CN103215135A - Method for synchronously extracting sage clary essential oil and sclareol from sage clary - Google Patents
Method for synchronously extracting sage clary essential oil and sclareol from sage clary Download PDFInfo
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Abstract
The invention relates to a method for synchronously extracting sage clary essential oil and sclareol from sage clary. The production technology comprises the steps of (a) crushing sage clary, (b) distilling essential oil by negative-pressure water vapor, (c) multi-stage countercurrent pulse extraction, (d) negative-pressure countercurrent film evaporation, (e) negative-pressure distillation concentration, (f) negative-pressure vapor distillation and desolvation, (g) condensation and separation of a solvent, (h) stewing by waste water, and (i) exhaust paraffin oil absorption. By adopting the method, the sage clary essential oil and the sclareol are synchronously extracted; the yields of the sage clary essential oil and the sclareol are greatly improved; large-scale and industrial continuous production of the sage clary essential oil and the sclareol is achieved; the problems of large solvent input and low extraction yield in industrial production of the sage clary essential oil and the sclareol are solved; and the method is free of environmental pollution and low in production cost, is an innovative technology of extracting the sage clary essential oil and the sclareol from the sage clary, and has great economic benefit and social benefit.
Description
Technical field
The present invention relates to the spices chemical field, relate in particular to a kind of production method from Salvia Sclare L. simultaneous extraction Salvia Sclare L. essential oil and sclareol.
Background technology
Salvia Sclare L. is a kind of biennial or perennial herb, high about 1～2 meter, and bottom stem lignifying, upright, branch, complete stool tomentellate.Single leaf is to life, oval or oblong.Originate in French Ge Lasi area, after extend to the Russia and the area, the peninsula, Crimea of Ukraine, and Moldova, Uzbekistan, the East European countries such as Bulgaria, the North Carolina Na Zhou of the U.S. also has establishing in large scale.Domestic main planting site is at present: Henan, Hebei, Shanxi, Shaanxi, Gansu and Xinjiang etc.Development product has Salvia Sclare L.oil, clary sage concrete, sclareol from Salvia Sclare L., products such as Sclareolide and imperial saliva ether.
Salvia Sclare L. essential oil and sclareol are important perfume bases, are the natural matters of producing imperial saliva ether, are mainly used in the typing of spices odor type.World market Salvia Sclare L. essential oil and sclareol by U.S.'s control, are Ukraine secondly mainly.Domestic, the world market is increasing to the demand of Salvia Sclare L. essential oil and sclareol.At present, domestic have only Shaanxi, the several producers in Xinjiang to extract Salvia Sclare L. essential oil and sclareol from Salvia Sclare L., all be to adopt jar group, batch production mode on a small scale to extract a kind of in Salvia Sclare L. essential oil or the sclareol, because be subjected to the restriction of production technique, its product production and quality do not satisfy the demand in market far away.CN102503775A discloses a kind of production technique of sclareol, and it is that 90～120 ℃ sherwood oil is an extraction agent that this method adopts boiling range, adopts molecular distillation technique to purify again extract sclareol medicinal extract in extraction kettle after; CN101323559A also discloses a kind of production technique of sclareol, is directly to adopt molecular still to extract sclareol from clary sage concrete.The production technique of above-mentioned sclareol adopts extraction kettle interrupted extraction technology, and not only output is little, energy consumption is high, and the medicinal extract extraction yield is low, residual sclareol amount is big in the Salvia Sclare L. slag.The Salvia Sclare L. essential oil then generally adopts the water vapour atmospheric distillation, and Salvia Sclare L. extracts essential oil rate is lower.
Therefore, be necessary to develop the high extraction of a kind of Salvia Sclare L. essential oil and sclareol and the production technique of environment-friendly type.
Summary of the invention
The object of the present invention is to provide a kind of from Salvia Sclare L. the production method of simultaneous extraction Salvia Sclare L. essential oil and sclareol; production method of the present invention has increased substantially Salvia Sclare L. essential oil and sclareol yield; mass-producing, the industrialization serialization production of Salvia Sclare L. essential oil and sclareol have been realized; there is not environmental pollution; production cost is low;, economic benefit and social benefit are huge.
