CN104211710A - Freezing crystallization extraction method of high-purity 1,8-cineole - Google Patents
Freezing crystallization extraction method of high-purity 1,8-cineole Download PDFInfo
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- CN104211710A CN104211710A CN201410504316.4A CN201410504316A CN104211710A CN 104211710 A CN104211710 A CN 104211710A CN 201410504316 A CN201410504316 A CN 201410504316A CN 104211710 A CN104211710 A CN 104211710A
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- Prior art keywords
- freezing
- cineole
- centrifugal
- crystallization
- raw material
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- WEEGYLXZBRQIMU-UHFFFAOYSA-N Eucalyptol Chemical compound C1CC2CCC1(C)OC2(C)C WEEGYLXZBRQIMU-UHFFFAOYSA-N 0.000 title claims abstract description 107
- 230000008014 freezing Effects 0.000 title claims abstract description 66
- 238000007710 freezing Methods 0.000 title claims abstract description 66
- 238000002425 crystallisation Methods 0.000 title claims abstract description 32
- 230000008025 crystallization Effects 0.000 title claims abstract description 30
- 238000000605 extraction Methods 0.000 title abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 29
- 239000007788 liquid Substances 0.000 claims abstract description 27
- 239000002994 raw material Substances 0.000 claims abstract description 23
- 229960005233 cineole Drugs 0.000 claims description 14
- 230000008018 melting Effects 0.000 claims description 9
- 238000002844 melting Methods 0.000 claims description 9
- 238000005057 refrigeration Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 229920002635 polyurethane Polymers 0.000 claims description 3
- 239000004814 polyurethane Substances 0.000 claims description 3
- 239000003507 refrigerant Substances 0.000 abstract description 7
- 238000005119 centrifugation Methods 0.000 abstract 2
- 239000012595 freezing medium Substances 0.000 abstract 1
- 239000010642 eucalyptus oil Substances 0.000 description 8
- 229940044949 eucalyptus oil Drugs 0.000 description 8
- 239000013078 crystal Substances 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 230000001105 regulatory effect Effects 0.000 description 4
- RFFOTVCVTJUTAD-UHFFFAOYSA-N cineole Natural products C1CC2(C)CCC1(C(C)C)O2 RFFOTVCVTJUTAD-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 238000010257 thawing Methods 0.000 description 2
- DSSYKIVIOFKYAU-XCBNKYQSSA-N (R)-camphor Chemical compound C1C[C@@]2(C)C(=O)C[C@@H]1C2(C)C DSSYKIVIOFKYAU-XCBNKYQSSA-N 0.000 description 1
- 241000723346 Cinnamomum camphora Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000001754 anti-pyretic effect Effects 0.000 description 1
- 239000002221 antipyretic Substances 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 229960000846 camphor Drugs 0.000 description 1
- 229930008380 camphor Natural products 0.000 description 1
- 239000012230 colorless oil Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001784 detoxification Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000007323 disproportionation reaction Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 241000411851 herbal medicine Species 0.000 description 1
- 238000000703 high-speed centrifugation Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 239000000341 volatile oil Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D493/00—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system
- C07D493/02—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system in which the condensed system contains two hetero rings
- C07D493/08—Bridged systems
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention provides a freezing crystallization extraction method of high-purity 1,8-cineole. The freezing crystallization extraction method of the high-purity 1,8-cineole comprises the specific steps of arranging raw materials with higher than 60% of 1,8-cineole content into a freezing storeroom to be kept for 5-15 hours for crystallization, wherein a freezing medium produced by a air-cooled type freezing device is used as a refrigerant in the freezing storeroom; using a centrifugal machine to centrifuge crystallized raw materials, performing centrifugation for 1-8 minutes at the rotating speed of 400-800 turns/min to collect liquid separated by the centrifugal machine, then improving the rotating speed of the centrifugal machine to be 100-1600 turns/min, and performing centrifugation for 1-6 minutes to collect separated liquid in the process; collecting the centrifuged remaining materials to be heated and melted to obtain the high-purity 1,8-cineole. The high-purity 1,8-cineole extracted by means of the freezing crystallization extraction method has the advantages of being high in extraction rate, low in raw material requirement, simple, practical and good in universality.
