CN102614682B - Material extraction device - Google Patents

Material extraction device Download PDF

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Publication number
CN102614682B
CN102614682B CN201210121714.9A CN201210121714A CN102614682B CN 102614682 B CN102614682 B CN 102614682B CN 201210121714 A CN201210121714 A CN 201210121714A CN 102614682 B CN102614682 B CN 102614682B
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leaching
liquid
container
heat exchanger
unit
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CN102614682A (en
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徐顺民
李治平
李学锋
何建秋
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Abstract

The invention discloses a material extraction device, which comprises a material leaching unit and a liquid heating unit which are vertically arranged side by side and are communicated, wherein the material leaching unit consists of a normal pressure leaching container; the liquid heating unit consists of a heat exchanger; a feed port, a solvent port, a sight glass, a cooling and collection unit and a condensation and reflux unit are arranged above the material leaching container, and a filter unit and a slag discharge door are arranged below the material leaching container; the filter unit below the material leaching container is communicated with the lower space of the heat exchanger through a leaching solution natural circulation passage or a leaching solution forcible circulation passage which can be selected and switched; and a leaching solution circulation and return passage inlet which is communicated with a leaching solution circulation outlet above the heat exchanger is formed on a side wall of a part above a working liquid surface of the material leaching container. According to the device, the heating mode of straight-through industrial steam can be effectively avoided, and the extraction of required components of the material can be finished with high efficiency and high quality in a closed natural circulation state; and the device is scientific, simple, convenient, efficient and energy-saving and can be widely applied to leaching of a material by water or an organic solvent and extraction/separation operation of steam distillation and the like.

Description

Material extraction element
Technical field
The present invention relates to a kind of material extraction element, be applicable to but be not limited only to the extraction to material component in field of traditional Chinese medicine pharmacy.
Background technology
Collect by modes such as leaching, distillations the required composition obtaining in material with corresponding solvent, though existing extensive application in field of traditional Chinese medicine pharmacy equally also has application in as other association area of food, spices, essence.Taking field of traditional Chinese medicine pharmacy as example, multi-function extractor is a kind of pressure vessel type Chinese medicine extractor being widely used at present, and maximum volume can reach 10m3.Although to the existing many improved reports of this kind equipment, some of its existence can directly affect the fundamental issue of extraction efficiency and product quality, still fail all the time to solve:
One, multi-function extractor leads directly to steam and two kinds of modes of interlayer heating at the bottom of possessing tank, because interlayer heating surface (area) (HS is less, the thermal efficiency is low, it is inhomogeneous to conduct heat, so the decocting of medicinal material is boiled or the process such as steam distillation in, routine operation mainly relies on by directly passing into industrial steam at the bottom of tank and is rapidly heated and makes material boiling, and chuck heating is only played auxiliary heating and kept backflow effect.Because be subject to the impact of the factor such as antiscale chemical treatment and the corrosion of conveyance conduit of boiler feed water, industrial steam is not clean steam, so straight-through industrial steam itself has just caused the pollution to liquid, does not therefore meet the principle that GMP specifies.If adopt organic solvent to extract medicinal material, can not use straight-through steam, can only lean on interlayer heating, material boiling is needed for a long time.
Its two, the medicinal material extract mode taking water as solvent generally adopt decoct reflux.It has been generally acknowledged that material can ensure higher leaching temperature under fluidized state, can make again its solid liquid interface produce convection current, can accelerate leaching velocity.But the essence of boiling is that the strong movements of hydrone can impel the materials such as medicinal material to expand, collide, rub and fragmentation, and discharges a large amount of impurity in the phenomenon of liquid internal and the simultaneous violent vaporization in surface.Particularly for many extractions containing baregin and the more medicinal material of starchiness, boiling effect and straight-through steam are very disadvantageous, the impurity component of a large amount of fragmentations, peptization and gelatinization obviously strengthens the viscosity of liquid, turbidity, not only reduce the quality of leachate, also greatly increased difficulty and the cost of leaching thing Separation of Solid and Liquid.
