Method for synthesizing terpene glycol from turpentine and preparing terpineol and acetate

A technology of terpineol ester and acetate, which is applied in the field of deep processing of forestry products, can solve the problems of low terpineol yield, large amount of waste acid treatment, and poor product aroma, and achieves easy industrial production and corrosion resistance. The effect of low sex and less impurity

Active Publication Date: 2020-10-13
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 glycol from turpentine oil and preparing terpineol and acetate, comprising the steps of:

[0044] (1) Hydration reaction: add turpentine, water, phosphoric acid (85% by mass), glycolic acid, zinc sulfate and level, and add them to the reaction kettle in a mass ratio of 100:80:80:10:1:1, Turn on stirring, control the reaction temperature to be 25°C, and the reaction time to be 24h to obtain a synthetic product;

[0045] (2) The synthetic product is left to stand for crystallization, filtered to obtain hydrated terpene glycol crystals, the filtrate is left to stand for stratification, the lower layer is acid water reuse, and the upper layer is oil containing the hydrated product;

[0046] (3) adding the above terpene glycol crystals into the dehydration reaction kettle and adding water with 3 times the mass of the terpene glycol, heating to 95°C, and reacting for 3 hours to obtain a crude terpineol product;

[0047] (4) adding the above ...

Embodiment 2

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

[0064] (1) Hydration reaction: add turpentine, water, phosphoric acid (85% by mass), citric acid, triethanolamine borate and level, and add them to the reaction at a mass ratio of 100:100:80:20:1:1 In the kettle, turn on stirring, control the reaction temperature to be 28°C, and the reaction time to be 20h to obtain a synthetic product;

[0065] (2) The synthetic product is left to stand for crystallization, filtered to obtain hydrated terpene glycol crystals, the filtrate is left to stand for stratification, the lower layer is acid water reuse, and the upper layer is oil containing the hydrated product;

[0066] (3) adding the above terpene glycol crystals into the dehydration reaction kettle and adding water with 4 times the mass of the terpene glycol, heating to 90°C, and reacting for 5 hours to obtain a crude terpineol product;

[0067] (4) a...

Embodiment 3

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

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

[0085] (2) The synthetic product is left to stand for crystallization, filtered to obtain hydrated terpene glycol crystals, the filtrate is left to stand for stratification, the lower layer is acid water reuse, and the upper layer is oil containing the hydrated product;

[0086] (3) adding above-mentioned terpene glycol crystals in the dehydration reactor and adding 5 times of terpene glycol quality water, then adding the oil of step (2) upper strata containing hydrated product, the amount added is 15% of the terpene glyc...

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Abstract

The invention discloses a method for synthesizing terpene diol from turpentine and preparing terpineol and acetate. Add turpentine, water, phosphoric acid, α-hydroxy acid, co-catalyst and emulsifier into a reaction kettle, start stirring, and react to obtain Synthetic product; the synthetic product is statically crystallized, filtered to obtain hydrated terpene diol crystals, the filtrate is allowed to stand for stratification, and the upper layer is oil containing hydration products; the above-mentioned terpene diol crystals are added to a dehydration reaction kettle and water is added, stirred and heated, react to obtain the crude terpineol product; add the above-mentioned terpene diol crystals into the esterification reaction kettle, add acetic anhydride, stir, and heat up to react to obtain the crude acetate product; use the crude terpineol product or ethyl ester product Neutralize in lime water, wash with water, and fractionate the product after washing under reduced pressure to obtain refined terpineol or acetate product. The method of the invention has the advantages of simple process, less discharge of three wastes, mild reaction conditions, high yield of terpineol, and better social, ecological and economic benefits.

Description

technical field [0001] The invention relates to the technical field of deep processing of forest chemical products, in particular to a method for synthesizing terpene glycol from turpentine and preparing terpineol and acetate. Background technique [0002] Terpineol is one of the three deep-processed products of turpentine. There are few natural products, and it is mainly obtained by synthesis. As a major derivative of pinene, it has important applications in many fields. Terpineol has a long-lasting lilac aroma with tree and floral scents, and can be added to soaps, cosmetics, and fragrances; in addition, terpineol has good biological activity and can be used as insect repellents , bacteriostatic and disinfectant; also used in large quantities as a flotation agent for non-ferrous metals. The preparation of terpineol by the hydration reaction of pinene is divided into two-step method and one-step method, wherein the two-step method is a traditional production method, and i...

Claims

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Application Information

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Patent Type & Authority Patents(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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