Provided by the present invention from Salvia Sclare L. the production method of simultaneous extraction Salvia Sclare L. essential oil and sclareol, comprise in the production technique: (a) Salvia Sclare L. is pulverized, (b) negative pressure wet distillation essential oil extracts the Salvia Sclare L. essential oil, (c) multi-stage countercurrent pulse extraction, (d) negative pressure adverse current thin film evaporation, (e) vacuum distillation concentration extraction sclareol;
Wherein the extraction solvent in the step (a) is a normal hexane, and the mass ratio of extraction solvent and Salvia Sclare L. is: 0.5～1.5:1, preferred 1:1.Wherein extraction solvent also can be industrial normal hexane.
As optimal technical scheme, described production method, after concentrating, vacuum distillation also carries out following technology: (f) negative pressure wet distillation precipitation, (g) solvent condenses is separated, (h) waste water boiling, (i) the tail gas paraffin oil absorbs.
Fig. 1 is a process flow sheet of the present invention.
Wherein, described step (a) Salvia Sclare L. crushing process is: it is long that the Salvia Sclare L. raw material is ground into 20～50mm with pulverizer.Contain moisture 10～60% in the Salvia Sclare L. raw material, sclareol content 〉=0.5%, Salvia Sclare L. essential oil content 〉=0.1%.
Wherein, described step (b) negative pressure wet distillation Salvia Sclare L. essential oil process is: the Salvia Sclare L. raw material after the pulverizing seals conveyor delivery in the wet distillation tower through material, feed the direct saturated steam of 0.05Mpa in the tower, Salvia Sclare L. essential oil in the Salvia Sclare L. is become gaseous state by wet distillation, enter condenser condenses again, enter diversion box after the condensation, Salvia Sclare L. essential oil and water sepn promptly get the Salvia Sclare L. essential oil.Isolated liquid water can be used as the Salvia Sclare L. toilet water; Salvia Sclare L. essential oil extraction yield 〉=95%.
Preferably, rectifying tower pressure is-0.03～-0.05MPa, for example be-0.035MPa ,-0.045MPa etc., be preferably-0.04MPa.
Wherein, the process of described step (c) multi-stage countercurrent pulse extraction is: the Salvia Sclare L. material behind the extraction essential oil seals conveyor delivery in extractor by material, under 50-55 ℃, be that 1.2%～1.5% extraction solvent spray soaks extraction earlier by containing the sclareol mass concentration, drain, and then be 1.0～1.1% through containing the sclareol mass concentration respectively, 0.8～0.9%, 0.6～0.7%, 0.4～0.5%, 0.2～0.3%, 0.05～0.15% extraction solvent seven grades of sprays successively soaks extraction, drain, cycling extraction 120～180min repeatedly, soak extraction with normal hexane solvent spray again, realize multi-stage countercurrent pulse extraction.Salvia Sclare L. in extractor, contain the sclareol amount from more to less, the normal hexane solvent sprays that it contains the sclareol amount from less to more in the extractor, realizes counter-current extraction.
For multi-stage countercurrent pulse extraction, its process is as follows:
Seven grades of sprays soak in the extraction process, in the end adopt pure normal hexane to soak extraction together as extraction solution, front Salvia Sclare L. is together extracted as extraction solution with the solution after this extraction then, by that analogy, sclareol concentration is more and more higher in its extraction solution like this, from back to front.
Seven grades of sprays soak the benefit that extracts and are, all adopt pure normal hexane with respect to each grade, the consumption of its normal hexane is very big, and the concentration of sclareol is very low, adopt aforesaid way, can reduce the consumption of solvent normal hexane, and obtain having the sclareol of higher concentration, reduce the load of subsequent evaporation operation.
Preferably, the mass concentration of described seven grades of spray immersion extraction liquids is 1.2%, 1.0%, 0.8%, 0.6%, 0.4%, 0.2%, 0.1%.
