CN102260314A - Betulin extraction method and device thereof - Google Patents
Betulin extraction method and device thereof Download PDFInfo
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- CN102260314A CN102260314A CN 201010181937 CN201010181937A CN102260314A CN 102260314 A CN102260314 A CN 102260314A CN 201010181937 CN201010181937 CN 201010181937 CN 201010181937 A CN201010181937 A CN 201010181937A CN 102260314 A CN102260314 A CN 102260314A
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Abstract
The invention discloses a betulin extraction method and a device thereof. The betulin extraction device comprises a condenser, an extractor, a distillation separator, a heating device and a separator plate with small holes; according to the betulin extraction method, the betulin extraction device is utilized to extract betulin and simultaneously carry out the betulin purification by using birch bark as a raw material and an ethanol-water mixed steam condensate liquid as a solvent. The extraction method provided by the invention has advantages of simple operation, low extraction cost, high extraction rate and high purity of the extracted betulin.
Description
Technical field
The present invention relates to the extraction of Cortex Betulae Luminiferae effective constituent, relates in particular to a kind of extracting method and equipment of betulin.
Background technology
Betulin (Betulin) (different name birch camphor, trochol) is a needle crystal, belongs to pentacyclic triterpenoid, is dissolved in ethanol, ether, chloroform and benzene, is slightly soluble in water, sherwood oil etc.Molecular formula: C
30H
50O
2, molecular weight 442.70, molecular structural formula:
Betulin derives from the root of feverfew Saussurea lappa Clarke (Salgssurea lappa Clarke), the bark of Betulaceae plant white birch (Betula platyphylla Suk.) etc.Betulin tool edge anti-tumor activity, its derivative betulinic acid are the remarkable anti-HIV of a kind of nontoxic substantially tool～1 and the active compound of melanoma, have a extensive future.
Publication number is that the application for a patent for invention of CN 1634972A discloses a kind of trochol and Betulinic acid extracting and purifying method, the betulin extracting and purifying method of this patent of invention adopts following steps: the Japanese birch bark after (1) will pulverize adds organic reagent and stirs extraction for several times, united extraction liquid removes residue.(2) concentrating under reduced pressure extracting solution is placed after-filtration, and with extracting the solvent washing precipitation, collecting precipitation removes filtrate.(3) precipitation is dissolved in the methyl alcohol, adds the gac refluxing extraction, filter.(4) collect filtrate, reclaim under reduced pressure methyl alcohol is collected filter residue, adds the methylene dichloride dissolving, adds pyridine and acetic anhydride again, stirs some hrs.(5) add diluted acid, bicarbonate aqueous solution, the Powdered insolubles in upper strata is collected in the pure water washing.(6) powder is dissolved in ethanol or methyl alcohol or the Virahol places, separate out the crystal after-filtration, washing, dry gained betulin crystal.
The extracting and purifying method of above-mentioned betulin is multiple extraction with process, complicated operation, and the cost height, yield is low.
In the chemical production field, sieve-tray tower is a kind of of Zha Banta, and the horizontal column plate of interior dress several layers has many apertures on the plate, and shape is as sieve; And upflow tube is housed or does not have upflow tube.During operation, liquid is entered by cat head, descends, and accumulates liquid layer onboard through upflow tube (part is through sieve aperture) step by step tray.Gas (or steam) is by entering at the bottom of the tower, and rise through sieve aperture and pass liquid layer, bubbling and going out, thereby two-phase can fully contact, and interact.In still-process, when dirty, just the phenomenon of leakage can appear through the duct when the kinetic energy of ascending gas is not enough to stop liquid.The flow velocity of control ascending gas is the major measure of control leakage.At present, sieve-tray tower is generally in distillation, absorption and dedusting etc.
The patent No. is that the utility model patent of ZL 96248019.3 discloses a kind of mining sieve-tray tower leaching reactor that soaks, form by cylindrical shell, lower cover, opening for feed, washing drain hole, inlet mouth, discharge port, upper cover, air outlet, the sieve plate that a gas distribution grid that has aperture with the reactor shell axis normal constitutes particularly is housed in the cylindrical shell of reactor.Wherein, the percentage of open area of gas distribution grid is 0.005%～8%, and hole diameter is 0.5 * 10
～3～8 * 10
～3Rice.This sieve plate leaches tower and compares with traditional leaching plant, and leaching rate is fast, and the cycle is short, and is simple in structure.
