WO1993004754A1 - Process and equipment for the extraction of solid, granular and/or crushed materials with a liquid and for pretreatment thereof to further extraction - Google Patents
Process and equipment for the extraction of solid, granular and/or crushed materials with a liquid and for pretreatment thereof to further extraction Download PDFInfo
- Publication number
- WO1993004754A1 WO1993004754A1 PCT/HU1992/000033 HU9200033W WO9304754A1 WO 1993004754 A1 WO1993004754 A1 WO 1993004754A1 HU 9200033 W HU9200033 W HU 9200033W WO 9304754 A1 WO9304754 A1 WO 9304754A1
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- WO
- WIPO (PCT)
- Prior art keywords
- solid
- liquid
- extraction
- orifice
- screw
- Prior art date
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B30—PRESSES
- B30B—PRESSES IN GENERAL
- B30B9/00—Presses specially adapted for particular purposes
- B30B9/02—Presses specially adapted for particular purposes for squeezing-out liquid from liquid-containing material, e.g. juice from fruits, oil from oil-containing material
- B30B9/12—Presses specially adapted for particular purposes for squeezing-out liquid from liquid-containing material, e.g. juice from fruits, oil from oil-containing material using pressing worms or screws co-operating with a permeable casing
- B30B9/18—Presses specially adapted for particular purposes for squeezing-out liquid from liquid-containing material, e.g. juice from fruits, oil from oil-containing material using pressing worms or screws co-operating with a permeable casing with means for adjusting the outlet for the solid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0215—Solid material in other stationary receptacles
- B01D11/0223—Moving bed of solid material
- B01D11/0226—Moving bed of solid material with the general transport direction of the solids parallel to the rotation axis of the conveyor, e.g. worm
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0215—Solid material in other stationary receptacles
- B01D11/0223—Moving bed of solid material
- B01D11/023—Moving bed of solid material using moving bands, trays fixed on moving transport chains
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B30—PRESSES
- B30B—PRESSES IN GENERAL
- B30B9/00—Presses specially adapted for particular purposes
- B30B9/02—Presses specially adapted for particular purposes for squeezing-out liquid from liquid-containing material, e.g. juice from fruits, oil from oil-containing material
- B30B9/12—Presses specially adapted for particular purposes for squeezing-out liquid from liquid-containing material, e.g. juice from fruits, oil from oil-containing material using pressing worms or screws co-operating with a permeable casing
- B30B9/127—Feed means
Definitions
- This invention relates to a process for extracting solid, granular and/or crushed materials with a liquid, for a pretreatment thereof to further extraction as well as an equipment for carrying out this process.
- the crushing is carried out by using various grinding apparatus (e.g. hammer mill, roll train and the like).
- various grinding apparatus e.g. hammer mill, roll train and the like.
- the removal of substances (extraction) can most favourably be effectuated from a material ground to a powder since the decomposition of cell walls occurs to the highest grade in this case.
- the extent of grinding is limited thereby that the flow of liquid through the ground solid aggregate being in powder form proceeds only with holdback and can even be stopped in extreme cases.
- the continuously working (operating) counter- current solid/liquid extractors are particularly sensitive therefore, the optimization of the grade (extent) of grinding is necessary. It should be noted that the operation of grinding is usually not directly connected to the extractor; the grinding apparatus is located farther, eventually in a separate space.
- An efficient chemical decomposition i.e. dissolution of the valuable substance (active agent) substantially requires the getting of the decomposing (extracting) liquid to each solid particle and a sufficient residence time thereof together with the solid particle.
- the decomposition of the periwinkle (Vinca minor L.) plant material is traditionally carried out in an apparatus fitted with a Z-arm: the ground plant material is stirred (kneaded) together with the added decomposing organic solvent for 3 hours, then the wet solid kneaded with (decomposed by) the liquid is introduced to the extractor through the feeding in system.
- the equipment described above is burdened by several unfavourable properties.
- the duration of the decomposition is long even in the case when the behaviour of the solid is extremely favourable from the point of view of extraction; the "Vinca minor L.” mentioned above is also a material of such type.
- the kneading equipment is technically rather complicated.
- the solid grist of great mass and the decomposing liquid are difficult to be mixed and even in the case of stirring them together for several hours, it occurs that the liquid cannot get to all solid particles whereby undecomposed particles are introduced to the extractor to result in a significant deterioration in the extraction efficiency thereof.
- Beside the continuously working extraction equipment the use of a kneading equipment operating periodically is unfavourable and in addition, the kneader and the feeder have a rather high space demand.
- a part of the granular solids to be extracted possesses unfavourable properties unpreferably influencing the process of obtaining the active agents particularly in the case when the obtaining (recovery) of the active agent from the solid, is carried out in continuous operation by a countercurrent liquid.
- Such unfavourable material characteristics are e.g. as follows:
- the solid particle possesses a cell wall being impermeable to the liquid, which cannot be treated by the traditional mechanical and chemical decomposition and therefore, the efficiency of the extraction cannot be increased beyond a certain (defined) limit value.
- the material transfer becomes slower and the extraction period is significantly increased (e.g. in the extraction of Cataranthus),
- the present invention is aimed to solve the pretreatment, i.e. decomposition for extracting a solid with a liquid, whereby materials having unfavourable properties from the viewpoint of extraction, e.g. fatty, diffusion-weakening cell walls or extreme swelling properties, can be extracted in the optimum (best) way namely, with an efficiency over 95%, low liquid/solid ratio and a short time of residence in the extractor.