Description
Technical field
The present invention relates to a kind of extracting method of 1, 8-Cineole, specifically a kind of freezing and crystallizing extracting method of high purity 1, 8-Cineole.
Background technology
1, 8-Cineole is colorless oil transparent liquid, has camphor breath and refrigerant herbal medicine taste, and fusing point is 1～1.5 ℃.1, 8-Cineole is present in folium eucalypti wet goods more than 270 plants in natural essential oil, have antibacterial, desinsection, dispelling wind is antipyretic, clearing damp detoxification has good transdermal penetration effect to multi-medicament simultaneously.
Existing 1, the refining method adopting of 8-cineole mainly contains fusion-crystallization method, freeze crystallization carries out the crystallization of cineole, wherein fusion-crystallization method is used the technique of crystallization, liquid separation, thawing, crystallization again, liquid separation, thawing to carry out 1,8-cineole is refining, need by operation repeatedly, obtain the product of 1, 8-Cineole content 99.5%.Freeze crystallization is to use the whizzer of fixed speed by non crystallized liquid separation in the 1, 8-Cineole crystal obtaining, and extracts the product of 1, 8-Cineole content 99.5%.
Existing freeze crystallization is higher to the content requirement of 1, 8-Cineole in the raw material dropping into, and extraction yield is not high.Mainly there is following defect in existing 1, 8-Cineole freezing and crystallizing extracting method:
(1) adopt that indirect type is freezing carries out freezing and crystallizing to raw material, refrigerant does not directly contact with material, by natural diffusion way, reduce temperature of charge, cause temperature distributing disproportionation even, freezing efficiency is low, and cineole crystallization effect is bad, and cannot regulate freezing temp, can not be applicable to the different raw material of freezing 1, 8-Cineole content;
(2) existing 1, in 8-cineole purification process, raw material after crystallization directly carries out separation by the high speed centrifugation of fixed rotating speed, in centrifugal process, easily cause part crystallization 1,8-cineole melts, obtain finished product materials and be containing 30%～50% 1, the liquid of 8-cineole, this partially liq is as need freezing and crystallizing again, at least need to be cooled to-70 ℃, equipment and be manually all difficult to reach this temperature requirement, has therefore caused in the non-crystallizable liquid of this part 1,8-cineole cannot the freezing extraction of secondary, has reduced extraction yield.
Summary of the invention
The invention provides a kind of freezing and crystallizing extracting method of high purity 1, 8-Cineole, its main purpose is to solve the problems such as high to ingredient requirement in 1, 8-Cineole freezing and crystallizing leaching process, extraction yield is low.
In order to solve the problems of the technologies described above, the present invention is a kind of freezing and crystallizing extracting method of high purity 1, 8-Cineole, and concrete steps are as follows:
(1) by 1, 8-Cineole content, be that more than 60% raw material is positioned in freezing storehouse and keeps carrying out for 5～15 hours crystallization, this freezing storehouse adopts air-cooled freezing device to freeze.
(2) raw material after using whizzer to crystallization carries out centrifugal, under the rotating speed of 400～800 revs/min, centrifugal 1～8 minute, collect the isolated liquid of described whizzer, then improve this centrifuge speed to 1000～1600 rev/min, centrifugal 1～6 minute, collect separately isolated liquid in this process;
(3) collect and carry out heating and melting through centrifugal remaining material, obtain high purity 1, 8-Cineole product.
Further, the metope of described freezing storehouse adopts polyurethane material to make, and in this freezing storehouse, is placed with material bracing frame, and this material bracing frame is provided with multilayer space, is placed with for holding the raw material splendid attire dish of raw material in every layer of space; Described air-cooled freezing device comprises the cold blast engine that is arranged at freezing storehouse inner top and the compressor that is arranged at this freezing storehouse outside.
Further, the refrigeration temperature of described air-cooled freezing compressor is adjustable, and the regulation range of this refrigeration temperature is 0 ℃～-40 ℃.
Further, the method for described heating and melting is for to melt pot by the stainless steel of putting into jacketed through centrifugal material, and passes into hot water in described chuck.