Summary of the invention
The object of the present invention is to provide a kind of production cost low, extract simple to operate, extraction yield height, the betulin extracting method that product purity is higher.
For realizing purpose of the present invention, one aspect of the present invention provides a kind of extraction equipment of betulin, comprises condenser, extractor, dividing plate, fractionation by distillation device that is linked in sequence from top to bottom and the heating unit that heat energy is provided for the fractionation by distillation device.
Wherein, the top of extractor is provided with opening for feed, and the bottom is provided with discharge port, and the top is provided with the vapor condensation interface, and the bottom is provided with extracting liquid outlet;
The top of fractionation by distillation device is provided with fluid inlet, and the bottom is provided with material liquid outlet, and the top is provided with vapour outlet;
Offer on the dividing plate for steam and the freely through hole of extracting solution, dividing plate is fixed together extractor, dividing plate and fractionation by distillation device by flange between extractor and fractionation by distillation device;
Condenser is fixed on the top of extractor by the vapor condensation interface at extractor top;
Heating unit is for the fractionation by distillation device provides heat energy.
Particularly, the heat-eliminating medium of described condenser is a water, and other solid, gas, liquid with cooling effect also is applicable to the present invention.
Particularly, described condenser is selected prolong.
Especially, described prolong is shaped as a kind of in straight shape, sphere, the snakelike or thorn shape.
Wherein, the opening for feed on extractor top is used to add raw material to be extracted, for example the Cortex Betulae Luminiferae powder; The discharge port of bottom is used to discharge the residue that soaks the raw material after extracting; The vapor condensation interface at top provides steam freely to enter condenser and provides from condenser condensed phlegma freely to be back to passage in the extractor; The extracting liquid outlet of bottom freely passes through for the steam and the interior extracting solution of extractor that come from the fractionation by distillation device.
Particularly, described extractor is spheric glass extractor or columniform stainless steel extractor.
Especially, the opening for feed of described extractor and discharge port remove and open when charging or discharging, and other times are closed state.
Wherein, the fluid inlet on fractionation by distillation device top is used for adding the extraction solvent to the fractionation by distillation device; The material liquid outlet of bottom is used to discharge solution and extract in the fractionation by distillation device; The vapour outlet at top freely passes through for steam that produces in the fractionation by distillation device and the extracting solution in the extractor.
Particularly, the internal diameter of the vapour outlet of fractionation by distillation device is 10～120 millimeters; Be preferably 50～60 millimeters.
Wherein, the vapour outlet of described fractionation by distillation device is identical with the internal diameter of extractor bottoms extracting liquid outlet, with the ratio of extractor internal diameter be 0.1～0.3: 1.
Especially, the fluid inlet of described fractionation by distillation device and products export are except that adding solvent or discharging the solution, and other times are closed state.
Wherein, the internal diameter in the space on the described dividing plate is 0.5～1.5 millimeter, is preferably 0.8～1.2 millimeter.
Particularly, the cross-sectional area sum of described the above hole of dividing plate is 0.09～0.2: 1 with the ratio of the cross-sectional area of the vapour outlet of fractionation by distillation device, is preferably 0.1～0.15: 1.
Wherein, described heating unit is arranged on the bottom of fractionation by distillation device or is wrapped in the outside of fractionation by distillation device, and wherein the power of heating unit can be regulated according to the heating needs.
The present invention provides a kind of method of extracting betulin on the other hand, comprises adopting the mixing steam phlegma of second alcohol and water that Cortex Betulae Luminiferae is carried out lixiviate.
Wherein, the mixing steam of described second alcohol and water is by being that 1～3: 1 the dehydrated alcohol and the mixed solution of water heat with volume ratio, the mixing steam that the boiling back produces.
Wherein, extraction time is 0.5～6 hour, is preferably 2～4 hours.
