CN101323559B - Preparing process of sclareol - Google Patents
Preparing process of sclareol Download PDFInfo
- Publication number
- CN101323559B CN101323559B CN2008101505421A CN200810150542A CN101323559B CN 101323559 B CN101323559 B CN 101323559B CN 2008101505421 A CN2008101505421 A CN 2008101505421A CN 200810150542 A CN200810150542 A CN 200810150542A CN 101323559 B CN101323559 B CN 101323559B
- Authority
- CN
- China
- Prior art keywords
- sclareol
- distillation
- temperature
- still
- open
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Landscapes
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a preparation technology of sclareol, which adopts a molecular still with a distance of 2cm to 5cm between an evaporating surface and a condensing surface. The technology of the invention is characterized in that the operation under the following technological conditions is carried out and comprises the following steps of: operating pressure for the still is 1Pa to 150Pa, distilling temperature is 100 DEG C to 400 DEG C, cooling temperature is minus 8 DEC G to minus 15 DEG C, rotating speed of a film applicator is 10rpm to 300rpm, remains of the first-step distillationare deemed as raw materials for a next distillation and are taken 2 times to 3 times of distillation, temperature contrast between the evaporating surface and the condensing surface is kept as 175 DEG C to 275 DEG C for each time of distillation, so as to completely separate and extract sclareol from clary sage concrete and ensure the yield of sclareol to reach 98 percent. The technology of the invention has the advantages of simple technology, short operating time, nonuse of solvent, nonproduction of other high boiling materials and pollution-free. The technology of the invention has high efficiency on extracting the sclareol, high product yield and high benefit, and is applicable to large-scale production of the sclareol.
Description
Technical field
The present invention relates to a kind of preparation technology of sclareol.
Background technology
Sclareol is a kind of good natural matter as synthetic Sclareolide and synthetic imperial saliva ethereal essence.Look into by retrieval new, domestic most producers after with Salvia Sclare L. plant extract Salvia Sclare L. essential oil residue or directly use the Salvia Sclare L. plant, adopt that the sherwood oil leaching is concentrated to obtain cyan clary sage concrete.But its contained sclareol is only at 35-50%, and kind is very low, is difficult to use in spices production.
The process for production of salvia sclarea alcohol that existing invention provides, be clary sage concrete to be dissolved in concentration be not less than 50% ethanol, through-17 ℃--20 ℃ of cryogenic freezing after-filtration add stoichiometric gac again, agitation and filtration, dilute with water filtrate makes concentration below 35%, and stirs, and the sclareol crystallization is separated out, refilter, centrifuge dehydration, vacuum drying, crushing packing.
Aforesaid method, though can obtain the sclareol of required purity, the weak point of this method: one is to use a large amount of solvents and gac, has increased production cost; The 2nd, required time is long, and production efficiency is low; The 3rd, lost part effective constituent, the product yield is low, influences economic benefit.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of technology simple at above-mentioned deficiency of the prior art, is convenient to operation, the preparation technology of the sclareol that production efficiency and product yield are high.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of preparation technology of sclareol, distance is the molecular still of 2-5cm between employing generating surface and the condensing surface, from clary sage concrete, extract sclareol, it is characterized in that operating with following processing condition: described distiller working pressure is 1-150pa, distillation temperature is 100 ℃-400 ℃, cooling temperature is-8 ℃--15 ℃, the blade applicator speed of rotation is 10-300rpm in the distiller, and the above single distilled steaming excess conduct of each distillation is the flow process of distillatory raw material next time, carry out 2-3 all over distillation, it is 175 ℃-275 ℃ that each distillation keeps the temperature head of molecular still generating surface and condensing surface.