- the invention is based on the recognition that materials disturbing the extraction process, chiefly fat, can be removed from the solid by wetting the solid to be extracted, pressing out a part of the wetting liquid from the solid while subjecting the solid to an influence mechanically decomposing the cell walls and subsequently again bringing liquid to the material thus treated; the cell walls weakening the diffusion in an undecomposed state become capable to let in and out the liquid; the formation of the cell liquor and the deformation of solid particles are already finished before their entry to the reactor; thus, the ideal conditions are ensured for a best extraction.
- the aim of the invention has been achieved by a process including mixing the solid with a liquid resulting in a chemical decomposition thereof and pressing out the liquid mixed with the material (product) to be obtained from the solid, which comprises
- granular and/or crushed material means all ground, milled, granulated materials and the like, from which any useful ingredient (component) can be obtained by extraction.
- the solid pressed out by an overpressure is pressed through a slit before its transfer to the extractor and by the edge of the wall bounding the slit an edge force is effected on the solid, which results in the mechanical destruction (decomposition) of the cells or a part thereof. Due to this measure, the further treatment of the material in the extractor can be carried out with a higher efficiency, particularly in the cases of materials possessing peculiar properties mentioned in the introduction of this description.
- the decomposing liquid is applied by spraying onto the crushed solid being in movement; thus, the contact of the media can be made more uniform and effective.
- a preferred embodiment of the process also consists therein that the pressure of the solid is continuously enhanced while continuously decreasing its volume during its transfer under an overpressure. This can be achieved by conveying the material by a screw, the threads of which have an increasing volume while passing from the site of feeding in up to the site of leaving.
- the equipment according to the invention has a screw conveyor for contacting the solid with the decomposing liquid as well as devices for removing the liquid containing also substance obtained from the wetted solid.
- the screw conveyor is built in as a part of such a conveying-wetting unit to the casing thereof, which has an orifice connected wi th a conduit used for feeding i n the ex t raction liquid, and a feeder joins the casing;
- the casing is in connection with a pressing-decomposing unit possessing a screw press, the thread-volumes of which decrease in the passage direction of the material and the screw press is at least partially surrounded by a filter mantle, the screw press is separated from a chamber by a wall containing an orifice opposed to the screw press, into which a conic destructive body extends, which is movable parallelly with the longitudinal geometric central axis of the screw press against an elastic force; the destructive body toegether with the rim of the orifice bounds a material-transmitting s
- the conveying-wetting unit has a casing formed by a twin-trough with duplicate wall and a cover closing it; the inner side walls of the trough pieces (members) are lower than the outer side walls thus, a common space is present between the trough pieces (members) and the screw conveyors situated in the trough pieces (members) are mounted revolvably in a direction opposed one to the other.
- the conveying-wetting unit contains: an upper fixed cover plate fitted with a feeding, material-transmitting inlet orifice leading to the region of one end of casing of the conveying-wetting unit; a lower fixed disk fitted with a material inlet orifice being displaced in relation to the said orifice; as well as a disk revolvably imbedded between the cover plate and the disk and fitting in thereto by the insertion of sealing; in the revolvable disk, several orifices are shaped which, during rotation of the disk, get to overlapping on the one hand with the orifice of the upper cover plate and on the other hand, with the orifice of the lower disk; around these orifices, sealings are situated between the intermediate revolvable disk and the fixed lower disk.
- ram plates are fastened, which trend horizontally on two sides in the cylindric space bounded by the filter mantle surrounding the screw press in the region of the longitudinal geometric central axis and extend up to the outer outline of the threads of the screw press.
- the volume ratio of the first screw-thread to the last one of the screw press (by considering the passage direction of the material) is 1.5:1 to 3:1, preferably about 2:1 whereas the volumes of the intermediate screw-threads gradually decrease while passing from the first one up to the last one.
- the pitch is constant and the volume decrease is ensured by decrease in the thread-depth.
- the adjustment of the sleeve is made possible by its conveniently threaded formation and connection.
- an inner wall being perpendicular to the longitudinal geometric central axis of the screw press is built in to the chamber and the sleeve is placed in the central orifice thereof whereas at least three orifices fitted with bearings are formed in the circumferential region of the wall; rods are led through these orifices in such a way that one end thereof is fastened to the disk connected with the socket and the other end thereof is fastened to an end disk, in which an orifice fitted with bearings is provided (formed) for receiving the end of the axis.
- Figure 1 shows a preferred embodiment of the equipment in a schematic vertical longitudinal section, partly from a side-view
- Figure 2 illustrates the feeding device and conveying-wetting unit on a higher scale
- Figure 3 shows the section taken along the line A-A signed in Figure 2;
- Figure 4 shows the section taken along the line B-B signed in Figure 2;
- Figure 5 indicates the detail D signed in Figure 2 on a higher scale
- Figure 6 illustrates the pressing-decomposing unit of the equipment according to Figure 1 on a higher scale in the section taken along the line I-I signed in Figure
- Figure 7 is a section taken along the line E-E signed in Figure 6;
- Figure 8 demonstrates the forces occurring in the decomposition process on the drawing containing the detail G of higher scale signed in Figure 6;
- Figure 9 shows a detail of the screw illustrated in Figure 6 on a higher scale
- Figure 10 illustrates the feeding-charging unit of the equipment according to Figure 1 on a higher scale
- Figure 11 is a section taken along the line H-H signed in Figure 10,
- Figure 12 illustrates the process according to the invention by the use of a combined equipment established by connecting the equipment according to Figure 1 with a solid/liquid extractor of bulk flow (conveyor) system.