Further aspect of the present invention provides a kind of method of utilizing said extracted equipment to extract betulin, comprises following step in sequence:
1) the Cortex Betulae Luminiferae powder of pulverizing is placed on the bottom of extractor and the top of dividing plate;
2) mixing solutions with the second alcohol and water places the fractionation by distillation device;
3) open heating unit and condenser, heating unit heats the fractionation by distillation device, makes the mixed solution boiling of second alcohol and water in the fractionation by distillation device, produces ethanol～water mixing steam;
4) ethanol～water mixing steam flows in the extractor after formation ethanol～water-cooled lime set successively by condensation under the effect of condenser behind dividing plate, the extractor, soaks and also extracts Cortex Betulae Luminiferae;
5) regulate the heating power of heating unit, the Cortex Betulae Luminiferae powder in the extractor is immersed in ethanol～water-cooled lime set all the time, the hole of a part of ethanol～water-cooled lime set by dividing plate in the extractor is back in the fractionation by distillation device;
6) soak extraction after 0.5～6 hour, stop heating, ethanol in the fractionation by distillation device～water extraction mixture is filtered in cooling, promptly gets betulin.
Wherein, water content＜20% at the powder of Cortex Betulae Luminiferae described in the step 1) is preferably 5～15%; Granularity is 1～20 order, is preferably 8～16 orders; Dehydrated alcohol is 1～3: 1 with the ratio of the volume of water in the mixing solutions of the alcohol and water of second step 2).
Particularly, step 2) consumption of the mixing solutions of second alcohol and water is 10～30 a milliliters/gram Cortex Betulae Luminiferae powder in, is preferably 20～30 milliliters/gram Cortex Betulae Luminiferae powder.
Wherein, the Cortex Betulae Luminiferae powder in the extractor is immersed in ethanol～water-cooled lime set all the time, the liquid level of wherein said ethanol～water-cooled lime set is higher than 10～50 millimeters in Cortex Betulae Luminiferae powder; Soaking extraction time described in the step 6) is preferably 2～4 hours.
Particularly, also comprise filtering obtaining filter residue, carry out vacuum-drying after the washing, obtain the betulin crude product.
Further aspect of the present invention provides a kind of betulin that is prepared from according to the method described above.
Advantage of the present invention is:
1, betulin of the present invention extract equipment with solid materials and solvent respectively in extractor and the fractionation by distillation device, separate with dividing plate between extractor and the fractionation by distillation device, by the perforate number of selecting dividing plate and the Heating temperature of controlling the fractionation by distillation device, when solvent vapo(u)r and cooling fluid thereof are extracted solid materials, constantly there is extracting solution to flow back in the fractionation by distillation device, and constantly there is solvent vapo(u)r to produce, thereby can reaches continuous extraction solid materials; In addition, adopt dividing plate that raw material Cortex Betulae Luminiferae to be extracted and extraction solvent are separated, overcome conventional thermal backflow and extracted back betulin and the isolating technical problem of raw material Cortex Betulae Luminiferae.
2, the present invention adopts cheap and nontoxic substantially organic solvent in the leaching process of betulin, utilize betulin to be soluble in the ethanol of heat, and under the room temperature in ethanol-water solution the significantly reduced characteristic of solubleness, the extraction and the separation and purification of betulin are carried out simultaneously, simple to operate.
3, be that raw material extracts betulin with the Cortex Betulae Luminiferae, raw material is that birch is felled and industrial wood waste, and the source is abundant, and is cheap and easy to get, can effectively improve the utilising efficiency of biomass resource.
The steam that has produced when 4, having made full use of heated solvent in the leaching process of the present invention has increased the less turbulence of liquid phase, has improved the rate of diffusion of solute, and extraction rate is accelerated, and extraction time is short, extraction efficiency and betulin extract yield height.
5, constantly having fresh solvent (phlegma) to add in the leaching process of the present invention, is to keep higher concentration gradient between solute and solvent, has obviously improved alternate mass transfer force; Because constantly the steam that rises and the phlegma of backflow meet in extractor, make the phlegma heating of backflow, leaching process is carried out in thermal environment, extraction rate is fast, has shortened extraction time, has improved extraction efficiency.