Wherein, described step (d) negative pressure adverse current thin film evaporation process is: the solution that contains sclareol that is obtained by step (c) filters through 120 order coarse filters earlier, filter through 320 order accurate filters again, pump into one by pump and imitate negative pressure adverse current thin-film evaporator, solution becomes film like and solvent vapo(u)r countercurrent flow in vaporizer, the normal hexane solvent of 50～65 ﹪ in the mixed solution is evaporated, mixed solution after the evaporation enters two successively and imitates thin vaporizer of adverse currents and the thin vaporizer of three-effect counter flow, evaporates 60～80% solvent and 95～98% solvent respectively.Wherein coarse filter removes by filter the impurity of larger particles, and accurate filter removes by filter fine impurity.
Preferably, the evaporating pressure of the thin vaporizer of described adverse current is-0.03～-0.05MPa, be preferably-0.04MPa;
Preferably, described one vaporization temperature of imitating the thin vaporizer of adverse current is 55～60 ℃, 65～70 ℃ of the vaporization temperatures of the thin vaporizer of two effect adverse currents, and the vaporization temperature of the thin vaporizer of three-effect counter flow is 80～85 ℃.
Wherein, the process of described step (e) vacuum distillation concentration extraction sclareol is: the sclareol solution that obtains after step (d) evaporation is pumped to reboiler and is heated to 90～95 ℃, enter then in the vacuum distillation tower and distill, remaining solvent is thoroughly distilled to be removed, and enters the solvent condenses system under suction function; Sclareol liquid after distillation concentrates behind cooling forming, becomes the solid sclareol again.The outward appearance of the solid sclareol that obtains is the olive-green solid, has grane ambra fragrance, fusing point: 50～60 ℃, and sclareol content 〉=60%, residual solvent≤100ppm.
Preferably, distillation tower has 3～5 layers of column plate.
Preferably, the pressure in distillation tower when distillation is-0.03～-0.05MPa, be preferably-0.04MPa.
Wherein, the process of described step (f) negative pressure wet distillation precipitation is: the Salvia Sclare L. behind the extraction sclareol enters in the continuous wet distillation precipitation of the vertical multilayer tower through handling equipment, be provided with the pre-delamination of multilayer in the precipitation tower, the heating of employing indirect steam, under stirring action, at first remove 70% free solvent, fall into two-layer air-permeable layer then, continue to remove the solvent in the Salvia Sclare L., then fall into wet distillation precipitation layer, pressure is that the saturated steam of 0.05MPa evenly sprays in the Salvia Sclare L., regulate open steam pressure the residual solvent of Salvia Sclare L. inner about 30% is distilled away, the solvent gas that evaporates with pre-delamination enters condenser system under suction function; The Salvia Sclare L. that removes solvent enters 28～30 ℃ of cold wind pull-ups again except that the moisture in the Salvia Sclare L..Extract the Salvia Sclare L. slag residual solvent≤300ppm behind the sclareol, moisture≤20%, the effective constituent in the Salvia Sclare L. residue can be protected, so that later use in the temperature of Salvia Sclare L. residue≤40 ℃ under this temperature; The Salvia Sclare L. slag as fertilizer sources that removes solvent returns the farmland, is good fertilizer, and waste residue becomes byproduct, has realized zero pollution, zero release.
Preferably, described wet distillation precipitation pressure tower is-0.01～-0.03MPa, be preferably-0.02MPa.
Wherein, described step (g) solvent condenses separating process is: the solvent gas that contains that comes out from step (c) enters the leaching condenser, the solvent vapo(u)r that evaporates from step (d) enters vaporizer-condenser, the solvent vapo(u)r that distills from step (e) enters distiller condenser, the solvent vapo(u)r that distills from step (f) enters to steam and takes off condenser, the not noncondensing gas of above-mentioned all condensers enters the further condensation of last condenser, solvent vapo(u)r is condensed into liquid state and enters diversion box, depositing in water is in lower floor, the normal hexane solvent floats over the upper strata and flows into solvent storehouse recycle, and isolated water enters the wastewater boilling tank boiling.
