A method for preparing high-purity 1,8-cineole from camphor crude oil

A technology of eucalyptol and crude oil, applied in the direction of organic chemistry, can solve the problems of low product purity, low temperature and high energy consumption, and achieve the effect of short process flow, simple equipment operation and higher energy consumption

Active Publication Date: 2021-06-29
成都市明典世家生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The present invention aims to provide a method for preparing high-purity 1,8-cineole from camphor crude oil, and provides a method for preparing high-purity camphor crude oil containing 48% to 58% of 1,8-cineole. The main purpose of the new production method and process route of 1,8-cineole is to solve the problems of low temperature (generally -20~-30°C) required by the freeze crystallization method and high energy consumption and low product purity caused by the vacuum distillation method

Method used

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  • A method for preparing high-purity 1,8-cineole from camphor crude oil
  • A method for preparing high-purity 1,8-cineole from camphor crude oil
  • A method for preparing high-purity 1,8-cineole from camphor crude oil

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Effect test

Embodiment 1

[0056] A kind of method concrete steps of preparing high-purity 1,8-cineole from camphor crude oil are as follows:

[0057] Step 1: Under the condition of pressure of -90kPa, collect the distillate section with a temperature of 75°C to 83°C at the top of the tower, which completely removes components with a boiling point above 200°C, and obtains 1,8-eucalyptus with a content of 82% leaf element.

[0058] Step 2: Put C 4 The bromotropine alcohol ionic liquid and ethylene glycol were heated and stirred at 55°C in a molar ratio of 1:5, and mixed uniformly to a transparent liquid, so as to prepare a low eutectic solvent for extraction.

[0059] Step 3: Add 200g of camphor leaf oil containing 82% 1,8-cineole and 200g of the eutectic solvent prepared in step 2 or recovered after extraction and separation into the mixing tank, and stir and mix at 10°C for 0.5h to make it Full exposure to mass transfer. After standing still for 1 hour, the supernatant liquid was released and transf...

Embodiment 2

[0061] A kind of method concrete steps of preparing high-purity 1,8-cineole from camphor crude oil are as follows:

[0062] Step 1: Same as Embodiment 1 (omitted here)

[0063] Step 2: Put C 6 The bromotropine alcohol ionic liquid and ethylene glycol were heated and stirred at 55° C. and mixed uniformly at a molar ratio of 1:10.

[0064] Step 3: Add 200g of camphor leaf oil containing 82% 1,8-cineole and 400g of the low eutectic solvent prepared in step 2 or recovered after extraction and separation into the mixing tank, stir and mix at 25°C for 1 hour to fully contact Mass transfer, after standing for 2 hours, transfer the supernatant to another stirring tank, add 600g of water and stir at 25°C for 1.5 hours, let stand for 1.5 hours, release the upper liquid to obtain 1,8-cineole with a purity of 99% .

Embodiment 3

[0066] A kind of method concrete steps of preparing high-purity 1,8-cineole from camphor crude oil are as follows:

[0067] Step 1: Same as Embodiment 1 (omitted here)

[0068] Step 2: Put C 8 The bromotropine alcohol ionic liquid and ethylene glycol were heated and mixed uniformly at 60°C at a molar ratio of 1:10.

[0069] Step 3: Add 200g of camphor leaf oil containing 82% 1,8-cineole and 600g of the low eutectic solvent prepared in step 2 or recovered after extraction and separation into the mixing tank, and stir and mix at 40°C for 1.5h to fully Contact mass transfer, after standing for 3 hours, transfer the supernatant to another stirring tank, add 720g of water, stir at 40°C for 2 hours, let stand for 2 hours, release the upper liquid to obtain 1,8-cineole with a purity of 97%.

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Abstract

The invention discloses a method for preparing high-purity 1,8-cineole from camphor crude oil. The method uses crude camphor oil as a raw material, and removes 1,8-cineole with a boiling point above 200°C through a simple vacuum distillation step. heavy fraction, and collect camphor leaf oil with an average content of 1,8-cineole of more than 80%, and then use tropin alcohol low eutectic solvent as a green medium from the oil containing 80% of 1,8-cineole Preparation of high-purity 1,8-cineole by liquid-liquid extraction from camphor leaf oil. The process of the present invention purifies 1,8-cineole from camphor leaf crude oil by using one-time rectification and one-time liquid-liquid extraction to prepare high-purity 1,8-cineole, compared with the existing one-step rectification and The two-step freezing and crystallization method has a simple process and is more energy-saving. In addition, the low eutectic solvent can be recycled and reused, and the process is green.

Description

technical field [0001] The invention belongs to the technical field of 1,8-cineole preparation, and in particular relates to a method for preparing high-purity 1,8-cineole from camphor crude oil. Background technique [0002] Camphor tree is planted in a large area as a natural spice tree species, which originated in the late 1970s in my country. The wood of camphor tree is hard and beautiful, with aromatic flavor, resistant to insects, suitable for making furniture, and volatile oil can be extracted from its roots, trunks, branches, leaves and fruits. One of the species of camphor tree is called oil camphor, and the volatile oil extracted from its leaves is called oil camphor crude oil for short. The main components are terpenes, sesquiterpenes and their oxygen-containing derivatives. The representative substances are α-pinene, Sabinene, 1,8-cineole, 4-terpineol, α-terpineol and other important components. 1,8-Cineole is the main component of camphor leaf oil, accounting ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D493/08
CPCC07D493/08
Inventor 宋航袁科王小东李福林张晶兰先秋
Owner 成都市明典世家生物科技有限公司
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