6, utilize the content of the betulin of betulin extraction equipment extraction of the present invention to reach more than 90%.
Description of drawings
Fig. 1 is the structural representation of the continuous extraction equipment of betulin of the present invention.
Fig. 2 is the front view of dividing plate of the present invention.
Description of reference numerals
1. condenser; 2. extractor; 21. vapor condensation interface; 22. extracting liquid outlet; 23. opening for feed; 24. discharge port; 3. dividing plate; 31. hole; 4. fractionation by distillation device; 41. fluid inlet; 42. material liquid outlet; 43. vapour outlet; 5. heating unit; 6. flange
The specific embodiment mode
As shown in Figure 1, betulin of the present invention extracts equipment by forming according to the condenser 1 that is linked in sequence from top to bottom, extractor 2, dividing plate 3, fractionation by distillation device 4 and heating unit 5.
Fixedlying connected with the vapor condensation interface 21 at extractor 2 tops in the bottom of condenser 1, is positioned at the top of extractor 2; Under the condenser effect, be back in the extractor 2 behind the vapor condensation of heat.
The top of extractor 2 is provided with opening for feed 23, is used to add the Cortex Betulae Luminiferae powder; The bottom is provided with discharge port 24, is used to discharge the Cortex Betulae Luminiferae powder residue of soaking after extracting; The top is provided with vapor condensation interface 21, provides steam freely to enter condenser 1 and provides from condenser 1 condensed phlegma freely to be back to passage in the extractor 2; The bottom is provided with extracting liquid outlet 22, freely passes through for the steam and the extractor 2 interior extracting solutions that come from the fractionation by distillation device 4.
The top of fractionation by distillation device 4 is provided with fluid inlet 41, is used for adding the extraction solvent to fractionation by distillation device 4; The bottom is provided with material liquid outlet 42, is used to discharge the extraction mixture in the fractionation by distillation device 4; The top is provided with vapour outlet 43, freely passes through for the extracting solution in steam that produces in the fractionation by distillation device 4 and the extractor 2.
The vapour outlet 43 of fractionation by distillation device 4 is identical with the internal diameter of extractor 2 bottom extracting liquid outlets 22, with the ratio of extractor 2 internal diameters be 0.1～0.3: 1.The internal diameter of the vapour outlet 43 of fractionation by distillation device 4 is 10～120 millimeters; Be preferably 50～60 millimeters.
Dividing plate 3 is fixed on by flange in the middle of the vapour outlet 43 of the extracting liquid outlet 22 of extractor 2 and fractionation by distillation device 4, offers a plurality ofly for steam and the freely through holes 31 of extracting solution on it, and hole 31 be a circle; The cross-sectional area sum of dividing plate 3 the above hole 31 is 0.09～0.2: 1 with the ratio of the cross-sectional area of the vapour outlet 43 of fractionation by distillation device 4, is preferably 0.1～0.15: 1; The internal diameter in space 31 is 0.5～1.5 millimeter, is preferably 0.8～1.2 millimeter, as shown in Figure 2.
The above hole 31 of dividing plate of the present invention 3 is except being the circle, can also be square, trilateral, rhombus, abnormity etc.; Condenser 1 is selected spherical condensation tube, and other condensers all are applicable to the present invention; Extractor 2, fractionation by distillation device 4 are globe; Heating unit is selected heating jacket, and maximum heating power is 2.0 kilowatts; The power of the shape of extractor, fractionation by distillation device and size, heating jacket is selected according to actual needs.
Below in conjunction with specific embodiment, further set forth the present invention.Be not used in but these embodiment only limit to the present invention is described and limit the scope of the invention.
In the extraction equipment of the betulin of present embodiment, the internal diameter of the vapour outlet 43 of fractionation by distillation device 4 is 50 millimeters, and extractor 2 internal diameters are 350 millimeters, and the internal diameter of the hole of being opened on the dividing plate 3 is 0.5 millimeter; The cross-sectional area sum of dividing plate 3 the above hole 31 is 0.15: 1 with the ratio of the cross-sectional area of the vapour outlet 43 of fractionation by distillation device 4.