They are three years old, current multifunctional extracting pot only below cleanout door is provided with the filtration for separating of exudate, its area is limited, therefore being easy to be seethed with excitement for a long time because of above-mentioned warp decoction causes the stickum such as fine powder, fiber and peptization, gelatinization excessively discharging to stop up, cause the isolated by filtration difficulty of leaching liquid, even residual large medicine amount liquid cannot be collected.Even if adopt the operation of pump forced circulation, also easily cause circulation not smooth, even stop up and cycle interruption phenomenon.This is the hard nut to crack existing in many decocting for Chinese herbal medicine leaching process.
The 4th, while adopting multifunctional extracting pot to carry out the volatile oil component in steam distillation operation collection medicinal material, the above-mentioned mode by straight-through industrial steam ebuillition of heated at the bottom of tank of conventional employing is carried out, not only liquid and distillate can be contaminated, because can body is higher, internal diameter and the disengagement area of tank are less, and the thickness that medicinal material is loaded and packing can serious hinder water vapour and the volatile oil steam speed seeing through that rises, and have affected the efficiency of steam distillation.If medicinal material is heated for a long time, the oxidation of some composition and hydrolysis are difficult to avoid, and also can have influence on the quality of collecting liquid.
Traditional Chinese medicine extraction is most important link in most Chinese medicine preparations, and exhausted major part in traditional Chinese medicinal material raw materials is all the impurity component being of no curative effect, and the relative amount of active principle is generally all very low.Advanced extractive technique should guarantee to extract to greatest extent active principle, reducing as far as possible impurity component proposes, on the one hand to ensure and to improve quality and the curative effect of Chinese medicine preparation, also can greatly reduce difficulty and the cost of follow-up separation, removal of impurities and purification operations simultaneously, particularly particularly important especially for the production of traditional medicine Injectio.
Except field of traditional Chinese medicine pharmacy, need to carry out in other field of material extraction, the problems referred to above also exist to some extent.
Summary of the invention
In view of above problem, the invention provides the material extraction element of a kind of brand new form and operation principle, can high efficiency, complete in high quality the extraction of material component, of many uses, and be specially adapted to suitability for industrialized production.
The basic structure of material extraction element of the present invention, includes and is vertically set up in parallel and the material leaching unit being made up of leaching container being interconnected and the liquid-heating unit being made up of heat exchanger.Wherein:
---the top of material leaching container is provided with charge door, solvent adds entrance, visor, cooling collector unit and condensing reflux unit, and below is provided with filter element and the cleanout door of leaching liquid;
---between the filter element and the below of heat exchanger of material leaching container below, through leaching liquid Natural Circulation passage or the leaching liquid forced circulation channel connection that can select to switch, in leaching liquid Natural Circulation passage, be provided with the first control valve, in leaching liquid forced circulation passage, be provided with successively liquor charging valve, piping filter, liquid delivery pump and the second control valve.Wherein piping filter is preferably the many bag filters that are applicable to large flow.Top at piping filter is provided with exhaust-valve, and the outlet of liquid delivery pump is also provided with bleeder valve;
---leach on the sidewall at position, operating fluid level (being the leaching liquid liquid level while making whole material submergence under normal operating conditions) top of container at material, be provided with the leaching liquid circulation backward channel import being connected with the leaching liquid loop exit of heat exchanger top.Wherein, the optimal way of said this leaching liquid circulation backward channel import, is to make the periphery tangential direction setting of its direction along wall material leaching container.
Generally, cooling collector unit and the condensing reflux unit of said material leaching container top in said apparatus, can be included in be not limited to be provided be linked in sequence every foam device, condenser, cooler, oil water separator, wherein above the side of oil water separator, be provided with separating valve.
Groundwork process and the principle of said extracted device of the present invention are: in the time making water (or organic solvent) carry out material extraction operation, first open and regulate leaching liquid forced circulation passage, and heat exchanger steam valve, the liquid of leaching container below is promoted to heat rapidly through heat exchanger by liquid delivery pump after filtering, and then return to leaching container by top, forced circulation heating so repeatedly, can make the fluid temperature leaching in container evenly increase, and approach very soon boiling temperature, now close forced circulation passage, open and regulate Natural Circulation passage and heat exchanger steam valve, the liquid of preheating can fast boiling in heat exchanger, due to the density contrast of liquid and the promotion of the climbing power of indirect steam, liquid is upwards flowed, and return to leaching container by top, thereby realize the Natural Circulation of leaching liquid.Experimental result demonstration, an outstanding feature of this cyclic process, is without increasing extra power again.The vapour-liquid that enters leaching container separates in the superjacent air space of container, steam returns to leaching container through the condensing reflux unit of top, the liquid of boiling temperature moves downward in leaching container, Natural Circulation so repeatedly, high-temp liquid (boiling point or approach boiling temperature) can be accelerated the leaching rate of material and leach balance under dynamic condition undoubtedly.
