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Method for synthesizing isobornyl acetate by camphene

A technology for isobornyl acetate and camphene, which is applied in the field of synthesizing isobornyl acetate from camphene, can solve the problems of difficult preparation of catalysts, difficult to reuse, easy to deactivate, etc., and achieves the advantages of being conducive to industrialized popularization and application, low cost, easy separation effect

Active Publication Date: 2018-11-23
GUANGXI FORESTRY RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention provides a method for synthesizing isobornyl acetate from camphene in order to overcome the problems of difficult catalyst preparation, easy deactivation, and difficult reuse of catalysts in the synthesis of isobornyl acetate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] A method for synthesizing isobornyl acetate from camphene, comprising the steps of:

[0033] (1) Synthesis reaction: camphene (commercially available camphene, containing 75.8% camphene and 17.3% tricyclic terpene, the same as in the following examples), glacial acetic acid, lactic acid, and boric acid, in a mass ratio of 100:200:18: The proportion of 2 was added to the reaction kettle, the stirring was started, the reaction temperature was controlled at 55°C, and the reaction time was 20h to obtain the synthetic product;

[0034] (2) Preliminary separation of the product: add 20% water of camphene mass to the synthetic product obtained in step (1), let it stand for stratification, the lower layer is acid water containing catalyst and acetic acid, and the upper oil layer is isobornyl acetate target product;

[0035] (3) Deacidification of the product: Add the above-mentioned target product into a washing tank, first add alkaline water to neutralize, and then add water ...

Embodiment 2

[0045] A method for synthesizing isobornyl acetate from camphene, comprising the steps of:

[0046] (1) Synthesis reaction: Add camphene, glacial acetic acid, mandelic acid, boric acid and acetic anhydride to the reaction kettle at a mass ratio of 100:100:20:3:10, start stirring, and control the reaction temperature to 85°C , The reaction time is 8h, and the synthetic product is obtained;

[0047] (2) Preliminary separation of the product: add 10% water of camphene mass to the synthetic product obtained in step (1), let it stand for stratification, the lower layer is acid water containing catalyst and acetic acid, and the upper oil layer is isobornyl acetate target product;

[0048] (3) Deacidification of the product: Add the above-mentioned target product into a washing tank, first add alkaline water to neutralize, and then add water to wash 3 times to obtain the crude product of isobornyl acetate;

[0049] (4) Product purification: The crude product is subjected to vacuum ...

Embodiment 3

[0058] A method for synthesizing isobornyl acetate from camphene, comprising the steps of:

[0059] (1) Synthetic reaction: Add camphene, glacial acetic acid, DL-mandelic acid, boric acid and zinc acetate into the reactor at a mass ratio of 100:250:25:6:10, start stirring, and control the reaction temperature to 65°C, the reaction time is 24h, and the synthetic product is obtained;

[0060] (2) Preliminary separation of the product: Add 80% water of camphene mass to the synthetic product obtained in step (1), let it stand for stratification, the lower layer is acid water containing catalyst and acetic acid, and the upper oil layer is isobornyl acetate target product;

[0061] (3) Deacidification of the product: Add the above-mentioned target product into a water washing tank, add alkaline water to neutralize it, and then add water to wash it twice to obtain the crude product of isobornyl acetate;

[0062] (4) Product purification: The crude product is subjected to vacuum fra...

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PUM

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Abstract

The invention discloses a method for synthesizing isobornyl acetate by camphene. The method comprises the following steps of adding camphene, glacial acetic acid, a main catalyst (hydroxycarboxylic acid) and an additive into a reaction kettle according to a mass ratio of 100:(20 to 400):(1 to 50):(1 to 20), starting to stir, controlling the temperature to 40 to 100 DEG C, and reacting for 2 to 24h, so as to obtain a synthesized product; adding a small amount of water into the synthesized product, standing and delaminating, wherein the upper oil layer is a target product containing isobornyl acetate, the lower layer is acid water containing the catalyst and acetic acid, and the acid water is dewatered and recycled; adding the target product into a water washing tank, adding alkaline water to neutralize, and then adding water to wash, so as to obtain a crude product of the isobornyl acetate; relieving pressure and distilling, so as to obtain the refined isobornyl acetate. The method forsynthesizing the isobornyl acetate by catalyzing the camphene has the advantages that the obtained product has high yield and high purity, and is easy to separate; the used catalyst has high catalyzing activity; the preparation is simple, the repeatability is good, the toxicity is avoided, the corrosion property is low, the isobornyl acetate belongs to regeneration resources, and the industrialization product is easy.

Description

technical field [0001] The invention relates to the technical field of deep processing of forestry products, in particular to a method for synthesizing isobornyl acetate from camphene. Background technique [0002] Isobornyl Acetate is a colorless liquid or crystalline powder, which has the same aroma as Bornyl Acetate and is more refreshing. Isobornyl acetate is produced by the reaction of camphene and acetic acid. It is mainly used as an intermediate in the synthesis of camphor. It is also commonly used as a flavoring agent for daily chemicals such as soap, talcum powder, toilet water, and air sprays. Isoborneol, also known as isoborneol, has a smell similar to camphor. It is used as a spice in daily chemical products and also as a preservative. The appearance and properties of white isoborneol are similar to camphor, and the cost is relatively low. It is gradually being used in many fields. As a substitute for camphor, the application prospect is very broad. Isoborneol ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/04C07C69/14B01J31/22B01J31/04B01J31/14
CPCB01J31/04B01J31/146B01J31/2213B01J31/2226C07C67/04C07C2602/42C07C69/14
Inventor 孟中磊蒋剑春
Owner GUANGXI FORESTRY RES INST
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