1, preparation Cortex Betulae Luminiferae powder
With Cortex Betulae Luminiferae 80 ℃ dry to water content be 15%, pulverize, making granularity is 12～16 purpose Cortex Betulae Luminiferae powder.
2, extract, separate
1) 300 gram Cortex Betulae Luminiferae powder is placed the bottom of extractor 2 and the top of dividing plate 3 by the opening for feed 23 of extractor 2;
2) be that 6000 milliliters of the mixed solutions of 2: 1 dehydrated alcohols and water place fractionation by distillation device 4 by the fluid inlet in the fractionation by distillation device 4 41 with volume ratio, wherein, the consumption of the mixed solution of ethanol and water is 20 a milliliters/gram Cortex Betulae Luminiferae powder;
3) open cold condenser 1 and heating unit 5 (heating jacket), heating jacket heats fractionation by distillation device 4, makes the boiling of ethanol and water mixed solution, produces ethanol～water mixing steam;
4) ethanol～water mixing steam enters extractor 2 by the hole on the dividing plate 3 31, pass the Cortex Betulae Luminiferae powder, hot steam heats material, continue to rise to spherical condensation tube (being condenser 1), ethanol～water mixing steam is condensed into ethanol～water-cooled lime set, phlegma is back in the extractor 2, the Cortex Betulae Luminiferae powder is soaked extraction, because constantly ethanol～water the mixing steam that rises and the ethanol～water-cooled lime set of backflow are met in extractor 2, make the phlegma heating of backflow, make to soak to be extracted in the thermal environment system and carry out, be beneficial to the leaching of betulin in the Cortex Betulae Luminiferae powder;
In order to make the betulin in the Cortex Betulae Luminiferae fully be dissolved in the solvent, by adjustment to the solvent Heating temperature, the lift velocity of control solvent vapo(u)r, make and produce the liquid flooding phenomenon in the extractor 2, increased solvent to the interaction force between the Cortex Betulae Luminiferae powder, solubility rate is further improved, make dissolution rate accelerate, reach the purpose that cuts down the consumption of energy, improves yield.
5) solvent in extractor 2 increases gradually, when the liquid level that extracts solvent reach a certain height, it is big that extracting solution liquid layer resistance becomes, when the steam flow rate by dividing plate 3 is not enough to overcome extracting solution liquid layer resistance, extracting section liquid can flow back in the fractionation by distillation device 4 by the hole on the dividing plate 3 31, by regulating the heating power of heating jacket 5, the flow velocity of control ethanol～water azeotropic steam, make the extracting solution submergence Japanese birch bark in the extractor 2, simultaneously constantly there is extracting solution to flow back in the fractionation by distillation device 4, control flows into the amount and the amount phase equilibrium that flow back into the ethanol～water azeotropic phlegma in the fractionation by distillation device 4 from extractor 2 of the ethanol～water azeotropic phlegma in the extractor 2 after making 1 condensation, and makes the extracting solution liquid level in the extractor 2 be higher than 10～30 millimeters in Cortex Betulae Luminiferae powder
6) soak extraction after 2 hours, stop heating, extracting solution in the extractor 2 flows in the fractionation by distillation device 4 from extracting liquid outlet 22, and the extraction mixture in the separator 4 to be distilled is cooled to room temperature (25 ℃), and betulin is separated out precipitation in the extraction mixture, filter, filter residue carries out vacuum-drying after washing 2 times, obtains betulin 98.4 grams, through efficient liquid phase chromatographic analysis, the content of betulin is 91.5%, and the extract yield of betulin is 30.01%.
Cortex Betulae Luminiferae powder residue in the extractor 2 is discharged from the discharge port 24 of extractor 2.
