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A kind of method that camphene synthesizes isobornyl acetate

A technology of isobornyl acetate and amphene, which is applied in the field of synthesizing isobornyl acetate from amphene, can solve the problems of difficult reutilization, difficult preparation of catalysts, easy deactivation, etc., and achieves the benefits of industrial promotion and application, low cost, easy separation effect

Active Publication Date: 2021-08-24
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 from amphene. The mass ratio of amphene, glacial acetic acid, main catalyst hydroxycarboxylic acid and co-catalyst is 100:20-400:1-50:1-20 The proportion of the mixture is added to the reaction kettle, the stirring is started, the temperature is controlled at 40-100°C, and the reaction is 2-24h to obtain the synthetic product; add a small amount of water to the synthetic product, let it stand for layers, and the upper oil layer is isobornyl acetate The target product, the lower layer is acid water containing catalyst and acetic acid, and the lower layer of acid water is recycled after dehydration; the target product is added to the washing tank, first neutralized with alkaline water, and then washed with water to obtain the crude product of isobornyl acetate ; Then carry out fractional distillation under reduced pressure to obtain refined isobornyl acetate. The method catalyzes camphene to synthesize isobornyl acetate, and the obtained product has high yield and high purity, and the product is easy to separate. Renewable resources, easy to realize industrial production.

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 Patents(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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