CN103215135B - 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 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 approximately 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 Peninsula, Crimea of Russia and Ukraine, and Moldova, Uzbekistan, the East European countries such as Bulgarian, 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.The product of developing from Salvia Sclare L. has Salvia Sclare L.oil, clary sage concrete, sclareol, the 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 sizing of spices odor type.World market Salvia Sclare L. essential oil and sclareol are mainly controlled by the U.S., are secondly Ukraine.Domestic, world market is increasing to the demand of Salvia Sclare L. essential oil and sclareol.At present, domestic only have Shaanxi, the several producers in Xinjiang from Salvia Sclare L., to extract Salvia Sclare L. essential oil and sclareol, all to adopt tank group, batch production mode on a small scale to extract a kind of in Salvia Sclare L. essential oil or sclareol, owing to being subject to the restriction of production technique, its product production and quality can not meet the demand in market far away.CN102503775A discloses a kind of production technique of sclareol, and it is that the sherwood oil of 90～120 ℃ is extraction agent that the method adopts boiling range, adopts molecular distillation technique to purify after extracting sclareol medicinal extract in extraction kettle again; CN101323559A also discloses a kind of production technique of sclareol, is directly from clary sage concrete, to adopt molecular still to extract sclareol.The production technique of above-mentioned sclareol adopts extraction kettle interrupted extraction technique, and not only output is little, energy consumption is high, and medicinal extract extraction yield is low, residual sclareol amount is large in Salvia Sclare L. slag.Salvia Sclare L. essential oil generally adopts water vapour atmospheric distillation, and the extraction yield of Salvia Sclare L. essential oil is lower.
Therefore, be necessary to develop a kind of Salvia Sclare L. essential oil and the high extraction of 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; having realized mass-producing, the industrialization serialization of Salvia Sclare L. essential oil and sclareol produces; there is no 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, production technique comprises: (a) Salvia Sclare L. is pulverized, (b) negative pressure wet distillation extraction of essential oil 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 step (a) is normal hexane, and the mass ratio of extraction solvent and Salvia Sclare L. is: 0.5～1.5:1, preferably 1:1.Wherein extraction solvent also can be industrial normal hexane.
As optimal technical scheme, described production method, after vacuum distillation is concentrated, also carry out following technique: (f) negative pressure wet distillation precipitation, (g) solvent condenses is separated, (h) waste water boiling, (i) tail gas paraffin oil absorbs.
Fig. 1 is process flow sheet of the present invention.
Wherein, described step (a) Salvia Sclare L. crushing process is: Salvia Sclare L. raw material is ground into 20～50mm with pulverizer long.In Salvia Sclare L. raw material, moisture content 10～60%, 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 pulverizing is transported in wet distillation tower through material envelope transfer roller, in tower, pass into the direct saturated steam of 0.05Mpa, Salvia Sclare L. essential oil in Salvia Sclare L. is become gaseous state by wet distillation, enter again condenser condenses, after condensation, enter diversion box, Salvia Sclare L. essential oil obtain Salvia Sclare L. essential oil separated with water.Isolated liquid water can be used as Salvia Sclare L. toilet water; Salvia Sclare L. extraction of essential oil rate >=95%.
Preferably, Rectification column pressure is-0.03～-0.05MPa, such as being-0.035MPa ,-0.045MPa etc., is preferably-0.04MPa.
Wherein, the process of described step (c) multi-stage countercurrent pulse extraction is: the Salvia Sclare L. material after extraction essential oil is by expecting that sealing transfer roller is transported in extractor, at 50-55 ℃, first by the extraction solvent spray that is 1.2%～1.5% containing sclareol mass concentration, soak extraction, drain, and then through containing sclareol mass concentration, be 1.0～1.1% respectively, 0.8～0.9%, 0.6～0.7%, 0.4～0.5%, 0.2～0.3%, 0.05～0.15% extraction solvent successively seven grades of sprays soaks extraction, drain, iterative cycles extraction 120～180min, with normal hexane solvent spray, soak extraction again, realize multi-stage countercurrent pulse extraction.Salvia Sclare L. in extractor containing sclareol amount from more to less, normal hexane solvent sprays in extractor it containing sclareol amount from less to more, realizes counter-current extraction.