Wherein, described step (h) waste water digestion process is: the isolated water of step (g) enters the wastewater boilling tank boiling, and boiling temperature is 92～98 ℃, is preferably 95～98 ℃.Waste water after the boiling does not contain solvent, has realized zero pollution, zero release.
Preferably, described step (i) tail gas paraffin oil absorption process is: from the last condenser of step (g), come out contain micro-normal hexane do not coagulate gas, be imported into the paraffin oil packed absorber bottom of solubilized normal hexane, the low paraffin oil of temperature from top to bottom, what contain solvent does not coagulate gas from bottom to top, paraffin oil and coagulate gas abundant counter current contact in packed absorber, the normal hexane that coagulates in the gas is not absorbed by paraffin oil, air is then drawn by induced draft fan and is discharged to outside the workshop, enter the filler Analytic Tower after paraffin oil is heated to 110～120 ℃ then, the normal hexane gas that parses enters condenser system and is condensed into liquid recycling; After the paraffin oil of having resolved normal hexane is cooled to 30～35 ℃, enters the absorption tower again and absorb normal hexane gas.Paraffin oil absorbs, resolves to a working cycle.
The invention has the beneficial effects as follows:
1, extraction yield height: the synergistic effect of the negative pressure wet distillation that adopts and industrial normal hexane solvent multi-stage countercurrent pulse extraction technology, make Salvia Sclare L. essential oil and sclareol its extraction yield when not adopting molecular distillation technology can reach more than 95%, especially when sclareol content is low to moderate 0.5% in the Salvia Sclare L., present method still can be extracted, and makes that sclareol content only is 0.05% in the Salvia Sclare L. slag;
2, save the energy: extraction solvent is than low, and industrial normal hexane and Salvia Sclare L. mass ratio are 0.5～15:1, and the quantity of solvent that puts into production reduces significantly, therefore evaporates the required energy and reduces significantly; The boiling point of extraction solvent industry normal hexane is lower than above-mentioned patent solvent sherwood oil, and the required energy is few during the solvent evaporation phase transformation;
3, good product quality: the sclareol purity height that extracts behind the employing negative pressure wet distillation extraction Salvia Sclare L. essential oil, of light color, outward appearance olive-green solid has grane ambra fragrance, fusing point: 50～60 ℃, residual solvent≤100ppm;
4, zero pollution, zero release: isolated waste water is not direct discharging after the solvent condenses, but increases cooking process one, and waste water is heated to 92～98 ℃, makes dissolved a small amount of solvent evaporative condenser recovery in the waste water, does not contain solvent in the waste water of final discharging; Adopt the paraffin oil solvent recovery technology from vent gas, do not contain solvent in the final discharge tail gas; Adopt negative pressure wet distillation precipitation technology, make Salvia Sclare L. flower slag return the farmland, do not have waste as good organic fertilizer.
5, output height: former intermittent type, pot group type are produced and can only be handled 30～50 tons of Salvia Sclare L. every day, and technology of the present invention makes output can reach 2000 tons of Salvia Sclare L. material every day.
The present invention increases substantially Salvia Sclare L. and extracts Salvia Sclare L. essential oil and sclareol output, and its yield can reach 95% when not adopting molecular distillation technique, has solved big, the low difficult problem of extraction yield of solvent input amount in the sclareol suitability for industrialized production; Do not have environmental pollution, production cost is low, has realized mass-producing, industrialization, the serialization production of Salvia Sclare L. essential oil and sclareol, is the innovative technology that Salvia Sclare L. extracts Salvia Sclare L. essential oil and sclareol, and economic benefit and social benefit are huge.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
For ease of understanding the present invention, it is as follows that the present invention enumerates embodiment.Those skilled in the art should understand that described embodiment helps to understand the present invention, should not be considered as concrete restriction of the present invention.