- Main parts of the equipment according to Figure 1 are: the charger 1, the conveying-wetting unit signed as a whole by the reference number 2, the pressing-decomposing unit 13, as well as the feeding-charging unit 26 joining the extractor 30, which are connected in series in the order of succession mentioned above. It should be noted that the vertical arrangement according to Figure 1 is suitable but, depending on the given endowments of location, the connection of the main partial units may also be carried out on an identical level by inserting material-conveying equipment parts.
- Main parts of the charger 1 are: throat 10, driving mechanism 11 and charging mechanism 12.
- the conveying-wetting unit 2 contains the partial units 2a, 2b possessing 4a, 4b screw conveyors situated in casings 3a, 3b to which a common drive 5 is adapted.
- the casings 3a, 3b are contacted (connected) through the transmitting orifice 6 one with the other.
- the charger 1 mentioned above leads from above to the end of casing 3a being opposite to the drive 5 and the transmitting orifice 6.
- the long geometric central axes of screws 4a, 4b are signed by the reference letters x 1 and x 2 , respectively.
- the feeding in conduits 7a, 7a' lead from above into the casings 3a, 3b.
- conduits serve for spraying in the wetting liquor (accordingly, nozzles /not illustrated/ are connected to the feeding orifices).
- a feeding in conduit 76 of the same kind leads to the casing 3b, too. Beneath the end of casing 3 being opposite to the transmitting orifice 6, an outlet 8 exists.
- a transfer tube 9 joins, which leads to casing 14 of the pressing-decomposing unit 13, to one end thereof fitted with the drive 17 through the inlet 9a.
- a screw 15 surrounded by the filter mantle 16 and connected to the drive 17 is formed, the longitudinal geometric central axis of which is signed by the reference letter x 3 .
- An outlet 18 leaves the casing 14 beneath.
- the wall 19 is one bounding wall of front-side of the chamber 21.
- the decomposing (destructive) mechanism signed as a whole by the reference number 31 is situated, which will be described in detail hereinafter.
- a feeding in conduit 22 leads to chamber 21 from above whereas an outlet 24 is in its lower part .
- a transfer tube 23 is connected, which leads through the inlet 25 from above to the end opposed to extractor 30 of the feeding-charging unit signed as a whole by the reference number 26.
- the feeding-charging unit 26 has a cylindric casing 27, wherein a screw 28 possessing the longitudinal geometric central axis x 4 is situated; this is connected with the drive 29.
- the longitudinal geometric central axes x 1 , x 2 of the screw conveyors 4a, 4b close an oblique angle ⁇ 1 , ⁇ 2 with the horizontal line.
- the longitudinal geometric central axis x 1 of the upper screw 4a trends from below upwards in the direction, where the solid passes according to the arrow c; the value of this angle ⁇ 1 , is between 0° and 20°, conventiently about 10o.
- the angle ⁇ 2 of the longitudinal geometric central axis x 2 of the lower screw 4b is also between 0° and 20°, and its slope is similarly in the direction of passing of the material signed by arrow e therefore, it extends with a descent and is not ascent (as the longitudinal geometric central axis x 2 ). However, there is no difficulty to form also the longitudinal geometric central axis x 2 in an ascent position. The ascent position deviating from the horizontal makes possible the development of a fluidized bed in the casing 3a or 3b, respectively.
- the conveying-wetting unit 2 according to Figure 1 as well as charger 1 are shown in Figures 2 to 5 in more detail by using the reference numbers of Figure 1 for signing the identical structural elements.
- FIGs 2, 4 and 5 contain the solvings for the parts of charger 1.
- a throat 10 and chamber 40 are connected from above and from beneath, respectively.
- the chamber 40 leads to casing 3a of the partial unit 2a of the wetting-conveying unit 2 (see also Figure 1).
- the charging mechanism 12 has a circular cover plate 35, wherein a similarly circular orifice 33 is shaped; the throat 10 mentioned above used for introducing the solid joins this orifice 33.
- the cover plate 35 has a fixed position: it is rigidly fastened to the rim extending outwards of chamber 40 by the means of screws 39.
- a circular revolvable disk 36 is situated, from which a verticular axis 37 led through the cover 35 extends upwards; this axis 37 is bound with drive 11 being capable in this way to revolve the disk 36 according to arrow n 1 ( Figures 2 and 4).
- n 1 Figures 2 and 4
- the disk 36 three lengthy radial orifices 36a are formed in the identical side interspaces one from another (separated by an angle of 120o each) are shaped.
- the casings 3a, 3b are formed by duplicate-wall, curved twin-troughs 43a, 43b wherein the screw conveyors 4a, 4a' and 4b, 4b' are situated one beside the other.
- the duplicate wall is necessary because it is suitable for carrying out the process of the invention in several cases over room temperature and the duplicate walls can be heated e.g. by hot water or by introducing saturated steam when it is required by the task given.
- the direction of rotation of the screws signed by the arrows n 2 , n 2 ' are opposite one to the other in the trough pieces of the twin-troughs 43a, 43b; i.e. one of the screws is always right-handed, the other screw is left-handed.
- Each of the screw conveyors is in functional connection with the drive 5.
- the outer walls 46a, 46b of the twin-troughs 43a, 43b as well as their frontal wall extend over the screw conveyors whereas the inner wall of the trough pieces are lower, extend only up to the longitudinal geometric central axes x 1 , x 2 of the screws according to the example of embodiment; thus, the screw pairs possess a common space 44a, 44b each, where they are in contact one with the other.
- the screws 4a, 4a' and 4b, 4b' are structurally formed in such a way that the steel plate streak forming the screw leaves 51 prepared from steel are helically rolled up on the axes 50 rotating during operation.