Test and also show, this initial forced circulation process is also of value to leaching container filtration surface and forms good filtering layer, is beneficial to follow-up simple and direct Natural Circulation process.
Equally, the dynamic circulation of high-temperature water solution is also conducive to diffusion, the emulsification and miscible in leaching liquid of volatile oil component in material.Adopt said process to enter high temperature leaching liquid fast boiling vaporization in heat exchanger of Natural Circulation, water vapour and volatile oil steam together steam, promote liquid and return to leaching container by top, the leaching that circulates downwards of the liquid of boiling temperature, and water vapour and volatile oil steam are through the cooling collector unit of container top, in oil water separator, collect and separate, can obtain material volatile oil component.Based on this new distillation mode of steam distillation principle, because its evaporation process is not subject to the impact of medicinal material thickness and density, the thermal distillation mode that adds of more traditional straight-through industrial steam, decapacitation ensures that outside the quality of distillate, experimental result also shows that its efficiency is higher.
Therefore, the above-mentioned material extraction element of the present invention has been avoided mode and the impact thereof of traditional straight-through industrial steam completely, what adopt is efficient external heating mode, to leach container separates with heating arrangement, leaching and the heating of high-temp liquid to material separately carried out, in closed system by rationally regulating control valve in circulation canal and/or the steam valve of heat exchanger, can effectively control liquid preheating speed, and the speed of liquid boiling evaporation, thereby realize the solvent extraction to material and steam distillation operation under Natural Circulation state of dissimilar/character.By making full use of the conversion of vaporizing liquid energy, make the high-temp liquid that reaches boiling point or approach boiling temperature, the material of relative static conditions is carried out to Dynamic Extraction operation, avoid straight-through steam and decocted the phenomenons such as boiling effect the material fragmentation, peptization and the gelatinization that cause, not only efficiency is high, quality is good, and has solved the problem of extracting liquid filtering difficulty.
On the basis of the above-mentioned material extraction element of the present invention, further can also adopt following corrective measure separately or in the mode of any combination:
Material leaching container in above-mentioned material extraction element, though without particular limitation of the general pressure vessel without adopting current multifunctional extracting pot form, can be adopted as the non-pressure vessel that is provided with thermal insulation layer.With traditional multifunctional extracting pot comparison, the manufacture difficulty of vessels not under pressure and cost can greatly reduce undoubtedly, and selectively larger on Mechanical Builds, are more conducive to the extraction operation of material.
The leaching liquid filter element of said material leaching container below, except include that traditional approach is arranged on the orifice plate filter net type bottom filtering structure on cleanout door and the bottom filtrate collection structure and bottom filtrate (liquid of answering in contrast, be also provided with ring-type perisporium filtration and the perisporium filtrate collection structure of answering in contrast and the perisporium filtrate (liquid of the board-like or orifice plate filter net type of annular aperture along the below inwall setting of material leaching container.
The inwall of material leaching container, at least in the lower ring frustum type structure that can be set to have downward contracted diameter, the said perisporium filtration ring-type filtration that the bottom perisporium of leaching container upwards continues of serving as reasons.The height of said this ring frustum type structure, can be according to the in the light of actual conditions appropriate design of capacity of leaching container, can be only for example in the regional area of leaching container near bottom, or extend to the central region of leaching container height, even can also further upwards extend.The extended height of said perisporium filtration, equally also can only be confined in the perisporium region at this ring frustum type structure place, or further extends upwardly in the position (being generally cylindrical tube shape region) on ring frustum type structural region.Obviously, arrange after this ring-type perisporium filtration, can make filter area be several times as much as the single filtration area on cleanout door of tradition.So the combination of filter element, can make the filter effect of leaching liquid be greatly improved, and has increased filtyration velocity and the flow of leachate, has fully ensured the mass-and heat-transfer process of leaching liquid high-efficiency dynamic circulation.