Embodiment 1
(a) the Salvia Sclare L. crushing process is: it is long that the Salvia Sclare L. raw material is ground into 20mm with pulverizer;
(b) negative pressure wet distillation Salvia Sclare L. essential oil: the Salvia Sclare L. raw material after the pulverizing seals conveyor delivery in the wet distillation tower through material, feed the direct saturated steam of 0.05Mpa in the tower, Salvia Sclare L. essential oil in the Salvia Sclare L. is become gaseous state by wet distillation, enter condenser condenses again, enter diversion box after the condensation, Salvia Sclare L. essential oil and water sepn promptly get the Salvia Sclare L. essential oil; Wherein rectifying tower pressure is-0.04M;
(c) multi-stage countercurrent pulse extraction: the Salvia Sclare L. material behind the extraction essential oil seals conveyor delivery in extractor by material, under 55 ℃, be that 1.2% extraction solvent spray soaks extraction, drains earlier by containing the sclareol mass concentration, and then respectively through contain the sclareol mass concentration be 1.0%, 0.8%, 0.6%, 0.4%, 0.2%, 0.1% extraction solvent successively seven grades of sprays soak extraction, drain, cycling extraction 180min repeatedly, soak extraction with normal hexane solvent spray again, realize multi-stage countercurrent pulse extraction;
(d) negative pressure adverse current thin film evaporation: the solution that contains sclareol that is obtained by step (c) filters through 120 order coarse filters earlier, filter through 320 order accurate filters again, pump into one by pump and imitate negative pressure adverse current thin-film evaporator, solution becomes film like and solvent vapo(u)r countercurrent flow in vaporizer, the normal hexane solvent of 50 ﹪ in the mixed solution is evaporated, mixed solution after the evaporation enters two successively and imitates thin vaporizer of adverse currents and the thin vaporizer of three-effect counter flow, evaporates 60% solvent and 98% solvent respectively; The evaporating pressure of the thin vaporizer of described adverse current is-0.05MPa; Described one vaporization temperature of imitating the thin vaporizer of adverse current is 55 ℃, 65 ℃ of the vaporization temperatures of the thin vaporizer of two effect adverse currents, and the vaporization temperature of the thin vaporizer of three-effect counter flow is 85 ℃;
(e) vacuum distillation concentration extraction sclareol: the sclareol solution that obtains after step (d) evaporation is pumped to reboiler and is heated to 90 ℃, enter then in the vacuum distillation tower and distill, remaining solvent is thoroughly distilled to be removed, and enters the solvent condenses system under suction function; Sclareol liquid after distillation concentrates behind cooling forming, becomes the solid sclareol again; The distillation tower column plate that is of five storeys; Pressure during the distillation tower distillation is-0.04MPa;
(f) negative pressure wet distillation precipitation: the Salvia Sclare L. behind the extraction sclareol enters in the continuous wet distillation precipitation of the vertical multilayer tower through handling equipment, be provided with the pre-delamination of multilayer in the precipitation tower, the heating of employing indirect steam, under stirring action, at first remove 70% free solvent, fall into two-layer air-permeable layer then, continue to remove the solvent in the Salvia Sclare L., then fall into wet distillation precipitation layer, pressure is that the saturated steam of 0.05MPa evenly sprays in the Salvia Sclare L., regulate open steam pressure the residual solvent of Salvia Sclare L. inner about 30% is distilled away, the solvent gas that evaporates with pre-delamination enters condenser system under suction function; The Salvia Sclare L. that removes solvent enters 28 ℃ of cold wind pull-ups again except that the moisture in the Salvia Sclare L.; Described wet distillation precipitation pressure tower is-0.02MPa;
(g) solvent condenses is separated: the solvent gas that contains that comes out from step (c) enters the leaching condenser, the solvent vapo(u)r that evaporates from step (d) enters vaporizer-condenser, the solvent vapo(u)r that distills from step (e) enters distiller condenser, the solvent vapo(u)r that distills from step (f) enters to steam and takes off condenser, the not noncondensing gas of above-mentioned all condensers enters the further condensation of last condenser, solvent vapo(u)r is condensed into liquid state and enters diversion box, depositing in water is in lower floor, the normal hexane solvent floats over the upper strata and flows into solvent storehouse recycle, and isolated water enters the wastewater boilling tank boiling;
(h) waste water boiling: the isolated water of step (g) enters the wastewater boilling tank boiling, and boiling temperature is 92～98 ℃.
