CN102503775A - Production process of sclareol - Google Patents
Production process of sclareol Download PDFInfo
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- CN102503775A CN102503775A CN2011103175682A CN201110317568A CN102503775A CN 102503775 A CN102503775 A CN 102503775A CN 2011103175682 A CN2011103175682 A CN 2011103175682A CN 201110317568 A CN201110317568 A CN 201110317568A CN 102503775 A CN102503775 A CN 102503775A
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- sclareol
- salvia sclarea
- extract
- molecular still
- production process
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Abstract
The invention relates to a production process of sclareol. The production process comprises the steps of: extracting Salvia sclarea extract from Salvia sclarea, and then distilling Salvia sclarea extract by a molecular distiller to extract sclareol. Specifically, the production process comprises the following process flows of: cutting Salvia sclarea into segments with size smaller than 10 cm, adding to an extraction kettle, adding petroleum ether with boiling range of 90-120 DEG C to immerge Salvia sclarea, heating to 70 DEG C, extracting for 2 hours, and concentrating to recover petroleum ether and obtain the Salvia sclarea extract; and heating and melting the Salvia sclarea, conveying to the molecular distiller, distilling at the operation pressure of the molecular distiller of 0.1-100 Pa, distillation temperature of 100-150 DEG C and cooling temperature of minus 13-minus 17 DEG C, condensing and crystallizing distillate, centrifugally separating, and drying the crystal to obtain the sclareol finished product. The production process has the advantages that the time from feeding to discharging is only several minutes, the solvent and crystallization process are not needed, the production time is greatly shortened, the extraction rate of sclareol is up to 98%, the purity of the extracted sclareol is more than 90% and the economic benefit is fairly obvious.
Description
Technical field
The present invention relates to a kind of production technique of spices, concrete relate to a kind of production technique of from Salvia Sclare L., extracting spices.
Background technology
Salvia Sclare L. can extract series product such as Salvia Sclare L. essential oil, sclareol, Sclareolide; It is important chemical material; Sclareol is the desirable feedstock of synthetic grane ambra product; Be mainly used in the synthetic of natural grane ambra surrogates such as Sclareolide and ambrox, also be used for the allotment of essence in a small amount, also have antibiotic, fungicidal activity.
It generally is that Salvia Sclare L. is extracted clary sage concrete through processing that Salvia Sclare L. is produced sclareol; Clary sage concrete is the raw material production sclareol; From clary sage concrete, extract sclareol at present and mainly adopt molecular distillation-acetone crystallization two-step approach; This method improvement traditional SX-concentrate-crystallization process, reduced production cost and extraction yield increased, but since distillation temperature up to 160 ℃; Reaction has taken place and has formed new impurity in the part sclareol in still-process, thereby has influenced product purity.
Summary of the invention
To the problems referred to above, the purpose of this invention is to provide a kind of working method of sclareol, technology is simple, and the sclareol purity of production is high, can reduce pollution simultaneously.
In order to address the above problem, technical scheme of the present invention is: a kind of production technique of sclareol is from Salvia Sclare L., to extract clary sage concrete earlier; Again clary sage concrete is passed through molecular still distillation extraction sclareol; It is characterized in that operating with following technical process: Salvia Sclare L. is cut into the segment less than 10cm, the extraction kettle of packing into, the sherwood oil that adds 90-120 ℃ of boiling ranges floods Salvia Sclare L.; Be heated to 70 ℃ of lixiviate 2h, concentrate the recovery sherwood oil and obtain clary sage concrete; With sending in the molecular still behind the clary sage concrete heating and melting; Under molecular still working pressure 0.1-100pa, 100-150 ℃ of distillation temperatures, cooling temperature-13--17 ℃ condition, distill, spinning after the condenses crystallization that distills out, the crystallisate oven dry obtains the sclareol finished product; The sclareol finished product is white powder shape solid; The light banksia rose, fusing point is 98.5-101 ℃, purity content is greater than 90%.
Further, the temperature difference between the cold and hot two sides of said molecular still is 90-160 ℃, and the rotating speed of blade applicator is 100-250rpm/min in the molecular still.