The internal diameter of vapour outlet 43 that extracts the fractionation by distillation device 4 of equipment except betulin is 55 millimeters, and extractor 2 internal diameters are 550 millimeters.The internal diameter of the hole of being opened on the dividing plate 3 is 0.8 millimeter; The cross-sectional area sum of dividing plate 3 the above hole 31 is 0.1: 1 with the ratio of the cross-sectional area of the vapour outlet 43 of fractionation by distillation device 4;
The water ratio of Cortex Betulae Luminiferae powder is 10% in the preparation Cortex Betulae Luminiferae powder process, and granularity is 8～12 orders;
The volume that adds the mixing solutions of the second alcohol and water in the fractionation by distillation device 4 in extraction, the sepn process is 9000 milliliters, wherein the ratio of the volume of dehydrated alcohol and water is 1: 1, make the extracting solution liquid level in the extractor 2 be higher than 10～20 millimeters in Cortex Betulae Luminiferae powder, soaking extraction time is outside 4 hours, and all the other are identical with embodiment 1.
Betulin 90.6 grams that make, through efficient liquid phase chromatographic analysis, the content of betulin is 90.1%, the extract yield of betulin is 27.21%.
The internal diameter of vapour outlet 43 that extracts the fractionation by distillation device 4 of equipment except betulin is 60 millimeters, and extractor 2 internal diameters are 200 millimeters.The internal diameter of the hole of being opened on the dividing plate 3 is 1.5 millimeters; The cross-sectional area sum of dividing plate 3 the above hole 31 is 0.2: 1 with the ratio of the cross-sectional area of the vapour outlet 43 of fractionation by distillation device 4;
The water ratio of Cortex Betulae Luminiferae powder is 12% in the preparation Cortex Betulae Luminiferae powder process, and granularity is 8～12 orders;
The volume that adds the mixing solutions of the second alcohol and water in the fractionation by distillation device 4 in extraction, the sepn process is 7500ml, wherein the ratio of the volume of dehydrated alcohol and water is 3: 1, make the extracting solution liquid level in the extractor 2 be higher than 20～50 millimeters in Cortex Betulae Luminiferae powder, soaking extraction time is outside 0.5 hour, and all the other are identical with embodiment 1.
Betulin 81.3 grams that make, through efficient liquid phase chromatographic analysis, the content of betulin is 92.2%, the extract yield of betulin is 25.00%.
The internal diameter of vapour outlet 43 that extracts the fractionation by distillation device 4 of equipment except betulin is 60 millimeters, and extractor 2 internal diameters are 200 millimeters.The internal diameter of the hole of being opened on the dividing plate 3 is 1.2 millimeters; The cross-sectional area sum of dividing plate 3 the above hole 31 is 0.09: 1 with the ratio of the cross-sectional area of the vapour outlet 43 of fractionation by distillation device 4;
The water ratio of Cortex Betulae Luminiferae powder is 5% in the preparation Cortex Betulae Luminiferae powder process, and granularity is 1～20 order;
The volume that adds the mixing solutions of the second alcohol and water in the fractionation by distillation device 4 in extraction, the sepn process is 6000ml, and wherein the ratio of the volume of dehydrated alcohol and water is 3: 1, and soaking extraction time is outside 6 hours, and all the other are identical with embodiment 1.
Betulin 94.6 grams that make, through efficient liquid phase chromatographic analysis, the content of betulin is 94.2%, the extract yield of betulin is 29.7%.
Claims (10)
1. the extraction equipment of a betulin comprises condenser (1), extractor (2), dividing plate (3), fractionation by distillation device (4) that is linked in sequence from top to bottom and the heating unit (5) that heat energy is provided for fractionation by distillation device (4).
2. extraction equipment as claimed in claim 1 is characterized in that:
Extractor (2), its top are provided with opening for feed (23), and the bottom is provided with discharge port (24), and the top is provided with vapor condensation interface (21), and the bottom is provided with extracting liquid outlet (22);
Fractionation by distillation device (4), top are provided with fluid inlet (41), and the bottom is provided with material liquid outlet (42), and the top is provided with vapour outlet (43);
Dividing plate (3) is offered on it for steam and the freely through hole of extracting solution (31), is positioned between extractor (2) and the fractionation by distillation device (4), by flange (6) extractor (2), dividing plate (3) and fractionation by distillation device (4) is fixed together;
Condenser (1) is fixed on the top of extractor (2) by the vapor condensation interface (21) at extractor (2) top;
Heating unit (5) is for fractionation by distillation device (4) provides heat energy.