The invention has the advantages that:
(1) utilize 1, 8-Cineole low temperature to form the physical properties of crystal, leaching process is physical process, and the major equipment that 1, 8-Cineole extracts is sizing or general-purpose equipment, is easy to buying and makes, simple, practical, highly versatile.
(2) use air-cooled freezing device to produce refrigerant, refrigerant is entered by freezer roof portion, effectively guarantee freezing storehouse temperature evenly, the material crystal that makes to contain 1, 8-Cineole evenly, stable.Refrigerant directly contacts with raw material in storehouse, improves the utilising efficiency of refrigerant.The refrigeration temperature of described air-cooled freezing device is adjustable, and has wider regulation range, is applicable to 1, 8-Cineole content at more than 60% raw material, has reduced the requirement to 1, 8-Cineole content in raw material.
(3) use that speed change is centrifugal carries out the separated of 1, 8-Cineole crystal and non-crystallizable component, have and utilize the extraction yield that improves 1, 8-Cineole.Under slow speed of revolution condition, first isolate a large amount of non crystallized liquid, then improve rotating speed, to be attached on a small quantity 1, the non-crystallizable liquid separation of 8-cineole plane of crystal, now, part 1, there is partial melting in 8-cineole, together be centrifuged separated with a small amount of non crystallized liquid, make this partially liq 1, 8-cineole content is higher, 1, 8-cineole content can reach 70%, reached in raw material 1, the requirement of 8-cineole content, its Tc is in equipment and the accessible scope of manual operation, this partially liq, can carry out the freezing extraction of secondary, realize the raising of cineole extraction yield.Product extraction yield reaches 50%～85% according to the difference of 1, 8-Cineole content in raw material.
Accompanying drawing explanation
Fig. 1 is the diagrammatic cross-section of freezing storehouse described in the present invention.
Embodiment
The present invention is further described in connection with embodiment.
Embodiment mono-
With reference to Fig. 1, a kind of freezing and crystallizing extracting method of high purity 1, 8-Cineole, concrete steps are as follows:
(1), by 3kg～15kg1, the eucalyptus oil that 8-cineole content is 60% is put in each the material splendid attire dish 4 that adds material placing rack 2 in described freezing storehouse, reinforced complete, close freezer door, regulating refrigeration temperature is-40 ℃, opens air-cooled freezing device, keeps carrying out for 8 hours crystallization.
(2) eucalyptus oil after using whizzer to crystallization carries out centrifugal, under the rotating speed of 800 revs/min, centrifugal 2 minutes, collect the isolated non-crystallizable liquid of described whizzer, then improve this centrifuge speed to 1400 rev/min, centrifugal 2 minutes, collect separately isolated liquid in this process, in gained liquid, 1, 8-Cineole content reaches 70%, can be used for crystallization again.
(3) collect and to carry out heating and melting through centrifugal remaining material, the stainless steel of putting into jacketed is melted to pot, and pass into hot water through centrifugal material in described chuck, obtain content and be 99.5% 1, 8-Cineole product, squeeze into storage tank, extraction yield can reach 52%
Embodiment bis-
With reference to Fig. 1, a kind of freezing and crystallizing extracting method of high purity 1, 8-Cineole, concrete steps are as follows:
(1) by 3kg～15kg1, the eucalyptus oil that 8-cineole content is 70% adds in each material splendid attire dish 4 of the material placing rack 2 in described freezing storehouse, reinforced complete, close freezer door, regulating refrigeration temperature is-35 ℃, opens air-cooled freezing device, keeps carrying out for 15 hours crystallization.
(2) eucalyptus oil after using whizzer to crystallization carries out centrifugal, under the rotating speed of 400 revs/min, centrifugal 8 minutes, collect the isolated non-crystallizable liquid of described whizzer, then improve this centrifuge speed to 1000 rev/min, centrifugal 6 minutes, collect separately isolated liquid in this process, in this liquid of gained, 1, 8-Cineole content reaches 70%, can be used for crystallization again.