Specific embodiment of the present invention is:
(1) will contain after the clary sage concrete chopping of sclareol 50% in the putting into material still, heater one then, making material still temperature rises gradually, open water ring vacuum pump simultaneously, organic solvent remaining in the clary sage concrete and volatile gas are extracted out, treating that clary sage concrete melts fully is liquid phase, keeps well heater one constant temperature;
(2) clary sage concrete after the liquefaction in the step (1) is imported in the good storage tank of preheating heater one; Open the one-level molecular still; Open refrigerator, make refrigerating fulid ethylene glycol at cold-trap one internal recycle; Open water ring vacuum pump; Open the fresh feed pump of one-level molecular still then;
(3) when opening the one-level molecular still, open secondary molecular still and three grades of molecule distillers, open refrigerator, open blade and Roots vaccum pump one, blade and Roots vaccum pump two, blade and Roots vaccum pump three and well heater one, making the generating surface of secondary molecular still and three grades of molecule distillers and condensing surface temperature head is 175 ℃-275 ℃; At this moment open the fresh feed pump of secondary molecular still and three grades of molecule distillers, in the still-process, it is the distillating material of secondary distillation that the one-level distillatory steams excess, and the steaming excess of secondary distillation is the distillating material of three-stage distillation, so distill for 2-3 time, promptly obtain pure content and be 90% sclareol.
For obtaining pure content at the sclareol product more than 95%, it with the pure content that makes in acetone solvent and the above-mentioned steps (3) 90% sclareol, with the weight percent sclareol: after the ratio of acetone solvent=1: 3, recrystallization in the airtight crystallization kettle one of successively packing into; Heater two under 40 ℃ of-45 ℃ of conditions of temperature, makes sclareol dissolving fully in crystallization kettle one, consoluet sclareol is imported in the crystallization kettle two leave standstill then, and cooling is opened water cooler again and lowered the temperature gradually naturally; Start agitator simultaneously, treat the sclareol sufficient crystallising after, filter, the sclareol after filtering is placed static oven dry in the vacuum shelf dryer, with the sclareol crushing screening of pulverizer after, promptly obtain pure content then at the sclareol more than 95% with crystallization.
The present invention compared with prior art has the following advantages: technology of the present invention is simple, and the operating time is short, does not use solvent, does not produce other high boiling material matter, environmentally safe; The present invention extracts sclareol efficient height, product yield height, and high efficiency is fit to the large-scale production sclareol.
Below by drawings and Examples, technical scheme of the present invention is described in further detail.
Description of drawings
Fig. 1 is preparation technology's schema of the present invention.
Fig. 2 is the process flow sheet of recrystallization of the present invention.
Description of reference numerals:
1-ization material still, 2-water ring vacuum pump, 3-one-level molecular still, 41-blade and Roots vaccum pump one, 42-blade and Roots vaccum pump two, 43-blade and Roots vaccum pump three, 5-secondary molecular still, three grades of molecule distillers of 6-, 7-well heater one, the 8-refrigerator, 9-electric control system, 10-cold-trap one, 11-cold-trap two, 12-cold-trap three, 13-cold-trap four, the 14-vacuum shelf dryer, 15-vacuum pump, 16-pulverizer, 17-crystallization kettle one, 18-agitator, 19-heating pipe line, 20-cooling pipeline, 21-crystallization kettle two, 22-whizzer, 23-well heater two, the 24-water cooler, the T-temperature is surveyed mouth, and the P-vacuum is surveyed mouth.
Embodiment
As shown in Figure 1, changing material still 1 is connected with Heat-transfer Oil Pump U by heating pipe line 19, Heat-transfer Oil Pump U is connected with well heater 1 by heating pipe line 19, cold-trap 1, cold-trap 2 11, cold-trap 3 12 all is connected with refrigerator 8 by cooling pipeline 20 with cold-trap 4 13, cold-trap 1 is connected with water ring vacuum pump 2 with change material still 1 respectively, cold-trap 2 11 is connected with blade and Roots vaccum pump group 1 with one-level molecular still 3 respectively, cold-trap 3 12 is connected with blade and Roots vaccum pump group 2 42 with secondary molecular still 5 respectively, cold-trap 4 13 is connected with blade and Roots vaccum pump group 3 43 with three grades of molecule distillers respectively, change material still 1 discharge port and be connected with storage tank P1, storage tank P1 is connected with one-level molecular still 3 opening for feeds by fresh feed pump Pi, one-level molecular still 3 discharge ports are connected with storage tank P2, storage tank P2 is connected with secondary molecular still 5 opening for feeds by fresh feed pump Pi, secondary molecular still 5 discharge ports are connected with storage tank P01 and P3, storage tank P3 is connected with three grades of molecule distiller 6 opening for feeds by fresh feed pump Pi, three grades of molecule distiller 6 discharge ports connect storage tank P02 and P4, storage tank P01, P02, P1, P2, P3, P4 is connected with well heater 1 by heating pipe line 19, changes material still 1, water ring vacuum pump 2, one-level molecular still 3, blade and Roots vaccum pump group 1, blade and Roots vaccum pump group 2 42, blade and Roots vaccum pump group 3 43, secondary molecular still 5, three grades of molecule distillers 6 all are connected with electric control system with Heat-transfer Oil Pump U.