For multi-stage countercurrent pulse extraction, its process is as follows:
Seven grades of sprays soak in extraction process, in the end adopt together pure normal hexane to soak extraction as extraction solution, then with the solution after this extraction, as extraction solution, Salvia Sclare L. together is above extracted, by that analogy, in its extraction solution, sclareol concentration is more and more higher like this, from back to front.
Seven grades of sprays soak the benefit extracting and are, with respect to every one-level, all adopt pure normal hexane, the consumption of its normal hexane is very large, 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 that seven grades of described sprays soak extraction liquid 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 containing sclareol being obtained by step (c) first filters through 120 order coarse filters, through 320 order accurate filters, filter again, by pump, pump into an effect 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 mixed solution is evaporated, mixed solution after evaporation enters the thin vaporizer of two effect adverse currents and the thin vaporizer of three-effect counter flow successively, evaporates respectively 60～80% solvent and 95～98% solvent.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, is preferably-0.04MPa;
Preferably, the vaporization temperature of the thin vaporizer of a described effect 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 obtaining after step (d) evaporation is pumped to reboiler and is heated to 90～95 ℃, then enter in vacuum distillation tower and distill, remaining solvent is thoroughly distilled and is removed, and enters solvent condenses system under suction function; Sclareol liquid after distillation and concentration after cooling forming, becomes solid sclareol again.The outward appearance of the solid sclareol obtaining is 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, pressure during distillation tower distillation is-0.03～-0.05MPa, is preferably-0.04MPa.
Wherein, the process of described step (f) negative pressure wet distillation precipitation is: the Salvia Sclare L. extracting after sclareol enters in the continuous wet distillation precipitation of vertical multi-layer tower through handling equipment, in precipitation tower, be provided with the pre-delamination of multilayer, adopt indirect steam heating, under stirring action, first remove 70% free solvent, then fall into two-layer air-permeable layer, continue to remove the solvent in Salvia Sclare L., then fall into wet distillation precipitation layer, pressure is that the saturated steam of 0.05MPa evenly sprays in Salvia Sclare L., regulate open steam pressure that the residual solvent of Salvia Sclare L. inner approximately 30% is distilled away, under suction function, enter condenser system with together with solvent gas that pre-delamination evaporates, the Salvia Sclare L. of desolvation enters 28～30 ℃ of cold wind pull-ups again except the moisture in Salvia Sclare L..Extract the Salvia Sclare L. slag residual solvent≤300ppm after sclareol, moisture≤20%, the effective constituent in Salvia Sclare L. residue can be protected in temperature≤40 ℃ of Salvia Sclare L. residue at this temperature, so that later use; The Salvia Sclare L. slag as fertilizer sources of desolvation returns to 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, is preferably-0.02MPa.
Wherein, the process of described step (g) solvent condenses separation is: from step (c) out enter leaching condenser containing solvent gas, the solvent vapo(u)r evaporating from step (d) enters vaporizer-condenser, the solvent vapo(u)r distilling from step (e) enters distiller condenser, the solvent vapo(u)r distilling from step (f) enters and steams de-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, normal hexane solvent floats over upper strata and flows into the recycle of solvent storehouse, isolated water enters wastewater boilling tank boiling.
Wherein, described step (h) waste water digestion process is: the isolated water of step (g) enters wastewater boilling tank boiling, and boiling temperature is 92～98 ℃, is preferably 95～98 ℃.Waste water after boiling, not containing solvent, has been realized zero pollution, zero release.
Preferably, described step (i) tail gas paraffin oil absorption process is: the solidifying gas that contains micro-normal hexane out from the last condenser of step (g), be imported into the paraffin oil packing material absorbing tower bottom of solubilized normal hexane, the low paraffin oil of temperature from top to bottom, the not solidifying gas that contains solvent from bottom to top, paraffin oil and solidifying gas abundant counter current contact in packed absorber, normal hexane in not solidifying gas is absorbed by paraffin oil, air is drawn and is discharged to outside workshop by induced draft fan, then paraffin oil enters filler Analytic Tower after being heated to 110～120 ℃, the normal hexane gas parsing enters condenser system and is condensed into liquid recycling, the paraffin oil of having resolved normal hexane is cooled to after 30～35 ℃, then enters absorption tower absorption normal hexane gas.Paraffin oil absorbs, resolves to a working cycle.