- screw structures of other sort may also be used.
- the pressing-decomposing unit signed as a whole by the reference number 13 in Figure 1 is described in detail in Figures 6 to 9; the structural elements previously discussed are signed by the reference numbers previously used.
- the pressing-decomposing unit 13 has sections I and II built together one with the other; the compression is carried out in the section I whereas section II is provided for decomposing the cells.
- the pressing-decomposing unit 13 is shaped in such a manner that, depending on the demands given, it can be operated in two different modes of working.
- Section I provided for compression can be operated alone or together with section II provided for the decomposing procedure by forming an operation series.
- the desired mode of working can be accomplished by adjusting the decomposing mechanism 31 dependently on the properties of the given raw material (grist) to be processed (see hereinafter).
- the stump 52 is connected, which represents a part of the transfer-tube 9 shown in Figure 1.
- the main structural element of section I is the rotating screw press 15 surrounded by a cylindric skeleton 53, this is covered by the filter mantle 16 mentioned above in relation to Figure 1, which is suitably prepared from screening cloth.
- the pitch of the screw press 15 is constant, however, the thread-depth gradually decreases in the passage direction signed by arrow 9 of the solid as it can clearly be seen in Figures 6 and 9.
- the horizontal ram plates 54 extending up to the outer outline of the screw leaves lead from both sides into the inner space of the skeleton 53 covered by the filter mantle 16. The intended purpose of the ram plates 54 will be described hereinafter.
- ram plates are situated on a horizontal plane passing through the longitudinal geometric central line x 3 and are fastened to skeleton 53, which latter is fixed to the cylindric casing 14.
- the truncated conic-shaped, hollow desctructive body 57 which can move back and forth according to the double arrow k 1 in the direction of the longitudinal geometric central axis x 3 , fits to the central orifice 20, which is situated oppositely to the screw press 15 in the wall 19 formed by the flat plate and closing the cylindrical casing 14 on its frontal side opposed to the inlet orifice 9a.
- the screw press 15 is shaped in such a manner that the mean thread-depth of the first screw-thread 55 being at the feeding in orifice 9a and the volume element v 1 , respectively corresponding to the area bounded by the thread-depth and stretched by hatching in Figure 9, are essentially greater than the volume element v u of the last screw-thread 56; besides, the volumes of the screw-threads between these two screw-threads 55, 56 gradually decrease while passing from screw-thread 55 to the screw-thread 56. It is suitable to bring the volume element ratio v u /v l between the following values:
- v u /v l The optimum value of v u /v l is about 1/2.
- this element which is an unconditionally important partial unit of the section II ( Figure 6) and decomposing mechanism 31, respectively together with a socket 58, which the axis 61 fastened to the screw press 15 is led through, the centre line of axis 61, socket 58 and screw press 15 is the same, i.e. the longitudinal geometric central axis x 3 .
- rods 62 preferably at least three or four rods being parallel to the longitudinal geometric central axis x 3 , is fastened to the edge of disk 59; the other end thereof is rigidly fastened to an end disk 68 where the central orifice 67 fitted with bearings is present; the end of axis 61 mentioned above joins this orifice 67 fitted with bearings in a manner allowing the free movement according to the double arrow k 1 ( Figure 6).
- an intermediate wall 63 prepared from plate is also incorporated in a fixed manner, which divides the inner space of the chamber to two parts. Near to the circumferential region of the wall 63, orifices 64 fitted with bearings are provided for leading through the rods 62 mentioned above.
- a central orifice 69 is present, with a threaded sleeve 70, thus being adjustable to the direction signed by the double arrow k 1 .
- the supporting plate 65 being perpendicular to the longitudinal geometric central axis x 3 is fastened to the edge thereof lying towards the disk 59.
- a prestressed helical spring 60 surrounding the axis 61 is situated; the supporting plate 65 mentioned above, which is mobile and can be fastened in an optional position between the terminal positions of its movement, is actually provided for supporting and prestressing the helical spring 60 on its one side.
- the transverse bearing 66 shown in Figure 6 serves to support the axis 61.
- the feeding in conduit 22 previously mentioned in relation to Figure 1 leads to the frontal part of the cylindric chamber 21, which is between the walls 63 and 19.
- the outlet orifice 24 also leads out from this frontal part of the chamber.
- the dimensions of the helical spring are selected and the grade of its prestress is adjusted in such a way that the P E edge force (indicated in Figure 8) occurring in the contact line of the wall 19 and the truncated conic-shaped destructive body 57 falls into the following range of values:
- the spring force should be adjusted in such a way that the outer conic mantle surface of the conic destructive body 57 be capable to extend by 5 to 10 mm from the edge of orifice 20 beside the operation of the edge force P E and thus, the solid be capable to leave while being decomposed by the slit (see later, Example 2). In this time, a surface overpressure of total 8 to 10 bar acts on the solid passing through the slit.
- the adjustment of the decomposing mechanism 31 is carried out as follows.
- the threaded socket 70 and the mobile supporting rate 65 moving therpwith are adjusted to the right starting position in order to stop the support of the helical spring 60 by the supporting plate.
- the outer conic mantle surface of the conic destructive body is removed from the edge of orifice 20 by about 30 mm and in this way the solid compressed in the section I, where it is under the effect of about 0.5-4.0 bar overpressure along the screw press 15, can freely leave through the "open slit" without any functioning of section II, i.e. the value of the edge force
- edge force P E arises from the prestress of the helical spring 60 when the conic destructive body 57 is stretched to the edge of orifice with a diameter D 1 of the disk-like wall 19.
