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Method for synthesizing terpinyl acetate from turpentine oil

A technology of terpineol acetate and turpentine oil, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds, and can solve the problems of low yield of terpineol acetate, difficult recovery of acetic acid, and difficult reuse of catalysts, etc. problems, to achieve the effect of improving product purity, reducing the discharge of three wastes, and inhibiting the occurrence of side reactions

Active Publication Date: 2018-08-17
GUANGXI FORESTRY RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention provides a method for synthesizing terpineyl acetate from turpentine in order to overcome the problems of low yield of one-step synthesis of terpineol acetate from turpentine, difficult recovery of acetic acid, and difficult reuse of catalysts

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] A method for synthesizing terpentine acetate from turpentine, comprising the following steps:

[0039] (1) Add turpentine, glacial acetic acid, citric acid and boric acid into the reaction kettle at a mass ratio of 100:200:15:3, turn on the heating and stir, control the reaction temperature to 60°C, and the reaction time to 10h;

[0040] (2) After the reaction is over, move the reaction solution into a freezing tank, cool the reaction solution to ≤10°C, and add frozen crystallized acetic acid as a seed to the reaction solution to crystallize the unreacted acetic acid in the system, then mix the reaction solution with Separation of acetic acid crystals;

[0041](3) Centrifuge the precipitated acetic acid crystals at low temperature, the temperature is controlled at ≤ 5°C, the centrifuged acetic acid crystals are used as raw materials for the next reaction, and the centrifuged liquid is mixed with the reaction liquid separated in the above step (2) to obtain a mixed liqui...

Embodiment 2

[0053] A method for synthesizing terpentine acetate from turpentine, comprising the following steps:

[0054] (1) Add turpentine, glacial acetic acid, citric acid, boric acid and acetic anhydride to the reaction kettle in a mass ratio of 100:200:20:3:10, start heating and stirring, control the reaction temperature to 12°C, and react The time is 50h;

[0055] (2) After the reaction is over, move the reaction solution into a freezing tank, cool the reaction solution to ≤10°C, and add frozen crystallized acetic acid as a seed to the reaction solution to crystallize the unreacted acetic acid in the system, then mix the reaction solution with Separation of acetic acid crystals;

[0056] (3) Centrifuge the precipitated acetic acid crystals at low temperature, the temperature is controlled at ≤ 5°C, the centrifuged acetic acid crystals are used as raw materials for the next reaction, and the centrifuged liquid is mixed with the reaction liquid separated in the above step (2) to obta...

Embodiment 3

[0068] A method for synthesizing terpentine acetate from turpentine, comprising the following steps:

[0069] (1) Add turpentine, glacial acetic acid, citric acid, boric acid and zinc sulfate into the reaction kettle at a mass ratio of 100:400:50:6:10, stir evenly, and stop when the room temperature is 15-30°C Stir and heat, place for 50h;

[0070] (2) After the reaction is over, move the reaction solution into a freezing tank, cool the reaction solution to ≤10°C, and add frozen crystallized acetic acid as a seed to the reaction solution to crystallize the unreacted acetic acid in the system, then mix the reaction solution with Separation of acetic acid crystals;

[0071] (3) Centrifuge the precipitated acetic acid crystals at low temperature, the temperature is controlled at ≤ 5°C, the centrifuged acetic acid crystals are used as raw materials for the next reaction, and the centrifuged liquid is mixed with the reaction liquid separated in the above step (2) to obtain a mixed...

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PUM

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Abstract

The invention discloses a method for synthesizing terpinyl acetate from turpentine oil, wherein the turpentine oil, glacial acetic acid and a catalyst are added into a reaction kettle, and heating andstirring are started; after the reaction is finished, a reaction liquid is transferred into a freezing tank for freezing to crystallize and precipitate unreacted acetic acid crystal in the systerm; the precipitated acetic acid crystal is centrifuged, the centrifuged acetic acid crystal is used as a raw material for the next reaction, and centrate is mixed with the reaction liquid; the liquid mixture is added to a distillation pot, water is added, stirring and heating are started, a product is accompanied by water vapor to enter an oil-water separator for separation, a separated oil layer is transported to a water washing tank, and lower layer water is returned to the distillation pot; water is added into the water washing tank for washing to obtain crude terpinyl acetate; the crude terpinyl acetate is fractionated to obtain a side product and a high purity terpinyl acetate product. The method not only can promote the conversion of pinene to the target product, pine oil ester, and improves the purity of the product, and has the advantages of simple process, less emission of three wastes, low cost, greenness, environmental protection and the like, and industrial production is easy to realize.

Description

technical field [0001] The invention relates to the technical field of deep processing of forestry products, in particular to a method for synthesizing terpineyl acetate from turpentine oil. Background technique [0002] Terpineyl acetate is also known as 1-terpene-8-ol acetate, terpineyl acetate, and a-terpineol acetate. CAS No. 80-26-2), has a unique aroma of lavender and bergamot, with citrus aroma, widely used in edible and daily flavors, often used in lavender, fragrant, cologne, pine needles, fruity, etc. It is also used in food flavors such as pomelo, citrus, orange, peach, apricot, cherry, lemon, spice and meat, and can also be used to enhance cardamom, marjoram, thyme and other seasoning essential oils Its spicy fragrance. [0003] In the industry, catalysts such as sulfuric acid and phosphoric acid are used, and terpineol and acetic acid or acetic anhydride are used as raw materials for esterification and then fractionated. There are many disadvantages such as la...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C67/58C07C67/54C07C69/145
CPCC07C67/08C07C67/54C07C67/58C07C2601/16C07C69/145
Inventor 孟中磊蒋剑春梁忠云李桂珍杨漓周丽珠秦荣秀谷瑶陈海燕温如丝
Owner GUANGXI FORESTRY RES INST
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