One-step method for synthesizing fenchol with turpentine

A technology for turpentine and fenol, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of oxygenated compounds, etc., can solve the problems of difficulty in obtaining high-purity fenol products, limited sources of raw materials, long process routes, etc. variety, increase fiscal revenue, and reduce costs

Inactive Publication Date: 2011-11-16
广西辰康生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a kind of turpentine one-step synthetic method in order to overcome the problems of limited source of raw materials, long process route, high operating cost, high energy consumption, and difficulty in obtaining high-purity fenchol products in the prior art for the preparation of fenchol Fenulol method

Method used

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  • One-step method for synthesizing fenchol with turpentine
  • One-step method for synthesizing fenchol with turpentine
  • One-step method for synthesizing fenchol with turpentine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] (1) Process setting:

[0042] Raw material formula (parts by weight): 12 parts of turpentine, 0.48 parts of a catalyst with a 1:1 ratio of inorganic acid and metal oxide, 2.26 parts of an esterifying agent with a 1:0.6 ratio of oxalic acid and oxalic acid, and 0.04 parts of an aromatic hydrocarbon additive.

[0043] Process parameters: Esterification temperature 85°C, esterification time 20h, first washing standing for 18h, saponification temperature 85°C, saponification time 7h, second washing standing 16h, fractionation A top temperature control is less than 100°C, fractionation B top temperature Control 100 ~ 140 ℃, crystallization temperature 2 ℃.

[0044] (2) Preparation method:

[0045] Add turpentine, catalyst, esterifying agent, and additives into a 20L glass reactor respectively, stir and raise the temperature to 85°C, and keep it for 20h. Sampling was carried out, and the reaction mixture was detected by GC. The pinene content was 0.42% (99.5% conversion rat...

Embodiment 2

[0049] (1) Process setting:

[0050] Raw material formula (parts by weight): 12 parts of turpentine, 0.60 part of catalyst of kaolin and metal oxide ratio of 1:1, 2.4 parts of esterifying agent of oxalic acid, p-toluenesulfonic acid and oxalic acid of 0.8:1:0.3 ratio, aliphatic hydrocarbon 0.06 part of auxiliary agent.

[0051] Process parameters: Esterification temperature 95°C, esterification time 22h, first wash and stand for 20h, saponification temperature 90°C, saponification time 6.5h, second wash stand for 20h, fractionation A top temperature control is less than 100°C, fractionation B top The temperature is controlled at 100-140°C, and the crystallization temperature is 8°C.

[0052] (2) Preparation method:

[0053] Add turpentine, catalyst, esterification agent and auxiliary agent respectively into a 20L glass reactor, stir and raise the temperature to 95°C, and keep it for 22h. Sampling was carried out, and the reaction mixture was detected by GC. The pinene content...

Embodiment 3

[0057] Raw material formula (parts by weight): 200 parts of turpentine, 100 parts of a mixture of by-product borneol, isoborneol and terpene in a ratio of 0.5:0.3:2, 13.9 parts of a catalyst of kaolin, inorganic acid and metal oxide in a ratio of 1:0.5:0.5 , 60 parts of an esterification agent with a ratio of 0.6:1 between oxalic acid and p-toluenesulfonic acid, and 1.2 parts of an auxiliary agent with a ratio of 1:0.5 between aromatic hydrocarbons and aliphatic hydrocarbons.

[0058] Preparation:

[0059] Add turpentine, by-product mixture, catalyst, esterification agent, and additives into a 500L enamel reaction kettle, stir and raise the temperature to 110°C, and keep it for 20h. Sampling was carried out, and the reaction mixture was detected by GC. The pinene content was 1.04% (98.4% conversion rate), and the reaction was stopped. The esterification reaction product was washed with water and left to stand for 24 hours to separate the oil layer and water layer mixture. Ad...

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Abstract

The invention discloses a one-step method for synthesizing fenchol with turpentine. In the method, turpentine is used as a raw material, CHKC-4 is used as a catalyst, the catalytic characteristics of the catalyst, namely high activity and selectivity are utilized to perform catalytic isomerization and hydration on pinene (terpene), isomerization and hydration are completed in one step, and then physical methods and chemical methods are combined, and various advanced separation technologies such as efficient vacuum fractionation and melt crystallization are utilized to perform assembly and integration and prepare the fenchol product of which the yield is no less than 50% and purity is 99%. The method has the following advantages: turpentine is used as a raw material which is abundant, is easy to obtain and has low cost, the synthesis and separation technologies are simple, the method is convenient to operate, the product has high purity and lower production cost, etc. The technology and cost of the method are obviously superior, and the competition of the product in international markets can be increased.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and relates to a method for synthesizing fenchol from turpentine in one step. Background technique [0002] Fenchyl alcohol, also known as fenchyl alcohol or fenchol, is a rare and expensive spice and chemical raw material, mainly used for the deployment of medicinal, lemon, citrus flavors and certain woody, grassy, ​​and floral flavors. It is also widely used as an intermediate in the synthesis of fine chemicals. Fenchol was first found naturally in the essential oil of old roots of longleaf pine, and was subsequently found in other plants. As a newly developed spice variety, fenchol has high added value, and it is currently only produced in a few countries such as Spain and India. There is no production of this product in China, and domestic consumption is completely dependent on imports. [0003] At present, the technological routes for the production of fenchol in the world include:...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C35/29C07C35/30C07C27/02
Inventor 何春茂陈祖洪张可钦邓倩李华杰吴明凤朱金忠
Owner 广西辰康生物科技有限公司
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