- P cs is the sliding (shear) force, against which the material leaves the material-transmitting slit of measure X ⁇ sin ⁇ opening along the mantle of the conic destructive body 57 as a result of the displacement X occurring during the compression.
- the shear force P P E ⁇ cos ⁇ "cuts" the solid particles along the edge of the orifice having a D 1 diameter.
- the feeding-charging unit 26 shown in Figure 1 is illustrated on a higher scale in Figures 10 and 11 while using the reference numbers and signs previously employed according to the sense.
- the longitudinal geometric central axis x 4 of screw 28 and therefore, the trough 71 with duplicate wall forming the casing 27 as well as its sealing cover are also horizontal.
- the feeding conduit 32 mentioned in relation to Figure 1 leads through the cover 72 near to the inlet orifice 25 into the inner part of casing 27.
- the trough 72 is connected to the extractor 30 (not shown here separatedly), more precisely to the stump thereof introducing the solid, by the aid of the rim 77 of trough 72 and screws 78.
- a feeding conduit 75 used for introducing a heating or cooling medium leads into the space between the walls of trough 71 having duplicate walls and an outlet conduit 76 used for removing this medium leaves.
- the screw leaves are formed by the plate streak helically rolled up to the revolvable axis 73.
- the material e.g. plant material previously decomposed mechanically, e.g. by grinding and thus being in a coarse-granular state is fed in according to arrow a signed in Figure 2 by the conveying mechanism (not illustrated) through the throat 10 by the means of the charging mechanism 12 through the chamber 40 into the conveying-wetting unit 2.
- a closed charging can be accomplished by using the charger 1 according to the invention since portions of identical volume are introduced through the orifices 33, 36a and 42 into the conveying-wetting unit 2 while the disk 36 rotates in such a way due also to the sealing rings 41a, 41b and 41d ( Figure 5), it is completely inhibited that through the orifices turned away one from the other, vapours arising from the liquid(s) introduced to the conveying-wetting unit 2 continuously get to the conveying mechanism joining the throat 10, which could be very dangerous when using e.g. liquid organic solvents.
- the air-dry solid grist fed in through chamber 40 according to arrow b is conveyed (transferred) in a free transportation by the rotating screws 4a, 4a' ( Figure 3) in the upper partial unit 2a of the conveying-wetting unit 2 in the direction of arrow c towards the transmitting orifice 6 ( Figures 1 and 2) while a liquid is sprayed onto the moving solid from above through the feeding conduits 7a, i.e. at various sites according to the arrows k.
- the solid moved-conveyed in a rotating state gets to intimate contact with the liquid and takes up a significant part thereof.
- the wetted solid falls through the transmitting orifice 6 according to arrow d into the partial unit 2b onto the rotating screws 4b, 4b' where, while passing under stirring (arrow e), the taking up of moisture is finished; when necessary, an additional amount of liquid can be introduced into the solid mass through the feeding conduit 7b (arrow l). Due to the moisture uptake a deformation, e.g. swelling, may occur in some kinds of solids.
- the wet, optionally swollen solid gets from the partial unit 2b through the outlet orifice 8, transfer-tube 9 and inlet orifice 9a, according to arrow f ( Figures 1 and 2) to the pressing-decomposing space 13.
- the solid pretreated by wetting and stirring for a relatively long time (which can be controlled by the number of revolutions of the screws) is led to the fore-part of section I ( Figure 6), more particularly into the first 55 threads of the screw press 15 of changing thread-depth within the pressing-decomposing unit 13. While rotating, the screw press 15 conveys the material towards the orifice 20, i.e. the destructive body 57 ( Figure 6) according to arrow g ( Figures 1 and 6).
- a fat-containing liquid usually containing also the active agent leaves the solid, which is led to further processing (into a collecting vessel) chiefly for isolating the active agent.
- the efficiency of liquid exemption achieved by the screw press 15 is enhanced by the horizontal ram plates 54 ( Figures 6 and 7) built into the cylindric space bounded by the filter mantle 16. These ram plates divide this space to two halves: namely, due to the presence of these ram plates (ribs), the whole mass of the wetted solid is forced to a passing movement without rotation.
- the conic destructive body 57 (ram cone) is braced by the controllable compressive force displayed by the chemical spring 60.
- the surface force can be controlled, which acts for achieving the needed decomposition of the cell wall on the aggregation of particles pressed through the slit between the wall 19 and the conic destructive body 57 extending into the orifice 20 being in the wall 19.
- the wet solid which has been pressed through along the destructive body 57 and exempted from the major part of its liquid content, and contains cells decomposed in their most part, falls down in the direction of arrow g, leaves the pressing-decomposing unit 13 under effect of gravity through the outlet orifice 24 according to arrow h ( Figures 1 and 6) and, as clearly shown in Figures 1 and 10, after falling into the feeding-charging unit 26 it gets to the screw 28 thereof through the inlet orifice 25. Then, this screw conveys the material into the extractor 30 according to arrow i.
- the granular solid can additionally be treated in the feeding-charging unit 26 with a liquid introduced through the feeding conduit 32 (arrow o ); usually, an extraction liquid is fed into casing 27 by spraying.
- the material being well mixed with this liquid during its screw conveyance gets to the extractor 30 according arrow j. It is of purpose to select the amount of the sprayed in extraction liquid in such a manner that it be identical or nearly identical with the amount of liquid removed from the solid in the pressing-decomposing unit 13. According to our experience the solid pretreated in this way can well be extracted e.g. in a countercurrent solid/liquid extractor.
