AT523275A4 - System for a mobile extraction - Google Patents

Abstract

The invention relates to a new system for the extraction of an extractable valuable substance (ES) from a solid material (FS) containing the same by means of conditioned solvents (LM) circulated several times and is characterized in that the extraction container (10) is connected to an extraction solvent (LM) loadable pressure vessel (2) with base base (12), with the outer wall cylinder (11) and central inner wall cylinder (13) connected to it, - in which container (10) one from the base base (12) and with an inlet filter element (14 ) formed solvent / liquid extract inlet space (15) is formed, - that within the extraction container base body (10) - an extraction chamber cover (16) connected to an overlay tube (19) is arranged, which is linearly displaceable in the extraction container, - with which a displaceable outlet filter element ( 17) is connected, whereby a liquid extract outlet space (16) is formed, - that between Ein Run (14) - and outlet filter element extraction material can be arranged and the solvent can flow through it and the liquid extract (FE) loaded with the extract substance (ES) from the outlet space (16) through the between the inner wall cylinder (13) and the one with the lid (16) connected overpipe (19) existing, narrow approximately annular cross-section having intermediate space (110) can be introduced into the outlet pipe (AR) opening into the pressure vessel (2).

Description

containing solid material.

A large number of extraction processes and systems for the extraction of the most varied of substances in the most varied of aggregate states from liquids and solid materials have become known, which here, in particular with regard to the

Extraction of solids, only briefly mentioned:

For example, the so-called Soxhlet extraction process has long been known from the laboratory sector, in which a solvent or extractant is evaporated from a solvent sump, condensed on a cooler and from there onto a comminuted solid containing extract material in a filter sleeve

drips, collects there and leaches the extract substance from the solid.

A major disadvantage of this process is, among other things, that the solvent condensed on the cooler is at a low temperature and therefore that for the extraction

required time is high.

On an industrial scale, extractions are carried out by means of extractors, a layer of the solid material to be extracted being arranged in a container essentially equipped with an inlet and outlet between two sieve plates or the like and the solvent, optionally in the heated state and under increased pressure

Cycle is carried out through said solid layer.

Especially recently, an extraction technique has been used which works with inert gases such as CO, which are in the so-called "supercritical" state,

enforced. These extraction processes are very selective and effective and have the

left behind, which is important for the food industry, for example.

As for the extraction processes as well as the extract substances and those containing them

Concerning solid materials, some examples are given below:

- Extraction of pharmaceutical raw materials such as leaf, bark, root, seed and flower drugs from the corresponding parts of the plant.

- In the case of polymers, catalysts and impurities can be washed out.

- Furthermore, valuable substances bound to adsorbents such as activated carbon can be recovered or pollutants adsorbed there can be removed from the adsorbent.

- Extraction of oil seeds, spices and / or smells and flavors, as well as biocidal or insecticidal substances from plant materials.

- Extraction of bones to obtain gelatin and animal waste to obtain fats.

- Extraction of dyes from materials containing them.

- Extraction of metals or metal compounds from rocks.

The extraction process can be based on various basic processes, such as the transfer of the extract substance into the solvent by diffusion, separation of the extract (miscella) from the residue (raffinate), by settling or filtering and expelling the extract still remaining in the residue by heating with

Steam, washing and / or squeezing.

An important process step is the separation of the extraction substance from the solvent: This is usually done by distillation or, nowadays, by means of

Membrane processes.

Success of every extraction process.

The smaller the particles, the larger the diffusion surface between the solvent and the solid. If the particle size is too small, the free circulation of the solvent through the solid can be hindered, e.g. by clumping. Such fine, non-percolation-able extraction material is beneficial for an extraction with a

coarse-grained, inert carrier material mixed.

For the extraction time until the extract substance concentration is equalized, there is an approximately quadratic dependence on the mean capillary length in the to be extracted

Solid material. A uniform particle size is beneficial.

The water content of the extraction material should be as low as possible when using hydrophobic solvents. If it is high, the extraction favorably becomes a drying step

upstream.

The solvent should have a low viscosity, selective dissolving power for the extract, narrow boiling limits and a low boiling point or a low one

Have enthalpy of vaporization.

The extraction rate increases in the course of each, preferably carried out in a cycle,

Extraction process, as the concentration gradient decreases.

The solubility and thus the extraction rate usually increases with increasing temperature. However, the ability to dissolve impurities also increases and

some extract substances decompose if the extraction temperatures are too high.

which part counts as "bound solution".