(3) collect and to carry out heating and melting through centrifugal remaining material, the stainless steel of putting into jacketed is melted to pot, and pass into hot water through centrifugal material in described chuck, obtain content and be 99.5% 1, 8-Cineole product, squeeze into storage tank, extraction yield can reach 60%
Embodiment tri-
With reference to Fig. 1, a kind of freezing and crystallizing extracting method of high purity 1, 8-Cineole, concrete steps are as follows:
(1), by 3kg～15kg1, the eucalyptus oil that 8-cineole content is 85% adds in each material splendid attire dish 4 of material placing rack 2 in described freezing storehouse, reinforced complete, close freezer door, regulating refrigeration temperature is-28 ℃, opens air-cooled freezing device, keeps carrying out for 5 hours crystallization.
(2) eucalyptus oil after using whizzer to crystallization carries out centrifugal, under the rotating speed of 600 revs/min, centrifugal 1 minute, collect the isolated non-crystallizable liquid of described whizzer, then improve this centrifuge speed to 1800 rev/min, centrifugal 1 minute, collect separately isolated liquid in this process, in this liquid of gained, 1, 8-Cineole content reaches 70%, can be used for crystallization again.
(3) collect and to carry out heating and melting through centrifugal remaining material, the stainless steel of putting into jacketed is melted to pot, and pass into hot water through centrifugal material in described chuck, obtain content and be 99.5% 1, 8-Cineole product, squeeze into storage tank, extraction yield can reach 70%.
Embodiment tetra-
With reference to Fig. 1, a kind of freezing and crystallizing extracting method of high purity 1, 8-Cineole, concrete steps are as follows:
(1), by 3kg～15kg1, the eucalyptus oil that 8-cineole content is 90% adds in each material splendid attire dish 4 of material placing rack 2 in described freezing storehouse, reinforced complete, close freezer door, regulating refrigeration temperature is-25 ℃, opens air-cooled freezing device, keeps carrying out for 8 hours crystallization.
(2) eucalyptus oil after using whizzer to crystallization carries out centrifugal, under the rotating speed of 700 revs/min, centrifugal 4 minutes, collect the isolated non-crystallizable liquid of described whizzer, then improve this centrifuge speed to 1600 rev/min, centrifugal 3 minutes, collect separately isolated liquid in this process, in this liquid of gained, 1, 8-Cineole content reaches 70%, can be used for crystallization again.
(3) collect and to carry out heating and melting through centrifugal remaining material, the stainless steel of putting into jacketed is melted to pot, and pass into hot water through centrifugal material in described chuck, obtain content and be 99.5% 1, 8-Cineole product, squeeze into storage tank, extraction yield can reach 80%.
With reference to Fig. 1, the concrete structure of the freezing storehouse described in above-described embodiment one, embodiment bis-, embodiment tri-, embodiment tetra-is as follows:
The metope 1 of described freezing storehouse adopts polyurethane material to make, and guarantees stopping property and the effect of heat insulation of freezing storehouse.In described freezing storehouse, be placed with material bracing frame 2, this material bracing frame 2 is provided with multilayer space 3, is placed with for holding the raw material splendid attire dish 4 of raw material in every layer of space 3.Described air-cooled freezing device comprises the cold blast engine 5 that is arranged at freezing storehouse inner top and the compressor 6 that is arranged at this freezing storehouse outside, in this cold blast engine 5, is provided with refrigerator pipe, and this refrigerator pipe is connected with described compressor 6.This cold blast engine 5 is provided with downwards and to the cold wind outlet of interior wall, the cold air blowing out forms random free diffusing downwards or with interior wall collision naturally, and the temperature of storehouse is consistent, and assurance raw material is homogeneously crystallized.
Above are only the specific embodiment of the present invention, but design concept of the present invention is not limited to this, allly utilizes this design to carry out the change of unsubstantiality to the present invention, all should belong to the behavior of invading protection domain of the present invention.