(i) the tail gas paraffin oil absorbs: from the last condenser of step (g), come out contain micro-normal hexane do not coagulate gas, be imported into the paraffin oil packed absorber bottom of solubilized normal hexane, paraffin oil and coagulate gas abundant counter current contact in packed absorber, enter the filler Analytic Tower after paraffin oil is heated to 120 ℃ then, the normal hexane gas that parses enters condenser system and is condensed into liquid recycling; After the paraffin oil of having resolved normal hexane is cooled to 35 ℃, enters the absorption tower again and absorb normal hexane gas.
Present embodiment Salvia Sclare L. extracts essential oil rate is 98%, obtains olive-green solid sclareol, has grane ambra fragrance, fusing point: 50～60 ℃, and sclareol content 66%, residual solvent 70ppm.
Embodiment 2
(a) the Salvia Sclare L. crushing process is: it is long that the Salvia Sclare L. raw material is ground into 50mm with pulverizer;
(b) negative pressure wet distillation Salvia Sclare L. essential oil: the Salvia Sclare L. raw material after the pulverizing seals conveyor delivery in the wet distillation tower through material, feed the direct saturated steam of 0.05Mpa in the tower, Salvia Sclare L. essential oil in the Salvia Sclare L. is become gaseous state by wet distillation, enter condenser condenses again, enter diversion box after the condensation, Salvia Sclare L. essential oil and water sepn promptly get the Salvia Sclare L. essential oil; Wherein rectifying tower pressure is-0.03M;
(c) multi-stage countercurrent pulse extraction: the Salvia Sclare L. material behind the extraction essential oil seals conveyor delivery in extractor by material, under 50 ℃, be that 1.5% extraction solvent spray soaks extraction, drains earlier by containing the sclareol mass concentration, and then respectively through contain the sclareol mass concentration be 1.1%, 0.9%, 0.7%, 0.5%, 0.3%, 0.05% extraction solvent successively seven grades of sprays soak extraction, drain, cycling extraction 120min repeatedly, soak extraction with normal hexane solvent spray again, realize multi-stage countercurrent pulse extraction;
(d) negative pressure adverse current thin film evaporation: the solution that contains sclareol that is obtained by step (c) filters through 120 order coarse filters earlier, filter through 320 order accurate filters again, pump into one by pump and imitate negative pressure adverse current thin-film evaporator, solution becomes film like and solvent vapo(u)r countercurrent flow in vaporizer, the normal hexane solvent of 65 ﹪ in the mixed solution is evaporated, mixed solution after the evaporation enters two successively and imitates thin vaporizer of adverse currents and the thin vaporizer of three-effect counter flow, evaporates 80% solvent and 95% solvent respectively; The evaporating pressure of the thin vaporizer of described adverse current is-0.03MPa; Described one vaporization temperature of imitating the thin vaporizer of adverse current is 60 ℃, 70 ℃ of the vaporization temperatures of the thin vaporizer of two effect adverse currents, and the vaporization temperature of the thin vaporizer of three-effect counter flow is 80 ℃;
(e) vacuum distillation concentration extraction sclareol: the sclareol solution that obtains after step (d) evaporation is pumped to reboiler and is heated to 95 ℃, enter then in the vacuum distillation tower and distill, remaining solvent is thoroughly distilled to be removed, and enters the solvent condenses system under suction function; Sclareol liquid after distillation concentrates behind cooling forming, becomes the solid sclareol again; The distillation tower column plate that haves three layers; Pressure during the distillation tower distillation is-0.05MPa.
Present embodiment Salvia Sclare L. extracts essential oil rate is 95%, obtains olive-green solid sclareol, has grane ambra fragrance, fusing point: 50～60 ℃, and sclareol content 69%, residual solvent 74ppm.
Applicant's statement, the present invention illustrates detailed process flow of the present invention by the foregoing description, but the present invention is not limited to above-mentioned detailed process flow, does not mean that promptly the present invention must rely on above-mentioned detailed process flow and could implement.The person of ordinary skill in the field should understand, any improvement in the present invention to the interpolation of the equivalence replacement of each raw material of product of the present invention and ancillary component, the selection of concrete mode etc., all drops within protection scope of the present invention and the open scope.