In said material leaching container, adapting with operating fluid level and not higher than the position of this operating fluid level, the highest can be contour but be preferably the position a little less than this operating fluid level with this operating fluid level, be also provided with the horizontal barrier structure with liquid flow hole gap.This horizontal barrier structure not only can play the effect that indicates and observe minimum operating fluid level, particularly in wet distillation process, liquid in leaching container can reduce gradually, need moisturizing to maintain liquid level, ensure normal Natural Circulation still-process, can also stop proportion whole gears are pressed in below liquid level compared with light material is floating simultaneously, are beneficial to sufficient leaching.In addition, in the cyclic process of leaching liquid, this horizontal barrier structure can also play the effect of current-sharing, and prevents the impact of circulation fluid to upper materials, to cause the phenomenons such as fragmentation, peptization and gelatinization.
This horizontal barrier structure in above-mentioned material leaching container, preferred mode is to adopt by the hinged two semicircular orifice plate arranging along diameter, particularly at least corresponding with charge door lower position half circular hole slab can be the upwards portable plate of turnover, the operation of both can conveniently having fed in raw material.
Said heat exchanger, is preferably one way vertical array tubular heat exchanger, and to make its tube side be leaching liquid passage, and the shell side that is provided with multiple hydraulic barriers is heating steam passage.Tubular heat exchanger simple in structure, heat transfer efficiency is high, and disposal ability is large, is heating and evaporative applications heat exchanger the most widely in producing at present.According to capacity and the height of material leaching container, select corresponding tubular heat exchanger.
For ensureing and promoting leaching liquid to return to as early as possible leaching container through said circulation canal above by heat exchanger in Natural Circulation process, avoid and reduce the delay of circulation fluid on heat exchanger upper perforated plate and produce resistance, upper perforated plate in said tubular heat exchanger, be preferably the lower edge that adapts with the position of leaching liquid loop exit and be not less than leaching liquid loop exit, more preferably adopt a little more than the mode on edge under this leaching liquid loop exit and arrange.
Be appreciated that thus, the structure of the above-mentioned material extraction element of the present invention and the course of work and principle, all be different from essence the multifunctional extracting pot of current traditional form, adopt the natural circulation mode of efficient external heat, and greatly improve and strengthened the leaching process of mass-and heat-transfer, significantly improve the leaching rate of active principle, not only avoid the use of straight-through industrial steam, also overcome the fragmentation in various degree of many materials that traditional decoction boiling mode causes, the problem such as peptization and gelatinization, reduce the leaching of impurity, obviously reduce the difficulty of later separation and refinement treatment, fully ensure product quality.This device science is simple and direct, energy-efficient, can be widely used in the different field including herbal pharmaceutical, is particularly suitable for those extraction and steam distillation operations containing baregin, the more material of starchiness.
Brief description of the drawings
Fig. 1 is a kind of structural representation of material extraction element structure of the present invention.
Detailed description of the invention
Material extraction element of the present invention as shown in the figure, include the material by the normal pressure right cone type leaching can form with thermal insulation layer 9 being vertically set up in parallel and leach the material leaching unit that container 10 forms, and the liquid-heating unit being formed by the one way vertical array tubular heat exchanger 27 of commonly using, in tubular heat exchanger 27, be provided with several shell side hydraulic barriers 26 with interlace mode.The top of leaching container 10 is provided with charge door 32, solvent adds entrance 33, visor 6, cooling collector unit and condensing reflux unit.The position a little less than normal operating fluid level height in leaching container 10, be provided with the board-like horizontal barrier structure 7 of two semi-circular hole that one deck connects via the hinge 8 along diameter setting, wherein the semicircle orifice plate corresponding with charge door 32 positions can upwards turn down, leaching container 10 wall portions above horizontal barrier structure 7, to be provided with leaching liquid circulation backward channel import 31 along tangent to periphery direction.
Above leaching container 10, be sequentially with in the usual way the cooling collector unit and the condensing reflux unit that comprise every compositions such as foam device 34, condenser 1, cooler 2, oil water separators 3.Wherein, side be provided with separating valve 4 above oil water separator 3.Between oil water separator 3 and leaching container 10, be provided with and regulate the return valve 5 of controlling capacity of returns.