- the pretreating equipment shown on the left side of Figure 12 as a whole signed by the reference number 80 is identical with the equipment according to Figures 1 to 11 whereas on the right side of Figure 12 an U-shaped, countercurrent solid/liquid extractor of bulk flow (conveyor) system is indicated signed as a whole by the reference number 30 used also in Figures 1 and 10.
- an extractor is known e.g. from the United States patent specification No. 3,279,890.
- perforated disks attached onto a drag chain pass in the direction of arrow r.
- the neighbouring disks bound cells one with the other, which are provided to receive the solid to be extracted. After compression and decomposition of the cells , the solid to be extracted arrives from the pretreating equipment
- the feeding-charging unit 26 shown in Figures 1 and 10 leads to the extractor 30 and smoothly passes in casing 79 up to the outlet 82 (arrow t).
- the extraction liquid passes in a counterflow (arrows z ) against the solid in casing 79, the extraction of solid occurs as a result of contact (intensified by the vibrator or pulsator 105) with the liquid and the active agent is transferred from the solid to the liquid.
- the solid exempted from the active agent and containing liquid gets to the screw press 83 according to arrow u , where the liquid is pressed out from the solid and the major part of liquid leaves through the filter mantle 84, i.e. the solid loses a significant part of its liquid content.
- the solid falls into the liquid-exempting unit 85 (e.g. drier, evaporator and the like).
- the solid here fully exempted from liquid is led through the conduit 92 to the conveying device 86, wherefrom it gets to vessel 87 according to arrow v 1 . If the liquid pressed out is valuable, i.e. not water, it is led through the conduit 106 into the vessel 88 supplying the system with extraction liquid.
- a conduit 89 containing the charging pump 90 leads out from the bottom of vessel 88.
- One conduit 89a branched off therefrom feeds the extraction liquid to the upper end of one shank of the U-shaped casing 79; through the other conduit 32 (previously mentioned in connection with Figures 1 and 6) branched off from conduit 89, and extraction liquid can be introduced by spraying from above into the feeding-charging unit 26 of the pretreating equipment 80.
- it is suitable to feed a little portion of the extraction liquid into the pressing-decomposing unit 13 of the pretreating equipment 80, which the conduit 22 is provided for. It should be noted that it may be convenient from a technological point of view to spray an extraction liquid into the feeding-charging unit 2, too, this becomes possible by using the conduits 7a, 7a' (with cross-connections not illustrated).
- the vessel 88 is supplied with fresh extraction liquid through the conduit 91.
- the extract containing the active agent is separated from the wet solid in the filter chamber 93 of the extractor 79. From here, the extract is led by a pump through the conduits 94, 96 and 96a into the vessel 97 collecting the extract; however the totel amount or a part of the extract may be fed through the conduits 96 and 97a into the partial unit 2a of the previously discussed conveying-wetting unit of the pretreating equipment 80 (see also Figure 1).
- the extract is led to further processing (isolation of the active agent) through the conduit 18 leaving section I signed in Figure 6 of the pressing-decomposing unit 13 as well as through the conduit 18a into the vessel 97 mentioned above, wherefrom it can be conveyed by the pump 98 through conduit 102 to the site of isolation of the active agent.
- the decomposing liquid required to the chemical pretreatment is sprayed from vessel 99 by the pump 100 into the partial units 2a, 2b of the conveying-wetting unit 2 through the conduits 7, 7a', 7b (described in connection with Figures 1 and 2).
- the conduit 100 leading to vessel 99 is provided for supplying the decomposing liquid.
- the liquid leaving the pressing-decomposing unit 13 through the conduit 18 is led not into the extract-collecting vessel 97 but through the conduit 18b into the vessel 103, and conveyed further by the pump 104 for annihilation.
- the active agent is extracted from dried ergot plant material ("drug").
- the dried plant material is pretreated by using the process of the invention. It is known that the alkaloid content of the sorts of dried ergot plant materials (“drugs") (containing ergotamine, ergocristine, ergocornine-ergocryptine and ergocryptine) varies between 4 g/kg and 6 g/kg.
- the dried plant material is ground to a material of 2 to 3 mm particle size on a roller mill.
- the grist is fed through the charger 1 of the pretreating equipment 80 into the conveying-wetting unit 2 by the means of a suitable conveyor.
- the charging of the dried plant material is controlled (regulated) in such a manner as to introduce 8D to 90 kg/hour of grist into the equipment.
- first extraction liquid 80 litres of ethyl acetate per hour as "first" extraction liquid and 40 litres of concentrated ammonium hydroxide per hour as chemically decomposing liquid are charged.
- the plant material is treated, i.e. wetted, stirred and conveyed in the partial units 2a, 2b of the wetting-conveying equipment 2, while being forced to a swirling movement, at room temperature (20 to 25 oC) under atmospheric pressure for about 60 minutes.
- the liquids are kneaded into the plant material and the particles of the plant material are swollen.
- the swollen plant material is led into the pressing-decomposing unit 13, where the major part of the cells are ruptured under the effect of the overpressure, which then continuously increases meanwhile the material passes forwards to result in about 80 litres of press liquor per one hour ("first" extract).
- the press liquor contains about 30 to 35% of the alkaloid content of the dried plant material together with strange substances, e.g. fat, which interfere with the further extraction.
- This "first" extract is introduced to the vessel 97 shown in Figure 12.
- the partially extracted plant material is conveyed by the means of the feeding-charging unit 26 into the extractor 30.
- the feeding unit 26 80 litres of ethyl acetate per hour are fed in as "second" extraction liquid and the residence time of the material is adjusted here to 15 minutes. An intimate contact occurs also here between the solid and the secondary extraction liquid during the conveyance by screw.