Conventional solids extractors work as discontinuous or semicontinuous or semi-continuous, or continuously operating systems, which, like the known ones

different extractor designs are not dealt with in detail here.

Briefly mentioned is the swiveling extractor known from AT 371716 B for leaching roots or herbs by means of a solvent, which has a closable opening for the removal of what has been dissolved out with it

Extract laden solvent containing container is formed.

From AT 411 154 B a method and a system for the extraction of solid materials are known, in the course of which the solvent is moved through a layer of solid material arranged in the extractor between the sieve plates and the extract laden with the extract material discharged from the extractor. with extract

loaded solvent is collected.

The present invention relates to a new system for an extraction of at least one extractable valuable substance from at least one preferably comminuted solid material containing the same, preferably comminuted, by means of, preferably in a range between -40 and + 140 ° C, movable with normal, over or under pressure, in particular in a range between -40 and + 140 ° C repeated circulating, appropriately conditioned solvent in the liquid phase, which through extractor between a fixed and a movable one

and a layer of the sieve provided for pressing out the extracted solids

- that the extraction container provided for the extraction can be connected in a pressure-tight manner, for example by means of a bayonet quick-release lock, to the opening on the top of a pressure container that can be charged with the extraction solvent,

- that the same is formed with an annular cross-section, with a base base on the underside, with the same connected, protruding outer wall cylinder and the same central, upwardly protruding inner wall cylinder forming a liquid extract overflow or outlet pipe opening into the pressure vessel,

- in which a close-meshed inlet filter element (mesh / sieve / filter) formed by a solvent / liquid extract inlet chamber (mesh / sieve / filter) is formed from the base base and with an upwardly liquid-permeable, upwardly liquid-permeable, narrow-meshed inlet filter element (mesh / sieve / filter),

- into which the feed line for solvent or liquid extract from the pressure vessel opens,

- that within the extraction container base body - at a distance from the base bottom towards the top - an extraction chamber cover is arranged, which is connected to an upwardly protruding, preferably closed, overlapping tube and which seals itself against the outer wall cylinder and against the inner wall cylinder and which is linear in the extraction container base body is movable

- with which a narrow-pore or -meshed liquid-permeable flow-through filter element, which is arranged at a distance from the same and linearly displaceable with it and also covers a ring cross-section, is connected, whereby a liquid extract discharge space is formed between the cover and the filter element,

- That in the extraction space between the inlet and outlet filter organ that of the

Extraction to —subject to solid material can be arranged and from the

can be brought in.

Since at least residues of extract material remain in and on the solid to be extracted when the concentration equilibrium is reached, it is advantageous to achieve the best possible recovery of valuable material if the cover with the filter element in the outer wall cylinder is mechanically or pneumatically, in particular by means of Compressed air, is displaceable while compressing the solid to be extracted, with solvent, in particular residual extract substance still adhering to the solid, flowing through the solid

containing liquid extract can be obtained.

A design of the system according to the invention has proven to be favorable in which the solvent enters the pressure vessel from above into the space above the

Solvent-liquid extract level can be introduced.

In order to essentially switch off the entry of disruptive atmospheric oxygen into the extraction process, it is advantageous if the pressure vessel containing the solvent or the liquid extract formed with the same and containing the extracted substance is also provided

an inert gas, in particular with CO- ,, can be charged.

In order to be able to design the extraction process as flexibly as possible, one is for its

Implementation to give preference to the installation of a pressure vessel with a

7720

Is provided.

Last but not least, an extraction system according to the invention is to be preferred, in particular due to its uncomplicated clear structure, in which it is provided that the liquid extract that has accumulated or has accumulated in the pressure vessel and loaded with the substance or extract substance to be extracted is preferably in each case after completion of the extraction process can be fed to a heat / cold exchanger via a discharge line equipped with a pump on the underside of the pressure vessel, and the liquid extract conditioned there can be fed via a line to a separator, where the extracted valuable substance or extract substance is separated from the solvent which has been converted into the gaseous state there , from where the solvent gas can be transferred to a condensing device via a conduit with a vapor evaporator and from there in re-liquefied form as a solvent or distillate enters the distillate tank and is pressurized via a line with a pump container

is traceable.

Such an overall system has proven particularly useful for trial extractions to be carried out with new plant material or plant material that has not been used up to now, in which

high flexibility of the process control parameters is required, proved to be suitable.