As shown in Figure 2, the crystallization kettle 1 that has agitator 18 is connected with well heater 1, the crystallization kettle 2 21 that has agitator 18 is connected with refrigerator 8, crystallization kettle one 17 discharge ports connect crystallization kettle 2 21 opening for feeds, crystallization kettle 2 21 discharge ports connect whizzer 22, whizzer 22 also is connected with vacuum shelf dryer 14, and vacuum shelf dryer 14 is connected with vacuum pump 15 with pulverizer 16.
The present invention adopts between generating surface and the condensing surface apart from putting for the molecular still of 2-5cm, operate with following processing condition: the distiller working pressure is 1-150pa, distillation temperature is 100 ℃-400 ℃, cooling temperature is-8 ℃～-15 ℃, the speed of rotation of blade applicator is 10-300rpm in the distiller, and the above single distilled steaming excess conduct of each distillation is the distillatory distillating material next time, carry out 2-3 all over distillation, it is 175 ℃-275 ℃ that each distillation keeps distiller generating surface and condensing surface temperature head, sclareol in the clary sage concrete can be obtained abundant separation and Extraction like this, the sclareol productive rate reaches 98%.
Embodiment 1
The first step: 200 kilograms of the clary sage concretes that will contain sclareol 50%, put into volume after the chopping and be 500 liters change material still 1, heater 1 then, making material still 1 temperature rises to 110 ℃ gradually, open water ring vacuum pump SH simultaneously, making material still 1 pressure reaches 0.08Mpa, and organic solvent remaining in the clary sage concrete and volatile gas are extracted out, treating that clary sage concrete melts fully is liquid phase, keeps well heater one 7 constant temperature.
Second step: the good volume of clary sage concrete after will liquefy importing preheating is among 300 liters the storage tank P1, heater 1, and make storage tank P1 temperature rise to 140 ℃; Open one-level molecular still 3 (its generating surface area is 0.8 square metre, and the condensing surface area is 1.2 square metres, and the blade applicator rotating speed is 50-300rpm); Open refrigerator 8 and keep cooling temperatures-12 ℃, make refrigerating fulid ethylene glycol at cold-trap one 10 internal recycle; Open water ring vacuum pump 2 (SH), make the working pressure of system reach 130pa; Heater 1 to heat-conducting oil heating, makes temperature-stable at 160 ℃, opens the fresh feed pump Pi of one-level molecular still 3 then, and feeding rate is 30 kilograms/hour, and the blade applicator rotating speed of one-level molecular still 3 is 73rpm.This step is with residual solvent in the clary sage concrete and the whole evaporative removals of volatile (lower boiling) material.
The 3rd step: when opening one-level molecular still 3, open secondary molecular still 5, three grades of molecule distillers 6.Open refrigerator 8, make the condensing surface temperature of secondary molecular still 5 and three grades of molecule distillers 6 remain on 30 ℃; Open blade and Roots vaccum pump 1, blade and Roots vaccum pump 2 42, blade and Roots vaccum pump 3 43, make system operation pressure reach 2.5pa; Heater 1, thermal oil is heated and circulates, make the generating surface temperature of secondary molecular still 5 and three grades of molecule distillers 6 reach 260 ℃, about 230 ℃ of the generating surface of maintenance secondary molecular still 5 and three grades of molecule distillers 6 and condensing surface temperature heads; At this moment open the fresh feed pump Pi of secondary molecular still 5 and three grades of molecule distillers 6, feeding rate maintenance 25-30 kilogram/hour; The blade applicator rotating speed 73rpm of secondary molecular still 5 and three grades of molecule distillers 6.In the still-process, it is the distillating material of secondary distillation that the one-level distillatory steams excess, and the steaming excess of secondary distillation is the distillating material of three-stage distillation.So 2-3 distillation promptly obtains pure content and is 106 kilograms of 90% sclareols, and pure content is 76.5 kilograms of 6% raffinates, 17.5 kilograms in the volatile liquid mixture of cooling recovery.The sclareol productive rate is 95.4%.