The invention has the beneficial effects as follows:
1, extraction yield is high: the synergistic effect of the negative pressure wet distillation that adopts and industrial normal hexane solvent multi-stage countercurrent pulse extraction technique, make Salvia Sclare L. essential oil and sclareol its extraction yield when not adopting molecular distillation technique can reach more than 95%, when especially in Salvia Sclare L., sclareol content is low to moderate 0.5%, present method still can be extracted, and to make sclareol content in Salvia Sclare L. slag be only 0.05%;
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 putting into production significantly reduces, therefore evaporate the required energy and significantly reduce; The boiling point of extraction solvent industry normal hexane is lower than above-mentioned patent solvent sherwood oil, and during solvent evaporative phase-change, the required energy is few;
3, good product quality: adopt negative pressure wet distillation to extract the sclareol purity of extracting after Salvia Sclare L. essential oil high, of light color, outward appearance olive-green solid, has grane ambra fragrance, fusing point: 50～60 ℃, residual solvent≤100ppm;
4, zero pollution, zero release: after solvent condenses, isolated waste water is not direct discharge, but increases by one cooking process, and waste water is heated to 92～98 ℃, reclaim a small amount of solvent evaporative condenser dissolving in waste water, do not contain solvent in the waste water of final discharge; Adopt paraffin oil solvent recovery technology from vent gas, in the tail gas of final discharge, do not contain solvent; Adopt negative pressure wet distillation precipitation technology, make Salvia Sclare L. flower slag return to farmland as good organic fertilizer, there is no waste.
5, output is high: former intermittent type, pot group type are produced and can only be processed 30～50 tons of Salvia Sclare L. every day, and technique 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 when not adopting molecular distillation technique, its yield can reach 95%, solved in sclareol suitability for industrialized production solvent input amount large, extract the low difficult problem of yield; There is no environmental pollution, production cost is low, and realized mass-producing, industrialization, the serialization of Salvia Sclare L. essential oil and sclareol and produced, be the innovative technology that Salvia Sclare L. extracts Salvia Sclare L. essential oil and sclareol, economic benefit and social benefit are huge.
Accompanying drawing explanation
Fig. 1 is 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, described embodiment helps to understand the present invention, should not be considered as concrete restriction of the present invention.
Embodiment 1
(a) Salvia Sclare L. crushing process is: Salvia Sclare L. raw material is ground into 20mm with pulverizer long;
(b) negative pressure wet distillation Salvia Sclare L. essential oil: the Salvia Sclare L. raw material after pulverizing is transported in wet distillation tower through material envelope transfer roller, in tower, pass into the direct saturated steam of 0.05Mpa, Salvia Sclare L. essential oil in Salvia Sclare L. is become gaseous state by wet distillation, enter again condenser condenses, after condensation, enter diversion box, Salvia Sclare L. essential oil obtain Salvia Sclare L. essential oil separated with water; Wherein Rectification column pressure is-0.04M;
(c) multi-stage countercurrent pulse extraction: the Salvia Sclare L. material after extraction essential oil is by expecting that sealing transfer roller is transported in extractor, at 55 ℃, first by the extraction solvent spray that is 1.2% containing sclareol mass concentration, soak extraction, drain, and then respectively through containing 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, iterative cycles extraction 180min, with normal hexane solvent spray, soak extraction again, realize multi-stage countercurrent pulse extraction;
(d) negative pressure adverse current thin film evaporation: the solution containing sclareol being obtained by step (c) first filters through 120 order coarse filters, through 320 order accurate filters, filter again, by pump, pump into an effect 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 mixed solution is evaporated, mixed solution after evaporation enters the thin vaporizer of two effect adverse currents and the thin vaporizer of three-effect counter flow successively, evaporates respectively 60% solvent and 98% solvent; Be-the 0.05MPa of evaporating pressure of the thin vaporizer of described adverse current; The vaporization temperature of the thin vaporizer of a described effect 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 obtaining after step (d) evaporation is pumped to reboiler and is heated to 90 ℃, then enter in vacuum distillation tower and distill, remaining solvent is thoroughly distilled and is removed, and enters solvent condenses system under suction function; Sclareol liquid after distillation and concentration after cooling forming, becomes solid sclareol again; The distillation tower column plate that is of five storeys; Pressure during distillation tower distillation is-0.04MPa;
