Preparation method of terpinyl acetate

A technology of terpineol acetate and terpineol, applied in the field of preparation of terpineol acetate, can solve the problems of low yield, low purity of terpineol acetate, low catalyst activity, etc., and achieve the effect of improving purity and yield

Inactive Publication Date: 2015-09-23
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 terpineol acetate, which can solve the problems of low purity and low yield of terpineol acetate produced 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 terpineol acetate comprises the following steps:

[0019] Put 1000g terpineol and 500g acetic anhydride into the reactor, then add 3g catalyst under nitrogen atmosphere, and heat to 50°C, react for 6 hours, then distill and wash under reduced pressure to obtain;

[0020] Wherein, the intake rate of nitrogen is 5ml / min;

[0021] The preparation method of described catalyst is:

[0022] A. Put 150g of zirconia and 100g of rare earth carbonate into 60% nitric acid solution respectively, acidify for 1 hour at normal temperature, and then wash until neutral;

[0023] B, put into 15% sodium hydroxide solution respectively through the zirconium oxide and the rare earth carbonate treated in step A, alkalinize 2 hours under normal temperature, then wash to neutrality;

[0024] C, put the zirconia and rare earth carbonate obtained after the B step treatment into the solution prepared by mixing hydrogen peroxide and 80% phosphoric acid in a ratio o...

Embodiment 2

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

[0029] Put 1000g of terpineol and 400g of acetic anhydride into the reactor, then add 1g of catalyst under nitrogen atmosphere, and heat to 60°C, react for 4 hours, then distill and wash under reduced pressure to obtain;

[0030] Wherein, the intake rate of nitrogen is 8ml / min;

[0031] The preparation method of described catalyst is:

[0032] A. Put 150g of zirconia and 100g of rare earth carbonate into 60% nitric acid solution respectively, acidify for 1 hour at normal temperature, and then wash until neutral;

[0033] B, put into 15% sodium hydroxide solution respectively through the zirconium oxide and the rare earth carbonate treated in step A, alkalinize 2 hours under normal temperature, then wash to neutrality;

[0034] C, put the zirconia and rare earth carbonate obtained after the B step treatment into the solution prepared by mixing hydrogen peroxide and 80% phosphoric acid in ...

Embodiment 3

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

[0039] Put 1000g of terpineol and 450g of acetic anhydride into a reactor, then add 5g of catalyst under a nitrogen atmosphere, heat to 55°C, react for 5 hours, then distill and wash under reduced pressure to obtain;

[0040] Wherein, the intake rate of nitrogen is 10ml / min;

[0041] The preparation method of described catalyst is:

[0042] A. Put 150g of zirconia and 100g of rare earth carbonate into 60% nitric acid solution respectively, acidify for 1 hour at normal temperature, and then wash until neutral;

[0043] B, put into 15% sodium hydroxide solution respectively through the zirconium oxide and the rare earth carbonate treated in step A, alkalinize 2 hours under normal temperature, then wash to neutrality;

[0044] C, put the zirconia and rare earth carbonate obtained after the B step treatment into the solution prepared by mixing hydrogen peroxide and 80% phosphoric acid in a r...

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PUM

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Abstract

The invention discloses a preparation method of terpinyl acetate and belongs to the technical field of preparation of sylvichemical products. The preparation method of terpinyl acetate comprises the following steps: adding terpilenol and acetic anhydride into a reactor according to a certain ratio, then adding a self-prepared catalyst under nitrogen condition, heating to 50-60 DEG C and reacting for 4-6 hours, then carrying out reduced-pressure distillation and washing to prepare terpinyl 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 purity and the yield of the product, namely terpinyl acetate, are improved.

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 terpineol acetate. Background technique [0002] Terpineol acetate is the esterification product of terpineol. It is an important general-purpose fragrance. It has a delicate and sweet fragrance, like bergamot and lavender, and has a long fragrance retention time. It is widely used in lavender, vanilla and cologne It is also commonly used in food flavors such as spice and meat, as well as flavoring essential oils such as cardamom, marjoram and thyme. [0003] At present, there are many preparation techniques for terpineol acetate, but due to the low activity of the catalyst used, the obtained terpineol acetate has the problems of low purity and low yield. Contents of the invention [0004] The invention provides a preparation method of terpineol acetate, which can solve the problems of low purity and low yield...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/145C07C67/08
CPCC07C67/08C07C2601/16C07C69/145
Inventor 陈键泉陈伟强黄宇平车乾池黄蕾岑潮锋
Owner WUZHOU SONGHUA AROMATIC CHEM
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