For reaching pure content at the sclareol product more than 95%, adopting the pure content that acetone solvent and embodiment 1 are made among the present invention is 90% sclareol, with the weight percent sclareol: the ratio of acetone solvent=1: 3, the volume of successively packing into are recrystallizations in 500 liters the airtight crystallization kettle 1.Heater 2 23, under 40 ℃ of-45 ℃ of conditions of temperature, make sclareol dissolving fully in crystallization kettle 1, consoluet sclareol is imported in the crystallization kettle 2 21 leave standstill then, naturally cooling is 4 hours, opens water cooler 24 again and is cooled to-15 ℃ gradually; Start agitator 18 simultaneously, stir speed (S.S.) 40rpm, need 10-12 hour approximately, treat its sufficient crystallising after, be the whizzer of 1000rpm again with rotating speed, 120 order filter clothes filter, sclareol after filtering is placed static oven dry in the vacuum shelf dryer 14, and during oven dry, vacuum shelf dryer 14 pressure are 0.08Mpa, temperature is at 45 ℃-55 ℃, and drying time is 10-12 hour.Use pulverizer 16 with the sclareol crushing screening after the crystallization then, obtain pure content at the sclareol more than 95%.With the double-deck non-toxic plastic bag airtight package of fiber can liner.
The embodiment of the invention two products obtained therefroms, pure content are more than 95%, and moisture content is below 0.3%.
Claims (2)
1. the preparation technology of a sclareol, distance is the molecular still of 2-5cm between employing generating surface and the condensing surface, from clary sage concrete, extract sclareol, operate with following processing condition: described distiller working pressure is 1-150pa, distillation temperature is 100 ℃-400 ℃, cooling temperature is-8 ℃--15 ℃, the blade applicator speed of rotation is 10-300rpm in the distiller, and the above single distilled steaming excess conduct of each distillation is the flow process of distillatory raw material next time, carry out 2-3 all over distillation, it is 175 ℃-275 ℃ that each distillation keeps the temperature head of molecular still generating surface and condensing surface; It is characterized in that specific embodiment is:
(1) will contain after the clary sage concrete chopping of sclareol 50% in the putting into material still, heater one then, making material still temperature rises gradually, open water ring vacuum pump simultaneously, organic solvent remaining in the clary sage concrete and volatile gas are extracted out, treating that clary sage concrete melts fully is liquid phase, keeps well heater one constant temperature;
(2) clary sage concrete after the liquefaction in the step (1) is imported in the good storage tank of preheating heater one; Open the one-level molecular still; Open refrigerator, make refrigerating fulid ethylene glycol at cold-trap one internal recycle; Open water ring vacuum pump; Open the fresh feed pump of one-level molecular still then;
(3) when opening the one-level molecular still, open secondary molecular still and three grades of molecule distillers, open refrigerator, open blade and Roots vaccum pump one, blade and Roots vaccum pump two, blade and Roots vaccum pump three and well heater one, making the generating surface of secondary molecular still and three grades of molecule distillers and condensing surface temperature head is 175 ℃-275 ℃; At this moment open the fresh feed pump of secondary molecular still and three grades of molecule distillers, in the still-process, it is the distillating material of secondary distillation that the one-level distillatory steams excess, and the steaming excess of secondary distillation is the distillating material of three-stage distillation, so distill for 2-3 time, promptly obtain pure content and be 90% sclareol.