Use technical scheme of the present invention, utilize molecular distillation method, under lower distillation temperature and according to the difference of molecular free path, directly obtain purity greater than 90% sclareol.This technology only needs short several minutes from the charging discharging, need not solvent and Crystallization Procedure, has shortened the PT greatly, and the extraction yield of sclareol is up to 95%, and economic benefit is fairly obvious.
Embodiment
Embodiment 1
The 1.8t Salvia Sclare L. of gathering is cut into the segment cleaning-drying less than 10cm, opens the charging lid of extraction kettle, Salvia Sclare L. is packed in the former charging basket in the extraction kettle into the opening for feed of sealing extraction kettle; Give to add sherwood oil in the extraction kettle and soak Salvia Sclare L., and heater heats, after the effective constituent in the raw material Salvia Sclare L. is extracted; Extraction liquid is pumped in the header tank, and the extraction liquid in the header tank at first gets in the evaporation concentration still, and extraction liquid is concentrated; The vaporised gas condensation separation reclaims sherwood oil wherein, and the extraction liquid after concentrating gets into vacuum still; Further distill out sherwood oil and moisture at this, remaining paste is clary sage concrete 18kg; With Salvia Sclare L. cream heating and melting in reaction kettle; Get into the molecular still distillation then; Molecular still is to distill under 0.5pa, 100 ℃ of distillation temperatures, cooling temperature-17 ℃ the condition at working pressure; Carry out spinning after the condenses crystallization that distills out, it is 90.3% sclareol 8.2kg that crystallisate oven dry promptly gets purity.
Embodiment 2
The 1t Salvia Sclare L. of gathering is cut into the segment cleaning-drying less than 10cm, opens the charging lid of extraction kettle, Salvia Sclare L. is packed in the former charging basket in the extraction kettle into the opening for feed of sealing extraction kettle; Give to add sherwood oil in the extraction kettle and soak Salvia Sclare L., and heater heats, after the effective constituent in the raw material Salvia Sclare L. is extracted; Extraction liquid is pumped in the header tank, and the extraction liquid in the header tank at first gets in the evaporation concentration still, and extraction liquid is concentrated; The vaporised gas condensation separation reclaims sherwood oil wherein, and the extraction liquid after concentrating gets into vacuum still; Further distill out sherwood oil and moisture at this, remaining paste is clary sage concrete 10kg; With Salvia Sclare L. cream heating and melting in reaction kettle; Get into the molecular still distillation then; Molecular still is to distill under 50pa, 120 ℃ of distillation temperatures, cooling temperature-13 ℃ the condition at working pressure; Carry out spinning after the condenses crystallization that distills out, it is 91.8% sclareol 4.5kg that crystallisate oven dry promptly gets purity.
Embodiment 3
The Salvia Sclare L. of the 1.5t that gathers is cut into the segment cleaning-drying less than 10cm, opens the charging lid of extraction kettle, Salvia Sclare L. is packed in the former charging basket in the extraction kettle into the opening for feed of sealing extraction kettle; Give to add sherwood oil in the extraction kettle and soak Salvia Sclare L., and heater heats, after the effective constituent in the raw material Salvia Sclare L. is extracted; Extraction liquid is pumped in the header tank, and the extraction liquid in the header tank at first gets in the evaporation concentration still, and extraction liquid is concentrated; The vaporised gas condensation separation reclaims sherwood oil wherein, and the extraction liquid after concentrating gets into vacuum still; Further distill out sherwood oil and moisture at this, remaining paste is clary sage concrete 15kg; With Salvia Sclare L. cream heating and melting in reaction kettle; Get into the molecular still distillation then; Molecular still is 20pa, 150 ℃ of distillation temperatures, cooling temperature-14 ℃ at working pressure, and the temperature difference between the cold and hot two sides of molecular still is 150 ℃, and the rotating speed of interior blade applicator is to distill under the condition of 250rpm/min; Carry out spinning after the condenses crystallization that distills out, it is 92.5% sclareol 7kg that crystallisate oven dry promptly gets purity.