Unexpectedly, the first attempts even prove the suitability of the new extraction system

for brewing beer.

The invention is explained in more detail with the aid of the drawing:

1 and 2 each show sectional views of the extraction vessel and FIG. 3

an entire extraction plant according to the invention:

Solvent LM and CO », in the pressure vessel 2.

An essential part of the extraction vessel 10 is ultimately formed by a base body 10 formed with the outer wall cylinder 11, the fixed base base 12 and the inner wall cylinder 13, which also serves as an outlet pipe AR

annular cross-section.

At a distance upwards from the base base 12 - keeping the solvent / liquid extract inlet space 15 free - the inlet filter element 14 covering the ring cross-section, with a mesh or pore size tailored to the structure, texture, grain size, fibrous structure or the like of the material to be extracted, in which inlet chamber 15 the supply line 25 for fresh solvent LM or, for example, circulated

Liquid extract FE containing extract substance ES opens.

The top cover 16, which in turn rests linearly inside the outer wall cylinder 11 or the base body 10 of the extraction vessel 1, is sealingly adjacent to the outer wall cylinder 11 and is connected to an overlapping cylinder 19 that is slipped over the inner wall cylinder 13 and is closed on the top

and from can be moved.

Connected to the cover 16 and therefore linearly displaceable with it is the outlet filter element, which is also arranged at a distance from it and also has an annular cross-section, that is to say the net, sieve, filter 18. Between the cover 16 and the filter element is the

Solvent / liquid extract outlet space is formed, which extends upwards into the

or outlet pipe AR and pull-over cylinder 19 continues.

The actual extraction space is located between the two filter elements 14 and 18

ER, which can be charged with the solid FS to be extracted.

The solvent LM, which is usually pumped under pressure into the stationary inlet chamber 15 of the extraction vessel 10 via the line 25, or the liquid extract FE loaded with the valuable substance to be extracted, i.e. extract substance ES, passes through the meshes, filter pores or the like of the filter element 14 In the material to be extracted, i.e. in the solid FS, the extract substance ES elutes from the same and there forms the liquid extract FE, which flows through the filter element 18 into the outlet space 17 and from there through the annular space Z as described above to the upper free end or edge of the inner wall cylinder 13 arrives and flows from there with reversal of direction into the outlet pipe AR and downwards into the pressure vessel 2, from which it is, for example, after the end of the extraction process in the further processing and

Obtaining the valuable substance to be extracted, i.e. extract substance ES, is promoted.

To avoid loss of extract material ES, it is provided that after the so-called "state of equilibrium" has been reached, the cover 16 and with it the outlet space 17 and the filter element 18 under mechanical loading or by pumping in compressed air 105 into the space 102 between the extractor cover ED and the outlet space cover 16 under pneumatic pressurization by increasing compression of the solid FS, preferably with solvent, the solid FS, flowing through it

Liquid extract FE adhering or still present in the solid is obtained.

If the meanings of the reference symbols otherwise remain the same, FIG. 2 shows on the basis of a

split sectional drawing shows the position of the individual components of the new Appendix 1 in

two different operating states, namely left half before or at the beginning and

during the extraction process and right to the end of the same.

On the left-hand side it can be seen that the interior of the extraction vessel 10 is completely closed

extracting solid FS, e.g. herbs.

Via line 25 first pure solvent LM, then optionally liquid extract FE, enters the solvent-liquid extract inlet space 15 between the base plate 12 and the filter element 14, flows through the solid FS, takes up extract ES there and becomes the liquid extract FE, passes through the upper one The filter element 18 reaches the outlet space 17 and flows into the space formed by the inner cylinder 13

Outlet pipe AR and finally into the pressure vessel 2.

On the right-hand side is the position of the downwardly shifted lid 16 with sieve 18 at the end of the extraction process - possibly during the extraction process, the solid FS now being compressed and still being flowed through by the solvent LM, which is loaded with the remaining extract substance ES as "thin "Liquid extract FE flows through the space Z, shown with thick lines, between the overlapping tube 19 and the outlet tube 13, which is also displaced with the cover 16

and ultimately passes through the outlet pipe 13 into the pressure vessel 2.

In Fig. 3 - with otherwise identical meanings of the reference symbols - the entire

Extraction process shown:

The liquid extract FE formed with the extract ES contained in the solvent LM passes by means of pump P2 and through line 23 into the heat exchanger 3, where it is heated and from there through line 34 into the separator 4, in which the separation of the extract ES from the im Put heat exchanger 3 in the gaseous state

Solvent LMg takes place.

