CN103012426A - Method for preparing high-purity natural 1,8-cineole by adopting freezing crystallization method - Google Patents
Method for preparing high-purity natural 1,8-cineole by adopting freezing crystallization method Download PDFInfo
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- CN103012426A CN103012426A CN 201310008169 CN201310008169A CN103012426A CN 103012426 A CN103012426 A CN 103012426A CN 201310008169 CN201310008169 CN 201310008169 CN 201310008169 A CN201310008169 A CN 201310008169A CN 103012426 A CN103012426 A CN 103012426A
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- cineole
- purity
- natural
- freezing
- preparing high
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- WEEGYLXZBRQIMU-UHFFFAOYSA-N Eucalyptol Chemical compound C1CC2CCC1(C)OC2(C)C WEEGYLXZBRQIMU-UHFFFAOYSA-N 0.000 title claims 10
- 230000008014 freezing Effects 0.000 title claims 4
- 238000007710 freezing Methods 0.000 title claims 4
- 238000002425 crystallisation Methods 0.000 title claims 2
- 238000000034 method Methods 0.000 title claims 2
- 238000013467 fragmentation Methods 0.000 claims 2
- 238000006062 fragmentation reaction Methods 0.000 claims 2
- 238000005119 centrifugation Methods 0.000 claims 1
- 230000008025 crystallization Effects 0.000 claims 1
- 229940044949 eucalyptus oil Drugs 0.000 claims 1
- 239000010642 eucalyptus oil Substances 0.000 claims 1
- 229910001220 stainless steel Inorganic materials 0.000 claims 1
- 239000010935 stainless steel Substances 0.000 claims 1
- 238000010257 thawing Methods 0.000 claims 1
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Abstract
The invention provides a method for preparing high-purity natural 1,8-cineole by adopting a freezing crystallization method. The method comprises the following steps: filling natural eucalyptus oil containing more than 85% of natural 1,8-cineole, obtained through distillation production process, into a stainless steel tray, conducting low-temperature freezing in a tank type cold storage, crushing condensed cineole by a crusher, pouring the crushed cineole into a high-speed centrifugal machine for centrifugally separating to obtain natural 1,8-cineole with the purity of more than 99.6%. The method has the characteristics of being simple in process, high in efficiency and the like.
Description
Technical field
The present invention relates to a kind of preparation method of high-purity natural 1, 8-Cineole, belong to the processing technology of chemical industry fine chemical product.
Background technology
Natural 1, 8-Cineole is because its special aromatic odour and good sterilization, disinfecting power are widely used in the fields such as daily necessities, medicine, food, Industrial Catalysis.At present, the method from the refining cineole of eucalyptus oil has: chemical reaction method, special extract rectification method, silica gel chromatography, fusion-crystallization method and freeze crystallization etc.It is feasible that chemical reaction method makes high-purity cineole, needs secondary separation but exist in the process engineering, and flow process more complicated, and also have harmful material in the technological process is not thorough during separation, also can affect the quality of cineole; The cineole content that the special extract rectification method makes can only reach 99%, can't satisfying the market to the needs of high-purity cineole; Silica gel chromatography is little because for the treatment of capacity, is not suitable for large-scale industrialization production; Chinese patent (CN1109887A) adopts the fusion-crystallization method to realize the preparation method of high-purity cineole, and the result has to the cineole of purity 99%.Chinese patent (CN1436783A) adopts the sedimentation crystallizer, produces the cineole more than 99.5%, and present method separation efficiency and yield are all higher, but turnout is little, and operating process is more loaded down with trivial details, is not suitable for large-scale industrialization production.Chinese patent (CN1064700A) adopts traditional freeze crystallization to produce cineole, although present method technique is simple, Device-General, the production cycle is longer, and can only obtain the cineole of content 99%.
Summary of the invention
Purpose of the present invention is exactly for the larger defective that overcomes the current technology existence and tries hard to realize that a kind of technique is simple, and the cycle is shorter, and yield is higher, and cost is lower, is applicable to the method for industrial high purity cineole.