- the passage rate of the solid is adjusted (by suitably selecting the rate of chain carrying the perforated cells) in such a way as to achieve a residence time of 120 minutes of the plant material in the extractor.
- a "third" extraction liquid 240 litres of ethyl acetate per hour are charged into the extractor 30 on its side opposite to the feeding in of the plant material .
- the extraction liquid passes in a counterflow against the solid (see arrows s and z on Figure 12).
- the extraction is carried out at room temperature (20 to 25 oC).
- the extract (“secondary" extract) leaves the extractor 30 through the conduit 94 and gets to the vessel 97.
- the total amount of the "first” and “second” extractions is 230 to 240 litres per hour and contains about 95 to 98% of the alkaloid content of the dried plant material.
- the solid extracted is removed from the extractor 30 through the press 83.
- Vinblastine is extracted from the dried Cataranthus plant material by using the process according to the invention. It is known that Cataranthus plant material is ground to a solid aggregation consisting of particles of 3 to 4 mm in size on a roller mill. The grist is fed in an amount of 50 to 60 kg per hour through the charger 1 into the conveying-wetting unit 2 of the equipment according to Figure 12. Into the same unit 70 litres of 5% aqueous tartaric acid solution and 90 litres of water per hour are charged as "first" extraction liquid through the conduits 7a and 7b. The residence time in the conveying-wetting unit 2 of the material is adjusted to 1 hour. The pretreatment is carried out at 50 oC. During this period, the material becomes completely wetted, the gel stock of cells takes up the water, the material particles swell and the diffusion starts.
- the swollen plant material is introduced to the pressing-decomposing unit 13, where the cells are ruptured under the decomposing effect of overpressure occurring in the section I (screw press period) as well as the edge force occurring at the beginning of section II; here, about 110 litres per hour of press liquor ("first" extract) are obtained, which contains 55-60% of the vinblastine content of the dried plant material.
- the rate of drag chain is adjusted so as to achieve a residence time of about 60 minutes of the plant material in the extractor 30.
- a "second" extraction liquid 110 litres per hour of water and 20 litres per hour of 5% aqueous tartaric acid are fed into the extractor 30 through the conduit 89a drawn in Figure 12, which passes (moves) counter- currently against the plant material.
- the amount of tartaric acid solution has been so selected as to obtain a pH value of 3 to 3.2 for both the "first" and “second” press liquors.
- the "second” press liquor (extract) leaves the filter unit 93 of extractor 30 and is conveyed by the pump 95 through the conduit 94 into the collecting vessel 97.
- the total amount of the "first" and “second” extracts is 210 to 220 litres per hour, which contains 95 to 97% of the vinblastine content of the dried plant material (35 to 37% of which are extracted in the extractor 30).
- the plant material extracted is removed from extractor 30 by the means of press 83 drawn in Figure 12.
- a substantially important advantage of the invention lies therein that substances possessing unfavourable properties from the viewpoint of extraction, e.g. high fat content, propensity to strong swelling, can also be extracted with a high efficiency and by their pretreatment the factors unfavourably influencing the extraction can be eliminated or at least essentially decreased by using the invention.
- the equipment according to the invention can be either connected to an existing extractor or built in as a partial unit of a novel establishment.
Abstract
Description
Claims
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP92918714A EP0643607A1 (en) | 1991-09-02 | 1992-08-29 | Process and equipment for the extraction of solid, granular and/or crushed materials with a liquid and for pretreatment thereof to further extraction |
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
HU912838A HU212591B (en) | 1991-09-02 | 1991-09-02 | Process and equipment for extraction of solid granular and/or cracked materials with liquid and for pretreatment of further extraction |
HU2838/91 | 1991-09-02 | ||
CN92111221A CN1080203A (en) | 1991-09-02 | 1992-09-02 | Method and apparatus with the liquid extraction solid material |
Publications (1)
Publication Number | Publication Date |
---|---|
WO1993004754A1 true WO1993004754A1 (en) | 1993-03-18 |
Family
ID=25742801
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/HU1992/000033 WO1993004754A1 (en) | 1991-09-02 | 1992-08-29 | Process and equipment for the extraction of solid, granular and/or crushed materials with a liquid and for pretreatment thereof to further extraction |
Country Status (6)
Country | Link |
---|---|
EP (1) | EP0643607A1 (en) |
CN (1) | CN1080203A (en) |
AU (1) | AU2498392A (en) |
HU (1) | HU212591B (en) |
WO (1) | WO1993004754A1 (en) |
ZA (1) | ZA926611B (en) |
Cited By (6)
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---|---|---|---|---|
