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Method for synthesizing terpinum from turpentine oil and preparing terpineol and acetic ester

A technology of terpene diol and terpineol, which is applied in the field of deep processing of forestry products, can solve problems such as low yield of terpineol, large amount of waste acid treatment, and poor product aroma, and achieve easy industrial production and low corrosiveness. Low and less impurity effect

Active Publication Date: 2018-11-06
GUANGXI FORESTRY RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to overcome the problems of large amount of waste acid in the traditional two-step synthesis of terpineol, severe equipment corrosion, low yield of one-step synthesis of terpineol, and poor aroma of the product, the present invention provides a synthetic terpineol with turpentine alcohol, and further dehydrating terpene diol to prepare the method for terpineol and acetate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] A method for synthesizing terpene diol from turpentine and preparing terpineol and acetate, comprising the steps:

[0044] (1) Hydration reaction: Add turpentine, water, phosphoric acid (mass fraction 85%), glycolic acid, zinc sulfate, and acetaminophen into the reactor at a mass ratio of 100:80:80:10:1:1, Turn on the stirring, control the reaction temperature to 25°C, and the reaction time to 24h to obtain the synthetic product;

[0045] (2) The synthetic product is left to crystallize, filtered to obtain hydrated terpene diol crystals, the filtrate is left to stand for stratification, the lower layer is reused with acid water, and the upper layer is oil containing hydration products;

[0046] (3) Add the above-mentioned terpene diol crystals into the dehydration reaction kettle and add water with 3 times the mass of terpene diol, heat to 95°C, and react for 3 hours to obtain the crude terpineol product;

[0047] (4) Add the above terpene diol crystals into the esteri...

Embodiment 2

[0063] A method for synthesizing terpene diol from turpentine and preparing terpineol and acetate, comprising the steps:

[0064] (1) Hydration reaction: Add turpentine, water, phosphoric acid (mass fraction 85%), citric acid, triethanolamine borate, and acetaminophen to the reaction in a mass ratio of 100:100:80:20:1:1 In the kettle, start stirring, control the reaction temperature to 28°C, and the reaction time to 20h to obtain the synthetic product;

[0065] (2) The synthetic product is left to crystallize, filtered to obtain hydrated terpene diol crystals, the filtrate is left to stand for stratification, the lower layer is reused with acid water, and the upper layer is oil containing hydration products;

[0066] (3) Add the above-mentioned terpene diol crystals into the dehydration reaction kettle and add water with 4 times the mass of terpene diol, heat to 90°C, and react for 5 hours to obtain the crude terpineol product;

[0067] (4) Add the above-mentioned terpene dio...

Embodiment 3

[0083] A method for synthesizing terpene diol from turpentine and preparing terpineol and acetate, comprising the steps:

[0084] (1) Hydration reaction: Add turpentine, water, phosphoric acid (mass fraction 85%), malic acid, zinc acetate, and emulsifier triethanolamine into the reactor at a mass ratio of 100:150:80:8:1:1.5 , start stirring, control the reaction temperature to 28°C, and the reaction time to 30h to obtain the synthetic product;

[0085] (2) The synthetic product is left to crystallize, filtered to obtain hydrated terpene diol crystals, the filtrate is left to stand for stratification, the lower layer is reused with acid water, and the upper layer is oil containing hydration products;

[0086] (3) Add the above-mentioned terpene diol crystals into the dehydration reaction kettle and add water 5 times the mass of terpene diol, then add the oil containing hydration products in the upper layer of step (2), the amount added is 15% of the mass of terpene diol crystal...

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Abstract

The invention discloses a method for synthesizing terpinum from turpentine oil and preparing terpineol and acetic ester. The method comprises the following steps: turpentine oil, water, phosphoric acid, alpha-hydroxy acid, a cocatalyst and an emulsifier are added into a reaction kettle, stirring is started, and a synthetic product is obtained after a reaction; the synthetic product is allowed to stand for crystallization, filtering is performed to obtain a hydrated terpinum crystal, a filter liquid is allowed to stand for delamination, and the upper layer is oil containing a hydrous product; the terpinum crystal is added into a dehydration reaction kettle and water is added thereto, stirring and heating are performed, and the reaction is allowed to obtain a crude terpineol product; the terpinum crystal is added into an esterification reaction kettle, acetic anhydride is added, stirring is performed, a temperature reaction is performed to obtain a crude acetic ester product; the crude terpineol product or the ethyl ester product is neutralized by lime water, water washing is performed, and a product after the water washing is subjected to vacuum fractionation to obtain a refined terpineol or acetic ester product. The method provided by the invention has the advantages of simple process, less discharge of three wastes, mild reaction conditions, high yield of terpineol, and relatively good social, ecological and economic benefits.

Description

technical field [0001] The invention relates to the technical field of deep processing of forestry products, in particular to a method for synthesizing terpineol from turpentine and preparing terpineol and acetate. Background technique [0002] Terpineol is one of the three deep-processed products of turpentine oil. There are few natural products and it is mainly obtained through synthesis. As a main derivative of pinene, it has important applications in many fields. Terpineol has a long-lasting lilac aroma with woody and floral aromas, which can be added to soaps, cosmetics, and blended essences; in addition, terpineol has good biological activity and can be used as an insect repellant , Antibacterial agent and disinfectant; It is also widely used as non-ferrous metal flotation agent. The hydration reaction of pinene to prepare terpineol is divided into two-step method and one-step method. The two-step method is a traditional production method, and its aroma has been wide...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/00C07C35/08C07C29/60C07C33/14C07C67/08C07C69/145
CPCC07C29/00C07C29/60C07C67/08C07C2601/14C07C2601/16C07C35/08C07C33/14C07C69/145
Inventor 孟中磊
Owner GUANGXI FORESTRY RES INST
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