(f) negative pressure wet distillation precipitation: the Salvia Sclare L. extracting after sclareol enters in the continuous wet distillation precipitation of vertical multi-layer tower through handling equipment, in precipitation tower, be provided with the pre-delamination of multilayer, adopt indirect steam heating, under stirring action, first remove 70% free solvent, then fall into two-layer air-permeable layer, continue to remove the solvent in Salvia Sclare L., then fall into wet distillation precipitation layer, pressure is that the saturated steam of 0.05MPa evenly sprays in Salvia Sclare L., regulate open steam pressure that the residual solvent of Salvia Sclare L. inner approximately 30% is distilled away, under suction function, enter condenser system with together with solvent gas that pre-delamination evaporates, the Salvia Sclare L. of desolvation enters 28 ℃ of cold wind pull-ups again except the moisture in Salvia Sclare L., described wet distillation precipitation pressure tower is-0.02MPa,
(g) solvent condenses is separated: from step (c) out containing solvent gas, enter leaching condenser, the solvent vapo(u)r evaporating from step (d) enters vaporizer-condenser, the solvent vapo(u)r distilling from step (e) enters distiller condenser, the solvent vapo(u)r distilling from step (f) enters and steams de-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, normal hexane solvent floats over upper strata and flows into the recycle of solvent storehouse, isolated water enters wastewater boilling tank boiling,
(h) waste water boiling: the isolated water of step (g) enters wastewater boilling tank boiling, and boiling temperature is 92～98 ℃.
(i) tail gas paraffin oil absorbs: the solidifying gas that contains micro-normal hexane out from the last condenser of step (g), be imported into the paraffin oil packing material absorbing tower bottom of solubilized normal hexane, paraffin oil and solidifying gas abundant counter current contact in packed absorber, then paraffin oil enters filler Analytic Tower after being heated to 120 ℃, and the normal hexane gas parsing enters condenser system and is condensed into liquid recycling; The paraffin oil of having resolved normal hexane is cooled to after 35 ℃, then enters absorption tower absorption normal hexane gas.
The extraction yield of the present embodiment Salvia Sclare L. essential oil is 98%, obtains the sclareol of olive-green solid, has grane ambra fragrance, fusing point: 50～60 ℃, and sclareol content 66%, residual solvent 70ppm.
Embodiment 2
(a) Salvia Sclare L. crushing process is: Salvia Sclare L. raw material is ground into 50mm with pulverizer long;
(b) negative pressure wet distillation Salvia Sclare L. essential oil: the Salvia Sclare L. raw material after pulverizing is transported in wet distillation tower through material envelope transfer roller, in tower, pass into the direct saturated steam of 0.05Mpa, Salvia Sclare L. essential oil in Salvia Sclare L. is become gaseous state by wet distillation, enter again condenser condenses, after condensation, enter diversion box, Salvia Sclare L. essential oil obtain Salvia Sclare L. essential oil separated with water; Wherein Rectification column pressure is-0.03M;
(c) multi-stage countercurrent pulse extraction: the Salvia Sclare L. material after extraction essential oil is by expecting that sealing transfer roller is transported in extractor, at 50 ℃, first by the extraction solvent spray that is 1.5% containing sclareol mass concentration, soak extraction, drain, and then respectively through containing 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, iterative cycles extraction 120min, with normal hexane solvent spray, soak extraction again, realize multi-stage countercurrent pulse extraction;
(d) negative pressure adverse current thin film evaporation: the solution containing sclareol being obtained by step (c) first filters through 120 order coarse filters, through 320 order accurate filters, filter again, by pump, pump into an effect 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 mixed solution is evaporated, mixed solution after evaporation enters the thin vaporizer of two effect adverse currents and the thin vaporizer of three-effect counter flow successively, evaporates respectively 80% solvent and 95% solvent; Be-the 0.03MPa of evaporating pressure of the thin vaporizer of described adverse current; The vaporization temperature of the thin vaporizer of a described effect 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 obtaining after step (d) evaporation is pumped to reboiler and is heated to 95 ℃, then enter in vacuum distillation tower and distill, remaining solvent is thoroughly distilled and is removed, and enters solvent condenses system under suction function; Sclareol liquid after distillation and concentration after cooling forming, becomes solid sclareol again; The distillation tower column plate that haves three layers; Pressure during distillation tower distillation is-0.05MPa.