2. according to the preparation technology of the described a kind of sclareol of claim 1, it is characterized in that the pure content that will make in acetone solvent and the step (3) is 90% sclareol, with the weight percent sclareol: the ratio of acetone solvent=1: 3, recrystallization in the airtight crystallization kettle one of successively packing into; Heater two under 40 ℃ of-45 ℃ of conditions of temperature, makes sclareol dissolving fully in crystallization kettle one, consoluet sclareol is imported in the crystallization kettle two leave standstill then, and cooling is opened water cooler again and lowered the temperature gradually naturally; Start agitator simultaneously, treat the sclareol sufficient crystallising after, filter, the sclareol after filtering is placed static oven dry in the vacuum shelf dryer, with the sclareol crushing screening of pulverizer after, promptly obtain pure content then at the sclareol more than 95% with crystallization.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008101505421A CN101323559B (en) | 2008-08-05 | 2008-08-05 | Preparing process of sclareol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008101505421A CN101323559B (en) | 2008-08-05 | 2008-08-05 | Preparing process of sclareol |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101323559A CN101323559A (en) | 2008-12-17 |
| CN101323559B true CN101323559B (en) | 2010-12-22 |
Family
ID=40187286
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2008101505421A Expired - Fee Related CN101323559B (en) | 2008-08-05 | 2008-08-05 | Preparing process of sclareol |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101323559B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107841377A (en) * | 2017-10-11 | 2018-03-27 | 广东贡品沉香产业投资有限公司 | A kind of agilawood essential oil decompression fractionation unit |
| CN108165433A (en) * | 2018-02-06 | 2018-06-15 | 青海省轻工业研究所有限责任公司 | A kind of Qinghai-Tibet characteristic assembled alcoholic drinks and preparation method thereof |
| 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 |
| 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 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1594303A (en) * | 2004-07-05 | 2005-03-16 | 天津大学 | Method for separation purification of sclareolide from synthetic sclareol composites |
-
2008
- 2008-08-05 CN CN2008101505421A patent/CN101323559B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1594303A (en) * | 2004-07-05 | 2005-03-16 | 天津大学 | Method for separation purification of sclareolide from synthetic sclareol composites |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101323559A (en) | 2008-12-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101323559B (en) | Preparing process of sclareol | |
| CN101851559A (en) | Method for extracting rose essential oil from rose dregs | |
| CN102031199A (en) | Method for extracting rose essential oil from fresh rose flowers | |
| CN102120935A (en) | Method for recycling heptane and saxol from waste saxol containing heptane | |
| CN102503775A (en) | Production process of sclareol | |
| CN101898947A (en) | Method for producing 2,4-dichloroacetophenone by using solid waste chlorobenzene tar as raw material | |
| CN101074258B (en) | Method for separating and extracting phytosterin and Vitamin E from soyabean deodorization distillate | |
| CN105541543B (en) | The method of purification of durol | |
| CN1298904A (en) | Process for preparing crystal lycopene and/or lycopene oil resin from tomato paste | |
| CN104844474B (en) | Method and device for recycling cyhalothrin and solvent thereof from cyhalothrin centrifugal mother liquid | |
| CN103484154A (en) | Condensed water stripped crude oil stabilization method and special device thereof | |
| CN105536275B (en) | A kind of concentrating and separating method and apparatus of antarctic krill oil extract solution | |
| CN102321436B (en) | Resin short path distiller and resin distillation process | |
| CN105272815A (en) | Method for extracting methylnaphthalene in C10 aromatics | |
| CN101381279B (en) | Fuel ethanol dehydration apparatus and method | |
| CN101487036A (en) | Production method of guanine nucleosides | |
| CN1923831A (en) | Preparation technology of grape seed polyphenols | |
| CN103012426A (en) | Method for preparing high-purity natural 1,8-cineole by adopting freezing crystallization method | |
| CN102260145B (en) | Method for continuous fractional separation and purification of effective ingredients of star anise | |
| CN206887051U (en) | A kind of essential oil extraction device | |
| CN212769939U (en) | Treatment system for cellulose production wastewater | |
| CN205501169U (en) | System for separation N - methyl 2 pyrrolidone chloroform | |
| CN109503663A (en) | A kind of industrialized preparing process of bis- (2,6- di-t-butyl -4- aminomethyl phenyl) pentaerythritol phosphites | |
| CN204952333U (en) | Instantaneous overheated steam distillation equipment | |
| CN205323246U (en) | Concentrated separator of euphausia superba oil extract |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20101222 Termination date: 20120805 |