The extract substance ES collects at the bottom of the separator 4 and can from there

subtracted from.

The gaseous solvent LMg passes through the line 45 and via the vapor evaporator Bv into the upper condensing part 5 of the distillate or solvent container 6, is liquefied there and collects as pure solvent LM in the lower part of the distillate container 6, from where it is pumped P3 via line 61 back into the

Pressure vessel 2 is returned.

For the real practice of the extraction process as a whole, it should be added or concluded

with reference to FIGS. 1 to 3, the following is explained in an explanatory manner:

The extraction system 1 according to the invention is a system which can be operated, for example, with butane, ethanol and many other explosive and non-explosive solvents LM. The extraction can be carried out at temperatures from + 120 ° C to -40 ° C

operate. The possible operating pressure of system 1 is -1 to + 20bar.

The extractor 1 or the extraction vessel 10 is located on, for example, a 5 liter pressure vessel 2 and is preferably tightly connected to the solvent-liquid extract container 12 by means of a bayonet lock or the like. The extractor 10 consists of a 0.5 liter container with a fixed bottom sieve 14, under which the inlet space 15 is located, into which the solvent LM or the extractant-laden solvent FE is pumped. In the middle of the extractor 10 is the overflow or outlet pipe 13. A plate with a sieve or the like, which is attached to the overflow or outflow pipe 13 and seals against the inner wall, prevents the extraction material, i.e. solid FS , e.g. herbs get into the outlet pipe. The raw materials FS to be extracted are poured into the space between the lower 14 and the upper sieve 18. An overall cover is screwed onto the jacket tube 11 or extraction vessel 10 at the top.

The sliding cover 16 seals on the one hand on the jacket tube 11 and on the other hand in the

Middle to the middle tube 13. The protruding overlay tube 19 is with the movable

upper screen 18 or cover 16 connected and vertically linearly displaceable with it.

The solvent, e.g. ethanol, butane, etc. is pumped into the pressure vessel 2 by means of pump P3. By means of the pump P1, the solvent LM is pumped from below via the "lower" bottom sieve 14 upwards through the material to be extracted (herb-solid) ES and then flows through the upper sieve 18 and ultimately over the

the upper edge of the outlet pipe 13 back into the solvent pressure vessel 2.

The upper movable sieve 18 prevents the solid FS, e.g. herbs, from passing through

the outlet pipe AR = 13 drains or is flooded into the solvent container 2.

This cycle is repeated until the solvent LM has been enriched with the substances ES to be dissolved to such an extent that there is no more exchange, i.e. until an ES concentration equilibrium between solvent LM and solid FS is established

Has.

At the end of the extraction process, the upper movable sieve 18 - here by means of compressed air DL (vacuum pump outlet) - is pressurized up to 5 bar and thereby presses on the herbs FS to be extracted. The discharged loaded solvent or liquid extract FE from the herbs is into the solvent via the overflow pipe 13

LM or liquid extract FE receiving pressure vessel 2 passed.

The enriched solvent, i.e. liquid extract FE, is pumped via line 23

P2 is pumped through the heat exchanger 3 and heated there, for example.

The heated, loaded solvent EF is sprayed into the separator 4 via a reducing valve. The solvent of the liquid extract FE that is sprayed in in this way evaporates in the

Separator 4, is there converted into the gaseous state, and the dissolved

or extracted valuable substances or extract substances ES collect in the bottom area of the

Separator 4.

The now gaseous solvent LMg is passed via a vapor compressor (BV) into the cooler 5, where it condenses and in liquid form in the distillate container 6

is collected.

From the distillate container 6, the distilled, that is to say pure, solvent (LM) is pumped back into the solvent pressure container 2 from above by means of pump P2. The fresh solvent is reintegrated into the extraction cycle. This process is repeated until the herbs, ie the solid, no longer contains any soluble ingredients or the desired valuable substances ES from the in particular solid raw material FS

are detached.

At the end of the extraction process, the distillate is collected in the distillate container 6.

The collected distillate is used again in the next extraction process.

The process sequence can be controlled by means of a PLC control system, whereby the control system is set up in such a way that the user is able to use his / her own as favorable

To program processes.