The extraction yield of the present embodiment Salvia Sclare L. essential oil is 95%, obtains the sclareol of olive-green solid, 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 above-described embodiment, but the present invention is not limited to above-mentioned detailed process flow, does not mean that the present invention must rely on above-mentioned detailed process flow and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to the selection of the interpolation of the equivalence replacement of each raw material of product of the present invention and ancillary component, concrete mode etc., within all dropping on protection scope of the present invention and open scope.
Claims (23)
1. the production method of simultaneous extraction Salvia Sclare L. essential oil and sclareol from a Salvia Sclare L., it is characterized in that, production technique comprises: (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 step (c) is normal hexane, the mass ratio of extraction solvent and Salvia Sclare L. is: 0.5～1.5:1, the process of described step (c) multi-stage countercurrent pulse extraction is: the Salvia Sclare L. material after extraction essential oil is by expecting that sealing transfer roller is transported in extractor, at 50-55 ℃, first by the extraction solvent spray that is 1.2%～1.5% containing sclareol mass concentration, soak extraction, drain, and then through containing sclareol mass concentration, be 1.0～1.1% respectively, 0.8～0.9%, 0.6～0.7%, 0.4～0.5%, 0.2～0.3%, 0.05～0.15% extraction solvent successively seven grades of sprays soaks extraction, drain, iterative cycles extraction 120～180min, with normal hexane solvent spray, soak extraction again, realize multi-stage countercurrent pulse extraction.
2. the method for claim 1, is characterized in that, the mass ratio of extraction solvent and Salvia Sclare L. is 1:1.
3. the method for claim 1, is characterized in that, also carries out following technique after vacuum distillation is concentrated: (f) negative pressure wet distillation precipitation, and (g) solvent condenses is separated, (h) waste water boiling, (i) tail gas paraffin oil absorbs.
4. the method as described in claim 1-3 any one, is characterized in that, described step (a) Salvia Sclare L. crushing process is: Salvia Sclare L. raw material is ground into 20～50mm with pulverizer long.
5. the method as described in claim 1-3 any one, it is characterized in that, described step (b) negative pressure wet distillation essential oil process is: the Salvia Sclare L. raw material after pulverizing is transported in wet distillation tower through material envelope transfer roller, in tower, pass into the direct saturated steam of 0.05Mpa, Salvia Sclare L. essential oil in Salvia Sclare L. is become gaseous state by wet distillation, enter again condenser condenses, after condensation, enter diversion box, Salvia Sclare L. essential oil obtain Salvia Sclare L. essential oil separated with water.
6. method as claimed in claim 5, is characterized in that, described distillation tower pressure is-0.03～-0.05MPa.
7. method as claimed in claim 6, is characterized in that, described distillation tower pressure is-0.04MPa.
8. the method for claim 1, is characterized in that, the mass concentration that seven grades of described sprays soak extraction liquid is 1.2%, 1.0%, 0.8%, 0.6%, 0.4%, 0.2%, 0.1%.
9. the method as described in claim 1-3 any one, it is characterized in that, described step (d) negative pressure adverse current thin film evaporation process is: the solution containing sclareol being obtained by step (c) first filters through 120 order coarse filters, through 320 order accurate filters, filter again, by pump, pump into an effect 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 mixed solution is evaporated, mixed solution after evaporation enters two effect adverse current thin-film evaporators and three-effect counter flow thin-film evaporator successively, evaporate respectively 60～80% solvent and 95～98% solvent.
