] The present invention relates to terpineol, especially relate to a kind of synthetic method of terpineol. Background technique [0002] Terpineol has a long-lasting lilac aroma and smells of trees and flowers. It can be used as spices, printing and dyeing agents, detergents, disinfectants, and flotation agents. It is widely used in spices, printing, daily chemicals, and pesticides. , electronics, mineral processing and other industries. At present, it has been found that terpineol exists in the leaves, flowers, and grass stems of more than 200 kinds of plants, among which D-terpineol exists in plant essential oils such as cypress, cardamom, star anise, and orange blossom, and L-terpineol exists in In lavender, Melaleuca, white lemon, cinnamon leaf and other plant essential oils, racemic terpineol exists in geranium oil, Melaleuca, citronella oil, but the economic value of extracting terpineol from plant essential oils is very high. Low, and the conte...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C33/14C07C29/48
Inventor 赖杰王宏涛上官光煜张俊杰阳观生李军翁新武苏玉忠洪燕珍
Owner FUJIAN QINGLIU MINSHAN CHEM