Claims (6)

1. Plant for an extraction of at least one extractable valuable substance (ES) from at least one preferably comminuted solid material (FS) containing the same, preferably comminuted, by means of normal, positive or negative pressure, in particular in a range between -40 and + 140 ° C , preferably in a multiple cycle, appropriately conditioned solvent (LM) in the liquid phase, which moves or flows through the extractor between a stationary and a movable sieve provided for pressing extracted solids (FM) through a layer of the solid material (FS) to be extracted where the valuable material to be extracted or extracted, i.e. extract substance (ES), enriched or loaded or liquid extract (FE) can be further processed to obtain the extracted valuable material (ES), characterized, - That the extraction container (10) provided for the extraction can be connected in a pressure-tight manner, for example by means of a bayonet quick-release lock, to the opening (21) on the top of a pressure container (2) that can be charged with the extraction solvent (LM), - That the same with an annular cross-section (Qr) having, with a base bottom (12) on the underside, with the same connected, protruding outer wall cylinder (11) and the same central, a liquid extract (FE) opening into the pressure vessel (2) -over or . Outflow pipe (AR) forming, protruding inner wall cylinder (13) is formed, - in which a close-meshed inlet filter element (14) (mesh / sieve / filter) is formed from the base base (12) and with an upwardly liquid-permeable ring-cross-section-covering, spaced apart from the base base (12) Solvent / liquid extract inlet space (15) is formed, - that within the extraction container base body (10) - at a distance from the base bottom (12) towards the top - a tube (19) which projects upwards and which is preferably closed at the top, is connected, even against the outer wall cylinder (11) and against the inner wall cylinder ( 13) sealing extraction chamber lid (16) is arranged, which is linearly displaceable in the extraction container base body (10), - with which a narrow-pore or -meshed liquid-permeable outlet filter element (17), which is arranged at a distance from the same and can be linearly displaced with it and also covers an annular cross-section, is connected, whereby a liquid extract outlet space (16) is formed between the cover (16) and the filter element (17) is, - That in the extraction space (ER) between the inlet (14) - and the outlet filter element (18) the solid material (FS) to be subjected to the extraction can be arranged and the solvent / liquid extract (LF) can flow through it, and that with the extract substance to be obtained (ES) loaded liquid extract (FE) from the outlet space (16) through the existing between the inner wall cylinder (13) or overflow or outlet pipe (AR) and the cover (19) connected to the cover (16) and displaceable with it , narrow, approximately annular cross-section having interspace (110) in the space formed by the inner cylinder (13) of the extraction vessel base body (10), in the Pressure vessel (2) opening overflow or outlet pipe (AR) can be introduced. 2. Plant according to claim 1, characterized in that, in particular after reaching the concentration equilibrium between the concentrations of the extract substance in the solid to be extracted (FS) and in the liquid extract (FE), the cover (16) with the filter element (18) in the outer wall cylinder ( 11) against the base plate (12) mechanically or pneumatically, in particular with compressed air, below Compression of the solid to be extracted (FS) is displaceable, with under Liquid extract (FE) containing solid (FS) adhesive extractant (ES) can be obtained. 3. Plant according to claim 1 or 2, characterized in that the solvent (LM) from above into the pressure vessel (2) in the space above the solvent Liquid extract level can be introduced. 4. Plant according to one of claims 1 to 3, characterized in that, in particular to maintain the absence of atmospheric oxygen, the pressure vessel (2) with an inert gas, in particular with CO- ,, can be charged. 5. Plant according to one of claims 1 to 4, characterized in that the pressure vessel (2) with a device for heating and / or cooling the solvent (LM) or the liquid extract (FE) is equipped. 6. Plant according to one of claims 1 to 5, characterized in that preferably in each case after the end of the extraction process, the liquid extract (FE) that has accumulated or has accumulated in the pressure vessel (2) and loaded with the substance or extract substance (ES) to be extracted ) can be fed to a heat / cold exchanger via a discharge line (23) arranged on the underside of the pressure vessel (2) and equipped with a pump (P2), and the correspondingly conditioned liquid extract (FE) can be fed to the separator (4) via line (34), where the extracted valuable substance or extract substance (ES) is separated from the solvent (LMg) which has been put into the gaseous state there, from where the solvent gas can be guided into the condensing device (5) via line (45) with vapor evaporator (Bv) and from there in re-liquefied form as solvent (LM) or distillate enters the distillate container (6) and can be returned to the pressure vessel (2) via line (61) with pump (P3).