GB2354720A (en) * | 1999-09-30 | 2001-04-04 | Imp Machine Company | Vertical screw press with cone weight having spring bias means and curved sides |
CN103657140A (en) * | 2013-12-19 | 2014-03-26 | 昆明旭邦机械有限公司 | Efficient continuous extraction device |
RU2518605C2 (en) * | 2012-08-27 | 2014-06-10 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Казанский государственный аграрный университет" (ФГБОУ ВПО Казанский ГАУ) | Device for production of plant extract |
ITCO20130050A1 (en) * | 2013-10-16 | 2015-04-17 | Austep S P A | "DEVICE AND PROCEDURE FOR FORSU TREATMENT" |
CN105749580A (en) * | 2014-08-10 | 2016-07-13 | 王选明 | Two-stage digestion equipment applied to extraction of rhododendron simsii active components |
CN108689184A (en) * | 2018-06-05 | 2018-10-23 | 深圳市胜百机械设备制造有限公司 | Upright powder feeder |
Families Citing this family (3)
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CN108295504A (en) * | 2018-03-15 | 2018-07-20 | 上海齐达重型装备有限公司 | A kind of efficient solid-liquid counter-current extraction device and leaching method |
CN108544789B (en) * | 2018-06-11 | 2023-08-22 | 中国人民解放军63908部队 | Roller-pressing type cartridge destroying machine |
CN109304045A (en) * | 2018-10-28 | 2019-02-05 | 飞潮(无锡)过滤技术有限公司 | A kind of separation of 700Mpa high hydrostatic pressure extraction and synchronous energy recovery process |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DD153326A5 (en) * | 1979-10-04 | 1982-01-06 | Raffinerie Tirlemontoise Sa | DEVICE FOR EXTRACTING SOLID INGREDIENTS FROM SOLIDS |
DE3101768A1 (en) * | 1981-01-21 | 1982-08-26 | Fabriques de Tabac Réunies S.A., 2003 Neuchâtel | DEVICE FOR EXTRACTING LIQUID-SOLUBLE COMPONENTS FROM SMALL-CUT PLANT PRODUCTS |
DE3343478A1 (en) * | 1983-12-01 | 1985-06-27 | Heinz 2050 Hamburg Schumacher | DEVICE AND METHOD FOR CONTINUOUS SOLID-LIQUID EXTRACTION |
DE3828097A1 (en) * | 1987-08-18 | 1989-03-02 | Defimas Societe A Responsabili | Process for isolating utilisable substances from natural products and use of an apparatus for carrying out the process |
-
1991
- 1991-09-02 HU HU912838A patent/HU212591B/en not_active IP Right Cessation
-
1992
- 1992-08-29 WO PCT/HU1992/000033 patent/WO1993004754A1/en not_active Application Discontinuation
- 1992-08-29 EP EP92918714A patent/EP0643607A1/en not_active Withdrawn
- 1992-08-29 AU AU24983/92A patent/AU2498392A/en not_active Abandoned
- 1992-09-01 ZA ZA926611A patent/ZA926611B/en unknown
- 1992-09-02 CN CN92111221A patent/CN1080203A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DD153326A5 (en) * | 1979-10-04 | 1982-01-06 | Raffinerie Tirlemontoise Sa | DEVICE FOR EXTRACTING SOLID INGREDIENTS FROM SOLIDS |
DE3101768A1 (en) * | 1981-01-21 | 1982-08-26 | Fabriques de Tabac Réunies S.A., 2003 Neuchâtel | DEVICE FOR EXTRACTING LIQUID-SOLUBLE COMPONENTS FROM SMALL-CUT PLANT PRODUCTS |
DE3343478A1 (en) * | 1983-12-01 | 1985-06-27 | Heinz 2050 Hamburg Schumacher | DEVICE AND METHOD FOR CONTINUOUS SOLID-LIQUID EXTRACTION |
DE3828097A1 (en) * | 1987-08-18 | 1989-03-02 | Defimas Societe A Responsabili | Process for isolating utilisable substances from natural products and use of an apparatus for carrying out the process |
Cited By (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB2354720A (en) * | 1999-09-30 | 2001-04-04 | Imp Machine Company | Vertical screw press with cone weight having spring bias means and curved sides |
RU2518605C2 (en) * | 2012-08-27 | 2014-06-10 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Казанский государственный аграрный университет" (ФГБОУ ВПО Казанский ГАУ) | Device for production of plant extract |
KR20160070792A (en) * | 2013-10-16 | 2016-06-20 | 아우스텝 에스.피.에이. | Device and method for the treatment of 'FORSU' |
ITCO20130050A1 (en) * | 2013-10-16 | 2015-04-17 | Austep S P A | "DEVICE AND PROCEDURE FOR FORSU TREATMENT" |
WO2015056073A1 (en) * | 2013-10-16 | 2015-04-23 | Austep S.P.A. | Device and method for the treatment of forsu |
US10449580B2 (en) | 2013-10-16 | 2019-10-22 | Austep S.P.A. | Device and method for the treatment of FORSU |
KR102314555B1 (en) * | 2013-10-16 | 2021-10-21 | 안디온 글로벌 인코퍼레이티드 | Device and method for the treatment of 'FORSU' |
CN103657140B (en) * | 2013-12-19 | 2016-02-10 | 昆明旭邦机械有限公司 | A kind of high-efficiency and continuous extraction element |
CN103657140A (en) * | 2013-12-19 | 2014-03-26 | 昆明旭邦机械有限公司 | Efficient continuous extraction device |
CN105749580A (en) * | 2014-08-10 | 2016-07-13 | 王选明 | Two-stage digestion equipment applied to extraction of rhododendron simsii active components |
CN105749580B (en) * | 2014-08-10 | 2018-09-21 | 嘉兴智慧园区营运管理有限公司 | Two level extraction equipment applied to the extraction of azalea active component |
CN108689184A (en) * | 2018-06-05 | 2018-10-23 | 深圳市胜百机械设备制造有限公司 | Upright powder feeder |
CN108689184B (en) * | 2018-06-05 | 2024-03-22 | 深圳市一胜百机械设备制造有限公司 | Vertical powder feeder |
Also Published As
Publication number | Publication date |
---|---|
CN1080203A (en) | 1994-01-05 |
AU2498392A (en) | 1993-04-05 |
HU912838D0 (en) | 1992-01-28 |
HU212591B (en) | 1996-08-29 |
ZA926611B (en) | 1993-05-17 |
EP0643607A1 (en) | 1995-03-22 |
HUT66578A (en) | 1994-12-28 |
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