Claims (10)
1. the production method of simultaneous extraction Salvia Sclare L. essential oil and sclareol from a Salvia Sclare L., it is characterized in that, comprise in the production technique: (a) Salvia Sclare L. is pulverized, (b) negative pressure wet distillation Salvia Sclare L. essential oil, (c) multi-stage countercurrent pulse extraction, (d) negative pressure adverse current thin film evaporation, (e) vacuum distillation concentration extraction sclareol;
Wherein the extraction solvent in the step (a) is a normal hexane, and the mass ratio of extraction solvent and Salvia Sclare L. is: 0.5～1.5:1, preferred 1:1.
2. the method for claim 1 is characterized in that, also carries out following technology after vacuum distillation concentrates: (f) negative pressure wet distillation precipitation, and (g) solvent condenses is separated, (h) waste water boiling, (i) the tail gas paraffin oil absorbs.
3. method as claimed in claim 1 or 2 is characterized in that, described step (a) Salvia Sclare L. crushing process is: it is long that the Salvia Sclare L. raw material is ground into 20～50mm with pulverizer.
4. method as claimed in claim 1 or 2, it is characterized in that, described step (b) negative pressure wet distillation essential oil process is: the Salvia Sclare L. raw material after the pulverizing seals conveyor delivery in the wet distillation tower through material, feed the direct saturated steam of 0.05Mpa in the tower, Salvia Sclare L. essential oil in the Salvia Sclare L. is become gaseous state by wet distillation, enter condenser condenses again, enter diversion box after the condensation, Salvia Sclare L. essential oil and water sepn promptly get the Salvia Sclare L. essential oil;
Preferably, rectifying tower pressure is-0.03～-0.05MPa, be preferably-0.04MPa.
5. method as claimed in claim 1 or 2, it is characterized in that, the process of described step (c) multi-stage countercurrent pulse extraction is: the Salvia Sclare L. material behind the extraction essential oil seals conveyor delivery in extractor by material, under 50-55 ℃, be that 1.2%～1.5% extraction solvent spray soaks extraction earlier by containing the sclareol mass concentration, drain, and then be 1.0～1.1% through containing the sclareol mass concentration respectively, 0.8～0.9%, 0.6～0.7%, 0.4～0.5%, 0.2～0.3%, 0.05～0.15% extraction solvent seven grades of sprays successively soaks extraction, drain, cycling extraction 120～180min repeatedly, soak extraction with normal hexane solvent spray again, realize multi-stage countercurrent pulse extraction;
Preferably, the mass concentration of described seven grades of spray immersion extraction liquids is 1.2%, 1.0%, 0.8%, 0.6%, 0.4%, 0.2%, 0.1%.
6. method as claimed in claim 1 or 2, it is characterized in that, described step (d) negative pressure adverse current thin film evaporation process is: the solution that contains sclareol that is obtained by step (c) filters through 120 order coarse filters earlier, filter through 320 order accurate filters again, pump into one by pump and imitate negative pressure adverse current thin-film evaporator, solution becomes film like and solvent vapo(u)r countercurrent flow in vaporizer, the normal hexane solvent of 50～65 ﹪ in the mixed solution is evaporated, mixed solution after the evaporation enters two successively and imitates thin vaporizer of adverse currents and the thin vaporizer of three-effect counter flow, evaporates 60～80% solvent and 95～98% solvent respectively;
Preferably, the evaporating pressure of the thin vaporizer of described adverse current is-0.03～-0.05MPa, be preferably-0.04MPa;
Preferably, described one vaporization temperature of imitating the thin vaporizer of adverse current is 55～60 ℃, 65～70 ℃ of the vaporization temperatures of the thin vaporizer of two effect adverse currents, and the vaporization temperature of the thin vaporizer of three-effect counter flow is 80～85 ℃.