The cleanout door 17 being operated by opening/closing control structure is arranged at the bottom of leaching container 10, is provided with the pot bottom filtration 14 of orifice plate filter net type, pot bottom filtrate collection structure 15 and the pot bottom filtrate (liquid 16 of answering in contrast on it; Also be provided with the ring taper that upwards continued by bottom perisporium and suitably orifice plate filter net type perisporium filtration 12, the corresponding sandwich-type ring-type perisporium filtrate collection chamber 11 of the cylinder shape of height in container 10 in leaching, and be provided with perisporium filtrate (liquid 13 at its lowest order.Leaching liquid after filtration is after filtrate (liquid at the bottom of tank 16 and 13 merging of perisporium filtrate (liquid, enter the leaching liquid Natural Circulation passage pipeline with the first control valve 24 of changeable selection, or enter the leaching liquid forced circulation passage pipeline that is provided with liquor charging valve 19, piping filter 20, liquid delivery pump 21 and the second control valve 23, enter liquid-heating unit by the inlet 25 of tubular heat exchanger 27.Be provided with exhaust-valve 18 at piping filter top; Exit at liquid delivery pump 21 is also provided with bleeder valve 22.
In liquid-heating unit, the shell side of tubular heat exchanger 27 is the heating steam of sending into through steam valve 28; The circulation leaching liquid of being sent into by the inlet 25 of its below, after tube side is heated, is sent through the vapour-liquid outlet 30 of tubular heat exchanger top, and the vapour-liquid import 31 corresponding with leaching container 10 tops connects returns to leaching container 10.Wherein, the upper perforated plate 29 of tubular heat exchanger 27 should be a little more than the lower edge of leaching liquid loop exit 30.
Liquid in material leaching container 10 is except need to circulating by the forced circulation passage pipeline being driven by liquid delivery pump 21 in the initial rapidly pre-warming stage, when being preheated to while approaching boiling temperature, liquid can close this forced circulation pipeline, steam regulation valve 28, open leaching liquid Natural Circulation passage pipeline by the first control valve 24, leaching liquid enters the high temperature leaching process of Natural Circulation, and the steam of generation can return to leaching container 10 through return valve 5 by condensing reflux unit.
In the time that leaching liquid enters high temperature Natural Circulation, the steam (gas) producing is by the cooling collector unit of leaching container 10 tops, regulate the separating valve 4 on return valve 5 and oil water separator 3, can carry out steam distillation operation, the volatile oil component in separated and collected material.
extract embodiment 1
Steam distillation to Fructus Schisandrae Chinensis volatile oil composition and the extraction of water soluble ingredient.
Operation 1: with multifunctional extracting pot, adopt routine to carry out steam distillation by straight-through steam at the bottom of tank and collect volatile oil component.After steam distillation finishes, broken serious due to the fruit of Chinese magnoliavine, material becomes " a pot of porridge " phenomenon, is difficult to separate, and extracts water soluble ingredient as boiling again, and it will be very difficult that the filtration of liquid is collected.For this reason, have the mode that the fruit of Chinese magnoliavine is packed as to many pouches to operate, its result had both been unfavorable for the leaching of material, also can the impacts such as material contamination liquid for marsupial, and both bothersome also science not.
Operation 2: the extraction element that adopts said structure of the present invention, control forced circulation is rapidly heated, regulate the evaporation rate of Natural Circulation, can ensure the abundant steam distillation of Fructus Schisandrae Chinensis volatile oil composition and collect until odorlessness, it is still complete that distillation finishes rear configuration of medicinal materials, fruit of Chinese magnoliavine extreme expansion is not but broken, and liquid very easily separates.Continue water high temperature Natural Circulation again and extract twice, liquid filters collects same being very easy to, and the turbidity of extract is lower, and in extract, the schizandrin content as index conforms with the regulations completely.
extract embodiment 2
90% alcohol extract of medicinal material red ginseng (infiltrating section).
Operation 1: adopt multifunctional extracting pot routine operation, add 90% alcohol reflux of 4 times of amounts of red ginseng to extract at every turn 2 hours, extract altogether 5 times, collect extract.Because solvent is ethanol, can only lean on interlayer heating to carry out, the time that is heated to boiling is long.In actual production, completing the extraction of 300kg red ginseng with 2m3 multifunctional extracting pot needs 16 hours, and the rate of transform of the active principle ginsenoside of extract is 70% ~ 75%.