3. extraction equipment as claimed in claim 2 is characterized in that the ratio of cross-sectional area of the vapour outlet (43) of the cross-sectional area sum of the above hole of dividing plate (3) (31) and fractionation by distillation device (4) is 0.09～0.2: 1.
4. a method of extracting betulin comprises and adopts the mixing steam phlegma of second alcohol and water that Cortex Betulae Luminiferae is soaked extraction.
5. method as claimed in claim 4, it is characterized in that soaking extraction time is 0.5～6 hour.
6. method of utilizing the arbitrary described extraction equipment of claim 1～3 to extract betulin comprises following step in sequence:
1) the Cortex Betulae Luminiferae powder of pulverizing is placed on the inside of extractor (2) and the top of dividing plate (3);
2) mixing solutions with the second alcohol and water places fractionation by distillation device (4);
3) open heating unit (5) and condenser (1), heating unit (5) heats fractionation by distillation device (4), makes the mixed solution boiling of the interior second alcohol and water of fractionation by distillation device (4), produces ethanol～water mixing steam;
4) ethanol～water mixing steam by dividing plate (3), extractor (2) back condensation under the effect of condenser (1), flows in the extractor (2) after formation ethanol～water-cooled lime set successively, soaks and also extracts Cortex Betulae Luminiferae;
5) heating power of adjusting heating unit (5), Cortex Betulae Luminiferae powder in the extractor (2) is immersed in ethanol～water-cooled lime set all the time, the hole (31) of a part of ethanol～water-cooled lime set by dividing plate (3) in the extractor (2) is back in the fractionation by distillation device (4);
6) soak extraction after 0.5～6 hour, stop heating, the interior ethanol of fractionation by distillation device (4)～water mixing mixed extract is filtered in cooling, promptly gets betulin.
7. method as claimed in claim 6 is characterized in that step 2) described in the mixing solutions of second alcohol and water the ratio of dehydrated alcohol and the volume of water be 1～3: 1.
8. as claim 6 or 7 described methods, the granularity that it is characterized in that the powder of Cortex Betulae Luminiferae described in the step 1) is 1～20 order.
9. as claim 6 or 7 described methods, it is characterized in that step 2) in the consumption of mixing solutions of second alcohol and water be 15～30 milliliters/gram Cortex Betulae Luminiferae powder.
10. betulin is characterized in that being prepared from according to method as described in arbitrary as claim 4～9.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102553293A (en) * | 2012-01-20 | 2012-07-11 | 东北林业大学 | Device for extracting betulinol |
| EP2842564A1 (en) * | 2013-08-30 | 2015-03-04 | "Latvian State Institute of Wood Chemistry" Derived public person | Method for the chemical processing of outer birch bark and apparatus for its realisation |
| CN105115848A (en) * | 2015-07-20 | 2015-12-02 | 山东科技大学 | Reflux type oil sand oil content and moisture synchronous determination system and determination method |
| CN105617710A (en) * | 2016-01-27 | 2016-06-01 | 福建师范大学 | Circular extraction device and method |
| CN106422406A (en) * | 2016-11-15 | 2017-02-22 | 营口天元化工研究所股份有限公司 | Normal-pressure fast purification device of organic solids and application thereof |
| CN114733222A (en) * | 2022-04-19 | 2022-07-12 | 华一鸣 | Ceramic pigment water-soluble substance filter equipment |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1094987A (en) * | 1993-05-14 | 1994-11-16 | 中南民族学院 | A kind of method that is used for the solid thermal extraction |
| CN2880210Y (en) * | 2006-02-07 | 2007-03-21 | 内蒙古师范大学 | Heating extracting device of plant useful component |
| CN101200486A (en) * | 2006-12-13 | 2008-06-18 | 上海睿智化学研究有限公司 | Method for abstracting and purifying betulin in birch bark |
-
2010
- 2010-05-25 CN CN 201010181937 patent/CN102260314A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1094987A (en) * | 1993-05-14 | 1994-11-16 | 中南民族学院 | A kind of method that is used for the solid thermal extraction |
| CN2880210Y (en) * | 2006-02-07 | 2007-03-21 | 内蒙古师范大学 | Heating extracting device of plant useful component |
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