7. method as claimed in claim 1 or 2, it is characterized in that, the spissated process of described step (e) vacuum distillation is: the sclareol solution that obtains after step (d) evaporation is pumped to reboiler and is heated to 90～95 ℃, enter then in the vacuum distillation tower and distill, remaining solvent is thoroughly distilled to be removed, and enters the solvent condenses system under suction function; Sclareol liquid after distillation concentrates behind cooling forming, becomes the solid sclareol again;
Preferably, distillation tower has 3～5 layers of column plate;
Preferably, the pressure in distillation tower when distillation is-0.03～-0.05MPa, be preferably-0.04MPa.
8. method as claimed in claim 2, it is characterized in that, the process of described step (f) negative pressure wet distillation precipitation is: the Salvia Sclare L. behind the extraction sclareol enters in the continuous wet distillation precipitation of the vertical multilayer tower through handling equipment, be provided with the pre-delamination of multilayer in the precipitation tower, the heating of employing indirect steam, under stirring action, at first remove 70% free solvent, fall into two-layer air-permeable layer then, continue to remove the solvent in the Salvia Sclare L., then fall into wet distillation precipitation layer, pressure is that the saturated steam of 0.05MPa evenly sprays in the Salvia Sclare L., regulate open steam pressure the residual solvent of Salvia Sclare L. inner about 30% is distilled away, the solvent gas that evaporates with pre-delamination enters condenser system under suction function; The Salvia Sclare L. that removes solvent enters 28～30 ℃ of cold wind pull-ups again except that the moisture in the Salvia Sclare L.;
Preferably, described wet distillation precipitation pressure tower is-0.01～-0.03MPa, be preferably-0.02MPa.
9. method as claimed in claim 2, it is characterized in that, described step (g) solvent condenses separating process is: the solvent gas that contains that comes out from step (c) enters the leaching condenser, the solvent vapo(u)r that evaporates from step (d) enters vaporizer-condenser, the solvent vapo(u)r that distills from step (e) enters distiller condenser, the solvent vapo(u)r that distills from step (f) enters to steam and takes off condenser, the not noncondensing gas of above-mentioned all condensers enters the further condensation of last condenser, solvent vapo(u)r is condensed into liquid state and enters diversion box, depositing in water is in lower floor, the normal hexane solvent floats over the upper strata and flows into solvent storehouse recycle, and isolated water enters the wastewater boilling tank boiling.
10. method as claimed in claim 2 is characterized in that, described step (h) waste water digestion process is: the isolated water of step (g) enters the wastewater boilling tank boiling, and boiling temperature is 92～98 ℃, is preferably 95～98 ℃.
Preferably, described step (i) tail gas paraffin oil absorption process is: from the last condenser of step (g), come out contain micro-normal hexane do not coagulate gas, be imported into the paraffin oil packed absorber bottom of solubilized normal hexane, paraffin oil and coagulate gas abundant counter current contact in packed absorber, enter the filler Analytic Tower after paraffin oil is heated to 110～120 ℃ then, the normal hexane gas that parses enters condenser system and is condensed into liquid recycling; After the paraffin oil of having resolved normal hexane is cooled to 30～35 ℃, enters the absorption tower again and absorb normal hexane gas.
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| CN108570354A (en) * | 2018-05-03 | 2018-09-25 | 新疆天山香紫苏香料科技有限公司 | A kind of production method of perfume Fructus Perillae quintessence oil |
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| CN104629900A (en) * | 2015-01-28 | 2015-05-20 | 安徽嘉旗粮油工程技术有限公司 | Production method of synchronously extracting tea-seed oil and tea saponin from tea seed cakes |
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| CN105154236A (en) * | 2015-09-23 | 2015-12-16 | 陈富强 | Full-automatic electric heating triple-effect plant essential oil extracting and purifying integrated device |
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| CN106565812B (en) * | 2016-09-26 | 2018-12-07 | 中国林业科学研究院亚热带林业研究所 | A kind of continuous Extraction solvent high efficiente callback technique of Tea Saponin |
| CN108570354A (en) * | 2018-05-03 | 2018-09-25 | 新疆天山香紫苏香料科技有限公司 | A kind of production method of perfume Fructus Perillae quintessence oil |
| 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 |
| 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 |
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