Operation 2: adopt the extraction element of said structure of the present invention, the consumption of 90% ethanol and extraction time biconditional operation 1, regulate and control high efficiency forced circulation warm and high temperature Natural Circulation leaching process.After measured, keep the Natural Circulation of larger flow, extract at every turn and can reach leaching balance in 1 hour.Therefore within 8 hours, can complete extraction operation.Precipitate after extract refrigeration is less, the rate of transform >=75% of active principle ginsenoside.
Contrast is extracted operating result and is shown, compare with extracting mode with traditional extraction equipment, material extraction element of the present invention can effectively solve the series of problems existing in current production, can ensure that leaching process is meticulousr, and efficiency is higher.

Claims (9)

1. material extraction element, is characterized in that comprising the material being made up of material leaching container (10) the leaching unit being vertically set up in parallel and be interconnected and the liquid-heating unit being made up of heat exchanger (27), wherein:
---material leaching container (10) is for being provided with the non-pressure vessel of thermal insulation layer (9), its top is provided with charge door (32), solvent adds entrance (33), visor (6), cooling collector unit and condensing reflux unit, below is provided with filter element and the cleanout door (17) of leaching liquid
---between the filter element and the below of heat exchanger (27) of material leaching container (10) below, through leaching liquid Natural Circulation passage and the leaching liquid forced circulation channel connection that can select to switch, in leaching liquid Natural Circulation passage, be provided with the first control valve (24), in leaching liquid forced circulation passage, be provided with successively liquor charging valve (19), piping filter (20), liquid delivery pump (21) and the second control valve (23)
---on the sidewall at position above the operating fluid level of material leaching container (10), be provided with the leaching liquid circulation backward channel import (31) being connected with the leaching liquid loop exit (30) of heat exchanger (27) top.
2. material extraction element as claimed in claim 1, is characterized in that the leaching liquid loop exit (30) of said heat exchanger (27) top and material leach the direction of the leaching liquid circulation backward channel import (31) between the corresponding site sidewall of container (10) operating fluid level top along the periphery tangential direction setting of wall material leaching container (10).
3. material extraction element as claimed in claim 1, it is characterized in that including in the cooling collector unit of material leaching container (10) top and condensation recovery unit be linked in sequence every foam device (34), condenser (1), cooler (2), oil water separator (3), be provided with separating valve (4) in the top, side of oil water separator (3).
4. material extraction element as claimed in claim 1, is characterized in that comprising at the leaching liquid filter element of said material leaching container (10) below:
---be arranged on the orifice plate filter net type bottom filtering structure (14) on cleanout door (17) and the bottom filtrate collection structure (15) of answering in contrast and bottom filtrate (liquid (16);
---ring-type perisporium filtration (12) and the perisporium filtrate collection structure (11) of answering in contrast and the perisporium filtrate (liquid (13) of the board-like or orifice plate filter net type of the annular aperture that arranges along material leaching container (10) below inwall.
5. material extraction element as claimed in claim 4, the inwall that it is characterized in that material leaching container (10) at least below be the ring frustum structure with downward contracted diameter, the ring-type filtration of said perisporium filtration (12) for upwards being continued by the bottom perisporium of material leaching container (10).
6. material extraction element as claimed in claim 1, is characterized in that adapting with operating fluid level and not higher than the position of this operating fluid level, being provided with the horizontal barrier structure (7) with liquid flow hole gap in said material leaching container (10).
7. material extraction element as claimed in claim 6, the two semicircular orifice plate that it is characterized in that serving as reasons horizontal barrier structure (7) in said material leaching container (10) hinge (8) that arranges along diameter connects, and at least corresponding with charge door (32) lower position half circular hole slab is the portable plate that can upwards turn down.
8. material extraction element as claimed in claim 1, is characterized in that said heat exchanger (27) is one way vertical array tubular heat exchanger, and its tube side is leaching liquid passage, and shell side is heating steam passage.
9. material extraction element as claimed in claim 8, is characterized in that the upper perforated plate (29) of said heat exchanger (27) and the position of leaching liquid loop exit (30) adapt and be not less than the lower edge of leaching liquid loop exit (30).
CN201210121714.9A 2012-04-24 2012-04-24 Material extraction device Expired - Fee Related CN102614682B (en)

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