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Method for synthesizing carane by hydrogenation of 3-carene

A kind of technology of carene and carane

Inactive Publication Date: 2016-01-27
WUZHOU SONGHUA AROMATIC CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of this invention is to provide a kind of method for the synthesis of carane by hydrogenation of 3-carene, the method can solve the problem that the purity and productive rate of the carane product that prior art makes are not high enough

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The method for the synthesis of carane by hydrogenation of 3-carene comprises the following steps:

[0017] A. Put 80g of 3-carene mixture with a 3-carene content of 95.1% and 1.6g of nickel catalyst into the reaction kettle, first replace it with nitrogen three times, then replace it with hydrogen three times, then pass in hydrogen, and then control the inside of the kettle The hydrogen pressure in the reactor is 0.08MPa, and then heating is started, so that the temperature of the reaction material in the reactor reaches 50°C, and the pressure-holding and heat-retaining reaction is carried out;

[0018] B. When the content of 3-carene in the reaction material of the reactor is less than or equal to 60%, adjust the hydrogen pressure to 0.12MPa, control the temperature of the reaction material to 60°C, and carry out the reaction under pressure and heat preservation;

[0019] C. When the content of 3-carene in the reaction material of the reactor is less than or equal to ...

Embodiment 2

[0024] The method for the synthesis of carane by hydrogenation of 3-carene comprises the following steps:

[0025] A, 400g 3-carene content is 93.6% 3-carene mixture and 4g nickel catalyst are put in the reactor, first replace three times with nitrogen, then replace three times with hydrogen, then pass into hydrogen again, then control the temperature in the still The hydrogen pressure is 0.5MPa, and then heating is started, so that the temperature of the reaction material in the reactor reaches 55°C, and the reaction is carried out under pressure and heat preservation;

[0026] B. When the content of 3-carene in the reaction material of the reactor is less than or equal to 60%, adjust the hydrogen pressure to 0.1MPa, control the temperature of the reaction material to 65°C, and carry out the reaction under pressure and heat preservation;

[0027] C. When the content of 3-carene in the reaction material of the reactor is less than or equal to 30%, adjust the hydrogen pressure ...

Embodiment 3

[0032] The method for the synthesis of carane by hydrogenation of 3-carene comprises the following steps:

[0033] A. Put 1200g of 3-carene content of 94.3% 3-carene mixture and 6g of nickel catalyst into the reactor, first replace it with nitrogen three times, then replace it with hydrogen three times, then pass into hydrogen, and then control the temperature in the kettle The hydrogen pressure is 0.03MPa, and then heating is started, so that the temperature of the reaction material in the reactor reaches 60°C, and the reaction is carried out under pressure and heat preservation;

[0034] B. When the content of 3-carene in the reaction material of the reactor is less than or equal to 60%, adjust the hydrogen pressure to 0.08MPa, control the temperature of the reaction material to 70°C, and carry out the reaction under pressure and heat preservation;

[0035] C. When the content of 3-carene in the reaction material of the reactor is less than or equal to 30%, adjust the hydrog...

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Abstract

The invention discloses a method for synthesizing carane through 3-carene hydrogenation, and relates to the technical field of terpenoid compound deep processing. According to the invention, reaction temperatures and hydrogenation pressures of various 3-carene content stages in a 3-carene hydrogenation synthesis reaction process are correspondingly regulated and controlled, such that the reaction is mildly and orderly oriented to a result of high carane yield. Therefore, carane yield and purity can be improved.

Description

technical field [0001] The invention belongs to the technical field of deep processing of terpenoids, and in particular relates to a method for synthesizing carane by hydrogenating 3-carene. Background technique [0002] Carane is a synthetic organic compound, and it is an isomer of pinane or kanane. There are many important derivatives of carane, such as carone, caranol, and caranamine. Among them, the three-membered ring of carane is a rare structural unit derived from nature. Like carene, it can be used as an intermediate raw material for various active substances, and it can also be broken to generate seven-membered ring derivatives for utilization. [0003] At present, most caranes are prepared from 3-carene by hydrogenation catalysis. For example, Chinese Patent Publication No. CN102173975 discloses that 3-carene and catalyst are heated in an autoclave for hydrogenation reaction, the reaction pressure is 3.0-10 MPa, the reaction temperature is 60°C-180°C, and the rea...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C13/40C07C5/03
Inventor 陈键泉陈伟强车乾池黄蕾李战冯玲
Owner WUZHOU SONGHUA AROMATIC CHEM
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