Terpinyl acetate synthesizing method

A kind of technology of terpineol acetate and synthesis method, which is applied in the direction of carboxylate preparation, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of unable to meet the production requirements, large amount of catalyst used, difficult operation, etc., and achieve improvement Utilization rate, short reaction time, simple effect required

Active Publication Date: 2016-01-06
云南森美达生物科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In a word, existing terpineol acetate synthetic method still can't satisfy the requirement of production, still exists following some shortcomings:
[0007] 1) The steps are cumbersome, the process is more complicated, and the operation is difficult;
[0008] 2) The amount of catalyst is large, the conversion rate is low, the selectivity is poor, and there are many by-products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Step 1: Add 10 g of SiO 2 Mix the aerosol with 100g of 30% zinc acetate aqueous solution, heat to 70-90°C and stir for 3-5h;

[0033] Step 2: Filter the mixed solution after stirring, and the resulting solid SiO 2 Dry and activate at 100-200°C for 1-3h under reduced pressure to obtain SiO 2 supported catalyst;

[0034] Step 3: Mix 40g raw oil (containing α-pinene 98%), 18g acetic acid aqueous solution (98%) and 1g SiO 2 Loaded zinc acetate catalyst was added to the reaction flask, and stirred at 65°C for 6 hours; the reaction solution contained 1.2% of α-pinene and 72.7% of terpineol acetate by gas chromatography.

[0035] Step 4: The reaction solution is filtered to recover SiO 2 Zinc acetate catalyst was loaded, the oil phase was distilled under reduced pressure, and the chromatographic content of terpineol acetate obtained was 99.1%.

Embodiment 2

[0037] Step 1: Add 10 g of SiO 2 Mix the aerosol with 50g of 40% copper acetate aqueous solution, heat to 70-90°C and stir for 3-5h;

[0038] Step 2: Filter the mixed solution after stirring, and the resulting solid SiO 2 Dry and activate at 100-200°C for 1-3h under reduced pressure to obtain SiO 2 supported catalyst;

[0039] Step 3: Mix 40g raw oil (containing 63.2% α-pinene), 24g acetic acid aqueous solution (90%) and 0.4g SiO 2 The supported copper acetate catalyst was added to the reaction flask, and stirred and reacted at 70°C for 5 hours; the reaction solution contained 1.7% of α-pinene and 46.7% of terpineol acetate by gas chromatography.

[0040] Step 4: The reaction solution is filtered to recover SiO 2 The copper acetate catalyst was loaded, and the oil phase was distilled under reduced pressure to obtain a chromatographic content of terpineol acetate of 99.2%.

Embodiment 3

[0042] Step 1: Add 10 g of SiO 2 Mix the aerosol with 70g of 40% cobalt acetate aqueous solution, heat to 70-90°C and stir for 3-5h;

[0043] Step 2: Filter the mixed solution after stirring, and the resulting solid SiO 2 Dry and activate at 100-200°C for 1-3h under reduced pressure to obtain SiO 2 supported catalyst;

[0044] Step 3: Mix 40g raw oil (containing α-pinene 78.2%), 20g acetic acid aqueous solution (95%) and 0.8g SiO 2 Loaded cobalt acetate catalyst was added into the reaction flask, and stirred and reacted at 80°C for 4 hours; the reaction solution contained 1.3% of α-pinene and 54.6% of terpineol acetate by gas chromatography.

[0045] Step 4: The reaction solution is filtered to recover SiO 2 The cobalt acetate catalyst was loaded, and the oil phase was distilled under reduced pressure to obtain a chromatographic content of terpineol acetate of 98.7%.

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Abstract

The invention discloses a terpinyl acetate synthesizing method and particularly relates to a method for synthesizing terpinyl acetate through an alpha-pinene one-step method. The method is characterized by including the following steps that firstly, SiO2 aerosol and a lewis acid aqueous solution are mixed, heated to 70-90 DEG C and stirred for 3-5 h; secondly, the stirred mixed solution is filtered, obtained solid SiO2 is dried and activated for 1-3 h at the temperature of 100-200 DEG C under the pressure reduction condition, and a SiO2 loaded catalyst is obtained; thirdly, raw oil containing alpha-pinene, an acetic acid aqueous solution and the SiO2 loaded catalyst are added into a reaction flask and stirred for reaction; fourthly, reaction liquid is filtered, the catalyst is recycled, reduced pressure distillation is carried out on an oil phase, and high-purity terpinyl acetate can be obtained. The conversion rate of raw oil alpha-pinene is as high as 98%, selectivity of the terpinyl acetate can be over 70%, and the utilization rate of the raw oil is greatly increased. The method has the advantages of being simple in process, convenient to operate, low in production cost and the like.

Description

technical field [0001] The invention relates to a method for synthesizing terpineol acetate, in particular to a method for synthesizing terpineol acetate from alpha-pinene in one step. Background technique [0002] Terpineylacetate is also known as 1-terpene-8-ol acetate, terpineyl acetate, a-terpineylacetate, English aliases α-Terpineylacetate, 1-p-Menthen-8-yl, acetateTerpineolacetate1 ( CASNO80-26-2), has a unique aroma of lavender and bergamot, and some citrus aromas, and is widely used in food and daily flavors, often used in daily chemical flavors such as lavender, xiangwei, cologne, pine needles, and fruit. It is also used in grapefruit, citrus, orange, peach, apricot, cherry, lemon, spicy and meaty flavors, and can also be used in cardamom, marjoram, thyme and other seasoning essential oils to enhance its spicy flavor fragrance. [0003] Terpentine acetate is mainly obtained from turpentine, which is currently the most produced and cheapest essential oil in the wor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/145C07C67/04B01J31/04
CPCY02P20/584C07C67/04B01J31/04B01J2231/49C07C69/145
Inventor 崔军涛
Owner 云南森美达生物科技股份有限公司
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