Purpose of the present invention can realize by following scheme: the method for the natural 1, 8-Cineole of a kind of freeze crystallization high purity is characterized in that may further comprise the steps:
(1) 85% eucalyptus oil is sub-packed in the stainless steel pallet, the pallet layering is placed on the interior support of box type refrigerated warehouse;
(2) open freezing button, made temperature be down to-28 ℃ through 30 seconds, freezing 10 hours of constant temperature;
(3) 1, 8-Cineole after will freezing takes out, and puts into crusher and carries out fragmentation;
(4) 1, 8-Cineole after the fragmentation is poured in 1200 rev/mins the supercentrifuge, centrifugation was taken out in 30 seconds afterwards, namely got the high-purity natural 1, 8-Cineole product of purity 〉=99.6% after the thawing.
The present invention has simple, the efficient high of technique.
Now with specific examples, further narrate the process that the inventive method is implemented:
Embodiment: be 85.3% eucalyptus oil 2000kg with purity, be loaded on respectively in 300 stainless steel pallets that are placed in the box type refrigerated warehouse, temperature of ice house is down to-28 ℃ gradually, and material forms crystallization in pallet, constant temperature kept after 10 hours, take out pallet, the cineole that condenses is poured in the crusher, the cineole after the fragmentation is put into 1200 rev/mins whizzer, took out afterwards in centrifugal 30 seconds and melt, namely get purity and be high-purity 1, 8-Cineole product 876.4kg of 99.62%, yield 43.8%.
Claims (1)
1. the method for the natural 1, 8-Cineole of freeze crystallization high purity is characterized in that having comprised the following step:
(1) 85% eucalyptus oil is sub-packed in the stainless steel pallet, the pallet layering is placed on the interior support of box type refrigerated warehouse;
(2) open freezing button, made temperature be down to-28 ℃ through 30 seconds, freezing 10 hours of constant temperature;
(3) 1, 8-Cineole after will freezing takes out, and puts into crusher and carries out fragmentation;
(4) 1, 8-Cineole after the fragmentation is poured in 1200 rev/mins the supercentrifuge, centrifugation was taken out in 30 seconds afterwards, namely got the high-purity natural 1, 8-Cineole product of purity 〉=99.6% after the thawing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201310008169 CN103012426A (en) | 2013-01-10 | 2013-01-10 | Method for preparing high-purity natural 1,8-cineole by adopting freezing crystallization method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201310008169 CN103012426A (en) | 2013-01-10 | 2013-01-10 | Method for preparing high-purity natural 1,8-cineole by adopting freezing crystallization method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103012426A true CN103012426A (en) | 2013-04-03 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201310008169 Pending CN103012426A (en) | 2013-01-10 | 2013-01-10 | Method for preparing high-purity natural 1,8-cineole by adopting freezing crystallization method |
Country Status (1)
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| CN (1) | CN103012426A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104211710A (en) * | 2014-09-28 | 2014-12-17 | 福建森美达生物科技有限公司 | Freezing crystallization extraction method of high-purity 1,8-cineole |
| CN104761566A (en) * | 2015-03-25 | 2015-07-08 | 昆明理工大学 | Method for crystallizing and purifying low-concentration eucalyptus oil |
| CN109293671A (en) * | 2018-09-04 | 2019-02-01 | 中粮德信行健康产业有限公司 | A kind of purification process of Cineole |
| CN110066285A (en) * | 2019-04-29 | 2019-07-30 | 江西思派思香料化工有限公司 | A kind of preparation method of Cineole |
-
2013
- 2013-01-10 CN CN 201310008169 patent/CN103012426A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104211710A (en) * | 2014-09-28 | 2014-12-17 | 福建森美达生物科技有限公司 | Freezing crystallization extraction method of high-purity 1,8-cineole |
| CN104211710B (en) * | 2014-09-28 | 2016-08-24 | 福建森美达生物科技有限公司 | A kind of freezing and crystallizing extracting method of 1,8-cineole |
| CN104761566A (en) * | 2015-03-25 | 2015-07-08 | 昆明理工大学 | Method for crystallizing and purifying low-concentration eucalyptus oil |
| CN104761566B (en) * | 2015-03-25 | 2017-03-01 | 昆明理工大学 | A kind of method of low concentration eucalyptus oil crystallization and purification |
| CN109293671A (en) * | 2018-09-04 | 2019-02-01 | 中粮德信行健康产业有限公司 | A kind of purification process of Cineole |
| CN110066285A (en) * | 2019-04-29 | 2019-07-30 | 江西思派思香料化工有限公司 | A kind of preparation method of Cineole |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20130403 |