Claims (4)
1. a freezing and crystallizing extracting method for high purity 1, 8-Cineole, concrete steps are as follows:
(1) by 1, 8-Cineole content, be that more than 60% raw material is positioned in freezing storehouse and keeps carrying out for 5～15 hours crystallization, this freezing storehouse adopts air-cooled freezing device to freeze;
(2) raw material after using whizzer to crystallization carries out centrifugal, under the rotating speed of 400～800 revs/min, centrifugal 1～8 minute, collect the isolated liquid of described whizzer, then improve this centrifuge speed to 1000～1600 rev/min, centrifugal 1～6 minute, collect separately isolated liquid in this process;
(3) collect and carry out heating and melting through centrifugal remaining material, obtain high purity 1, 8-Cineole product.
2. a kind of high purity 1 as claimed in claim 1, the freezing and crystallizing extracting method of 8-cineole, it is characterized in that: the metope of described freezing storehouse adopts polyurethane material to make, in this freezing storehouse, be placed with material bracing frame, this material bracing frame is provided with multilayer space, is placed with for holding the raw material splendid attire dish of raw material in every layer of space; Described air-cooled freezing device comprises the cold blast engine that is arranged at freezing storehouse inner top and the compressor that is arranged at this freezing storehouse outside.
3. the freezing and crystallizing extracting method of a kind of high purity 1, 8-Cineole as claimed in claim 2, is characterized in that: the refrigeration temperature of described air-cooled freezing device is adjustable, and the regulation range of this refrigeration temperature is 0 ℃～-40 ℃.
4. the freezing and crystallizing extracting method of a kind of high purity 1, 8-Cineole as claimed in claim 1, is characterized in that: the method for described heating and melting is for to melt pot by the stainless steel of putting into jacketed through centrifugal material, and passes into hot water in described chuck.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410504316.4A CN104211710B (en) | 2014-09-28 | 2014-09-28 | A kind of freezing and crystallizing extracting method of 1,8-cineole |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410504316.4A CN104211710B (en) | 2014-09-28 | 2014-09-28 | A kind of freezing and crystallizing extracting method of 1,8-cineole |
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| Publication Number | Publication Date |
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| CN104211710A true CN104211710A (en) | 2014-12-17 |
| CN104211710B CN104211710B (en) | 2016-08-24 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104761566A (en) * | 2015-03-25 | 2015-07-08 | 昆明理工大学 | Method for crystallizing and purifying low-concentration eucalyptus oil |
| 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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|---|---|---|---|---|
| EP0270023A1 (en) * | 1986-12-03 | 1988-06-08 | Union Camp Corporation | Improved method of preparing cineoles |
| CN1109887A (en) * | 1994-12-28 | 1995-10-11 | 天津大学 | Process for preparing high-purity natural eudesmin |
| CN1436783A (en) * | 2003-03-05 | 2003-08-20 | 云南省化工研究院 | Prepn process and plant of high-purity eudesmin |
| CN103012426A (en) * | 2013-01-10 | 2013-04-03 | 江西金林香料香精有限公司 | Method for preparing high-purity natural 1,8-cineole by adopting freezing crystallization method |
-
2014
- 2014-09-28 CN CN201410504316.4A patent/CN104211710B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0270023A1 (en) * | 1986-12-03 | 1988-06-08 | Union Camp Corporation | Improved method of preparing cineoles |
| CN1109887A (en) * | 1994-12-28 | 1995-10-11 | 天津大学 | Process for preparing high-purity natural eudesmin |
| CN1436783A (en) * | 2003-03-05 | 2003-08-20 | 云南省化工研究院 | Prepn process and plant of high-purity eudesmin |
| CN103012426A (en) * | 2013-01-10 | 2013-04-03 | 江西金林香料香精有限公司 | Method for preparing high-purity natural 1,8-cineole by adopting freezing crystallization method |
Non-Patent Citations (1)
| Title |
|---|
| 李士雨: "桉叶素的纯化", 《精细化工》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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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| CN104211710B (en) | 2016-08-24 |
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Denomination of invention: A freezing crystallization extraction method of 1,8-cineole Effective date of registration: 20210909 Granted publication date: 20160824 Pledgee: Bank of China Limited Yongan Branch Pledgor: FUJIAN SUMMIT BIOTECHNOLOGY Co.,Ltd. Registration number: Y2021350000106 |
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