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A purification method, eucalyptol technology, applied in the field of 1,8-cineole purification, can solve the problems of complex operation and process, low raw material utilization rate, high equipment requirements, etc., to reduce production costs and improve utilization rate , the effect of easy operation
Active Publication Date: 2013-12-25
云南森美达生物科技股份有限公司
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Problems solved by technology
[0008] 3) For the raw material oil with relatively low 1,8-cineole content, it is difficult to separate high-purity 1,8-cineole from it, and the raw material utilization rate is low;
[0009] 4) The operation and process are complicated, and the requirements for equipment are high;
[0010] 5) The catalyst used is highly toxic, difficult to recycle, and pollutes the environment
Method used
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Embodiment 1
[0029] Add 300g blue eucalyptus oil (containing 1,8-cineole 51%, limonene 25.4%), 500g acetic acid aqueous solution (90%) and 15.2g phosphotungstic acid into the reaction bottle; heat and stir at 40°C for 39h; react The limonene content of the liquid was detected by gas chromatography to be 1.1%, and the content of eucalyptol was 51.8%. After the reaction, the reaction liquid was filtered to recover the catalyst, and the oil phase was subjected to vacuum distillation to obtain 1,8-cineole with a purity of 99.97%. .
Embodiment 2
[0031] Add 300g blue eucalyptus tail oil (containing 15% 1,8-cineole, 62% limonene), 100g acetic acid (100%) and 12g phosphotungstovanadate heteropoly acid into the reaction bottle; heat and stir at 50°C Reacted for 35 hours; the limonene content of the reaction solution was detected by gas chromatography to be 0.6%, and the content of eucalyptol was 15.2%. After the reaction, the reaction solution was filtered to recover the catalyst, and the oil phase was subjected to vacuum distillation to obtain 1,8 with a purity of 99.95%. - Eucalyptol.
Embodiment 3
[0033] Add 150g blue eucalyptus tail oil (containing 15% 1,8-cineole, 62% limonene), 50g acetic acid aqueous solution (90%) and 5.0g phosphotungstovanadate heteropolyacid into the reaction flask; Heated and stirred for 33 hours; the limonene content of the reaction solution was detected by gas chromatography to be 0.7%, and the content of eucalyptol was 14.9%; after the reaction, the reaction solution was filtered to recover the catalyst, and the oil phase was rectified under reduced pressure to obtain 1 , 8-cineole.
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Abstract
The invention discloses a purification method for 1, 8-cineole and particularly discloses a separation and purification method for 1, 8-cineole in low-content raw oil. The method is characterized by comprising the steps of (1) adding raw oil, acetic acid or a water solution of acetic acid and a catalyst into a reaction flask, wherein the raw oil contains 1, 8-cineole and limonene; (2) heating and stirring to react; (3) after the reaction is ended, filtering a reaction solution to recycle the catalyst, and carrying out reduced pressure distillation on an oil phase to obtain 1, 8-cineole with high purity. By using the purification method, the content of 1, 8-cineole in the raw oil can be kept constant after being treated, and the content of limonene as an impurity can be reduced to 0.2-1.1%, so that 1, 8-cineole with high purity can be obtained. Meanwhile, after reacting, limonene in the raw oil generates alpha-terpinene, gamma-terpinene, alpha-terpilenol and the like which all have higher additional values and can not affect the distillation of 1, 8-cineole, therefore, the purification method is a low-cost and green-chemical purification method.
Description
technical field [0001] The invention relates to a method for purifying 1,8-cineole, in particular to a method for removing impurities that are difficult to separate by rectification in the process of purifying 1,8-cineole. Background technique [0002] 1,8-Cineole is also known as eucalyptol, eucalyptol, 1,8-epoxy-p-mentane, okanabutol, chemical name 1,3,3-trimethyl-2-oxa Bicyclo[2.2.2.]octane (CAS NO 470-82-6) is widely used in pharmaceutical products, cough drops, artificial mints, gargles, toothpaste, and air cleaners. [0003] The development of 1,8-cineole separation process has benefited from the purchase of high-purity products by foreign customers, but it is not easy to separate and purify high-purity 1,8-cineole from raw material oil, mainly because the raw materials In addition to the high content of 1,8-cineole, there are limonene, pinene and other terpinene substances in the oil; these substances are either isomers with 1,8-cineole, or It has similar physical a...
Claims
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