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The preparation method of linalyl acetate

A technology of linalyl acetate and linalool, applied in the field of preparation of linalyl acetate, can solve the problems of low yield of terpineol acetate, low catalyst activity and the like, and achieve the effect of improving yield

Inactive Publication Date: 2016-08-24
WUZHOU SONGHUA AROMATIC CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The invention provides a method for preparing linalyl acetate, which can solve the problem of low yield of terpineol acetate due to the low activity of existing catalysts

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] The preparation method of this linalyl acetate comprises the following steps:

[0019] Put 1000g of linalool and 800g of acetic anhydride into a reactor, then add 6g of catalyst under a nitrogen atmosphere, and heat to 100°C for 2 hours, then distill and wash under reduced pressure to obtain;

[0020] Wherein, the intake rate of nitrogen is 10ml / min;

[0021] The preparation method of described catalyst is:

[0022] A. Put 150g of zinc oxide and 100g of rare earth carbonate into 25% ammonia solution, alkalinize for 2 hours at normal temperature, and then wash until neutral;

[0023] B. Put the zirconia and rare earth carbonate treated in step A into 60% nitric acid solution respectively, acidify for 1 hour at normal temperature, and then wash to neutrality;

[0024] C. Put the zirconia and rare earth carbonate obtained after the treatment in step B into the solution prepared by mixing 30% hydrogen peroxide solution and silicotungstic acid in a ratio of 5:2 by mass, im...

Embodiment 2

[0028] The preparation method of this linalyl acetate comprises the following steps:

[0029] Put 1000g of linalool and 850g of acetic anhydride into a reactor, then add 5g of catalyst under nitrogen atmosphere, and heat to 110°C, react for 3 hours, then distill and wash under reduced pressure to obtain;

[0030] Wherein, the intake rate of nitrogen is 12ml / min;

[0031] The preparation method of described catalyst is:

[0032] A. Put 150g of zinc oxide and 100g of rare earth carbonate into 25% ammonia solution, alkalinize for 2 hours at normal temperature, and then wash until neutral;

[0033] B. Put the zirconia and rare earth carbonate treated in step A into 60% nitric acid solution respectively, acidify for 1 hour at normal temperature, and then wash to neutrality;

[0034] C. Put the zirconia and rare earth carbonate obtained after the treatment in step B into the solution prepared by mixing 30% hydrogen peroxide solution and silicotungstic acid in a ratio of 5:2 by mas...

Embodiment 3

[0038] The preparation method of this linalyl acetate comprises the following steps:

[0039] Put 1000g of linalool and 820g of acetic anhydride into the reactor, then add 8g of catalyst under nitrogen atmosphere, and heat to 120°C, react for 1 hour, then distill and wash under reduced pressure to obtain;

[0040] Wherein, the intake rate of nitrogen is 15ml / min;

[0041] The preparation method of described catalyst is:

[0042] A. Put 150g of zinc oxide and 100g of rare earth carbonate into 25% ammonia solution, alkalinize for 2 hours at normal temperature, and then wash until neutral;

[0043] B. Put the zirconia and rare earth carbonate treated in step A into 60% nitric acid solution respectively, acidify for 1 hour at normal temperature, and then wash to neutrality;

[0044] C. Put the zirconia and rare earth carbonate obtained after the treatment in step B into the solution prepared by mixing 30% hydrogen peroxide solution and silicotungstic acid in a ratio of 5:2 by ma...

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PUM

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Abstract

The invention discloses a preparation method of linalyl acetate and belongs to the technical field of preparation of sylvichemical products. The preparation method of the linalyl acetate comprises the following steps: adding 100 parts of linalool and 80-85 parts of acetic anhydride into a reactor according to a certain ratio, then adding 0.5-0.8 part of a self-prepared catalyst under nitrogen condition, heating to 100-120 DEG C and reacting for 1-3 hours, then carrying out reduced-pressure distillation and washing to prepare the linalyl acetate. According to the method, the special self-prepared catalyst is matched with the corresponding raw material ratio and is used for controlling the corresponding nitrogen gas supply amount, so that the yield of the product, namely linalyl acetate, is increased.

Description

technical field [0001] The invention belongs to the technical field of preparation of forest chemical products, and in particular relates to a preparation method of linalyl acetate. Background technique [0002] Linalyl acetate, also known as agarwood acetate, has an elegant aroma similar to essential oils such as lily of the valley and lavender. It can be widely used in the preparation of soap essence, perfume essence, cosmetic essence, food essence and other essences. It has a wide range of uses. [0003] At present, there are many preparation techniques for linalyl acetate, but due to the low activity of the catalyst used, there is a problem of low yield in the obtained linalyl acetate. Contents of the invention [0004] The invention provides a method for preparing linalyl acetate, which can solve the problem of low yield of terpineol acetate due to the low activity of existing catalysts. [0005] In order to solve the problems of the technologies described above, the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/145C07C67/08
CPCC07C67/08C07C69/145
Inventor 陈键泉陈伟强车乾池黄宇平苏炳连董俊
Owner WUZHOU SONGHUA AROMATIC CHEM