Claims (3)
1. the production technique of a sclareol; Be from Salvia Sclare L., to extract clary sage concrete earlier, again clary sage concrete passed through molecular still distillation extraction sclareol, it is characterized in that operating: Salvia Sclare L. is cut into the segment less than 10cm with following technical process; The extraction kettle of packing into; The sherwood oil that adds 90-120 ℃ of boiling ranges floods Salvia Sclare L., is heated to 70 ℃ of lixiviate 2h, concentrates the recovery sherwood oil and obtains clary sage concrete; With sending in the molecular still behind the clary sage concrete heating and melting; Under molecular still working pressure 0.1-100pa, 100-150 ℃ of distillation temperatures, cooling temperature-13--17 ℃ condition, distill; Spinning after the condenses crystallization that distills out, the crystallisate oven dry obtains the sclareol finished product.
2. the production technique of sclareol according to claim 1 is characterized in that the temperature difference between the cold and hot two sides of said molecular still is 90-160 ℃.
3. the production technique of sclareol according to claim 1 is characterized in that the rotating speed of blade applicator in the molecular still is 100-250rpm/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103175682A CN102503775A (en) | 2011-10-19 | 2011-10-19 | Production process of sclareol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103175682A CN102503775A (en) | 2011-10-19 | 2011-10-19 | Production process of sclareol |
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| Publication Number | Publication Date |
|---|---|
| CN102503775A true CN102503775A (en) | 2012-06-20 |
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| CN2011103175682A Pending CN102503775A (en) | 2011-10-19 | 2011-10-19 | Production process of sclareol |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103215135A (en) * | 2013-04-07 | 2013-07-24 | 安徽嘉旗粮油工程技术有限公司 | Method for synchronously extracting sage clary essential oil and sclareol from sage clary |
| CN112679314A (en) * | 2020-12-29 | 2021-04-20 | 西安天美生物科技股份有限公司 | Preparation process of sclareol |
| CN112778084A (en) * | 2021-01-29 | 2021-05-11 | 西安天美生物科技股份有限公司 | Extraction process of sclareol |
| CN114573421A (en) * | 2022-03-17 | 2022-06-03 | 北京理工大学 | Method for extracting and purifying sclareol from sclareol fermentation liquor |
| CN114988983A (en) * | 2022-06-09 | 2022-09-02 | 新疆师范大学 | Method for separating sclareol from sclareol extract |
| CN115350495A (en) * | 2022-08-19 | 2022-11-18 | 焦作市馨之源科技有限公司 | Equipment and process for extracting sclareol |
| CN115636729A (en) * | 2022-10-31 | 2023-01-24 | 焦作市馨之源科技有限公司 | Method and device for purifying sclareol |
| CN117866705A (en) * | 2023-02-24 | 2024-04-12 | 吉林省久仙草农副产品加工有限责任公司 | Processing method for treating perilla seed residues after oil extraction by squeezing |
-
2011
- 2011-10-19 CN CN2011103175682A patent/CN102503775A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103215135A (en) * | 2013-04-07 | 2013-07-24 | 安徽嘉旗粮油工程技术有限公司 | Method for synchronously extracting sage clary essential oil and sclareol from sage clary |
| CN112679314A (en) * | 2020-12-29 | 2021-04-20 | 西安天美生物科技股份有限公司 | Preparation process of sclareol |
| CN112778084A (en) * | 2021-01-29 | 2021-05-11 | 西安天美生物科技股份有限公司 | Extraction process of sclareol |
| CN114573421A (en) * | 2022-03-17 | 2022-06-03 | 北京理工大学 | Method for extracting and purifying sclareol from sclareol fermentation liquor |
| CN114988983A (en) * | 2022-06-09 | 2022-09-02 | 新疆师范大学 | Method for separating sclareol from sclareol extract |
| CN115350495A (en) * | 2022-08-19 | 2022-11-18 | 焦作市馨之源科技有限公司 | Equipment and process for extracting sclareol |
| CN115350495B (en) * | 2022-08-19 | 2023-11-21 | 焦作市馨之源科技有限公司 | Equipment and process for extracting sclareol |
| CN115636729A (en) * | 2022-10-31 | 2023-01-24 | 焦作市馨之源科技有限公司 | Method and device for purifying sclareol |
| CN117866705A (en) * | 2023-02-24 | 2024-04-12 | 吉林省久仙草农副产品加工有限责任公司 | Processing method for treating perilla seed residues after oil extraction by squeezing |
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Application publication date: 20120620 |