10. method as claimed in claim 9, is characterized in that, the evaporating pressure of described adverse current thin-film evaporator is-0.03～-0.05MPa.
11. methods as claimed in claim 10, is characterized in that, be-0.04MPa of the evaporating pressure of described adverse current thin-film evaporator.
12. methods as claimed in claim 9, is characterized in that, the vaporization temperature of a described effect adverse current thin-film evaporator is 55～60 ℃, 65～70 ℃ of the vaporization temperatures of two effect adverse current thin-film evaporators, and the vaporization temperature of three-effect counter flow thin-film evaporator is 80～85 ℃.
13. methods as described in claim 1-3 any one, it is characterized in that, the concentrated process of described step (e) vacuum distillation is: the sclareol solution obtaining after step (d) evaporation is pumped to reboiler and is heated to 90～95 ℃, then enter in vacuum distillation tower and distill, remaining solvent is thoroughly distilled and is removed, and enters solvent condenses system under suction function; Sclareol liquid after distillation and concentration after cooling forming, becomes solid sclareol again.
14. methods as claimed in claim 13, is characterized in that, distillation tower has 3～5 layers of column plate.
15. methods as claimed in claim 13, is characterized in that, pressure during distillation tower distillation is-0.03～-0.05MPa.
16. methods as claimed in claim 15, is characterized in that, pressure during distillation tower distillation is-0.04MPa.
17. methods as claimed in claim 3, it is characterized in that, the process of described step (f) negative pressure wet distillation precipitation is: the Salvia Sclare L. extracting after sclareol enters in the continuous wet distillation precipitation of vertical multi-layer tower through handling equipment, in precipitation tower, be provided with the pre-delamination of multilayer, adopt indirect steam heating, under stirring action, first remove 70% free solvent, then fall into two-layer air-permeable layer, continue to remove the solvent in Salvia Sclare L., then fall into wet distillation precipitation layer, pressure is that the saturated steam of 0.05MPa evenly sprays in Salvia Sclare L., regulate open steam pressure that the residual solvent of Salvia Sclare L. inner approximately 30% is distilled away, under suction function, enter condenser system with together with solvent gas that pre-delamination evaporates, the Salvia Sclare L. of desolvation enters 28～30 ℃ of cold wind pull-ups again except the moisture in Salvia Sclare L..
18. methods as claimed in claim 17, is characterized in that, described wet distillation precipitation pressure tower is-0.01～-0.03MPa.
19. methods as claimed in claim 18, is characterized in that, described wet distillation precipitation pressure tower is-0.02MPa.
20. methods as claimed in claim 3, it is characterized in that, the process of described step (g) solvent condenses separation is: from step (c) out enter leaching condenser containing solvent gas, the solvent vapo(u)r evaporating from step (d) enters vaporizer-condenser, the solvent vapo(u)r distilling from step (e) enters distiller condenser, the solvent vapo(u)r distilling from step (f) enters and steams de-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, normal hexane solvent floats over upper strata and flows into the recycle of solvent storehouse, isolated water enters wastewater boilling tank boiling.
21. methods as claimed in claim 3, is characterized in that, described step (h) waste water digestion process is: the isolated water of step (g) enters wastewater boilling tank boiling, and boiling temperature is 92～98 ℃.
22. methods as claimed in claim 21, is characterized in that, described boiling temperature is 95～98 ℃.
23. methods as claimed in claim 3, it is characterized in that, described step (i) tail gas paraffin oil absorption process is: the solidifying gas that contains micro-normal hexane out from the last condenser of step (g), be imported into the paraffin oil packing material absorbing tower bottom of solubilized normal hexane, paraffin oil and solidifying gas abundant counter current contact in packed absorber, then paraffin oil enters filler Analytic Tower after being heated to 110～120 ℃, and the normal hexane gas parsing enters condenser system and is condensed into liquid recycling; The paraffin oil of having resolved normal hexane is cooled to after 30～35 ℃, then enters absorption tower absorption normal hexane gas.
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| CN105154236B (en) * | 2015-09-23 | 2018-08-14 | 陈富强 | Full-automatic electric heating triple effect plants essential oil extraction purification integrated apparatus |
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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 |
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