JPS5914243B2 - Method and apparatus for comminuting a mixture of substances and separating the components of the mixture - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for comminuting a mixture of substances, especially one consisting of plant products, and separating the components of the mixture by extraction.

By the term plant products, all products with solid and liquid components are to be understood. Generally, plant products are composed of small cells. In this case, each cell contains a liquid component, such as liquid juice or oil, inside. These liquid components are surrounded by cell walls. Examples of such plant products include, for example, seeds and fruits. The object of the invention is, on the one hand, to be able to simply and economically grind existing substance mixtures, i.e. in particular existing plant products, down to the ultimate cell- or liquid-containing substance particles and, on the other hand, to extract The objective was to find a method by which the components of a mixture could be separated.

This problem is solved according to the invention by exposing the mixture of substances to high pressure by supplying a compressed gas, and subsequently applying the compressed gas at a high velocity so that the components of the mixture of substances are ruptured by the pressure created in the mixture. Relieve the pressure by releasing it,
In order to separate the ground mixture components by extraction, the mixture components are converted into a neutral, non-healthy, supercritical gas, the substance to be extracted from the corresponding mixture component. The gas is subsequently depressurized to the subcritical range to separate the extracted material from the gas and to convert the gas back to the supercritical state and in the circulation system. solved by returning the substance mixture to be separated.

Advantageous embodiments of the method according to the invention are defined in the claims 2 to 3.
It is described in Section 11.

Furthermore, the invention relates to an apparatus for carrying out the method according to the invention.

The device of the invention comprises at least one pressure chamber for comminution of a substance mixture, a pressure relief chamber arranged below the pressure chamber, a blocking mechanism between the pressure chamber and the pressure relief chamber, and a compressed gas , in particular a device for supplying compressed air to the pressure chamber, and for the shutoff mechanism to relieve and discharge the upper pressure chamber in each case into the pressure or relief chamber located below,
It is configured as a pressure-controlled valve and is further provided with a filling device for filling the uppermost pressure chamber with the substance mixture to be ground, and furthermore with a filling device for filling the uppermost pressure chamber with the substance mixture to be ground, and furthermore with a filling device for filling the ground substance mixture to separate the mixture components. A receiving device for the mixture is connected, which receiving device supplies the substance mixture to be separated and a conveying device for discharging the extracted residual material, neutral and non-injurious to health. a circulation system for the gas, characterized in that the circulation system is provided with a pressurization and/or heating device and a depressurization or demixing vessel for converting the gas into a supercritical state. do. Furthermore, advantageous embodiments of the device according to the invention are provided by claim 13.
-25.

The invention will now be explained in detail with reference to the illustrated embodiments:
The figure schematically shows a device for comminuting a substance mixture, in particular a substance mixture consisting of plant products.

This device is particularly suitable for obtaining vegetable oil from oil-containing fruits and seeds. The structure and function of this device are as follows.

Dosing device 1 after being normally cleaned and subjected to suitable pretreatment
The fruits or seeds fed into reach the collection chamber 3 of the common pressure cylinder 2 in the direction of the arrow 1a.

During this feeding process, the valve 6 is open, so that the substance mixture can flow unhindered into the first pressure chamber 4 of the pressure cylinder 2. During this filling process, valve r is controlled by control valve 15.
, by conduit 16 and under the action of air pressure supplied by compressor 10. Once the pressure chamber 4 has been filled with the substance mixture, the valve 6 is closed automatically, in particular by the air pressure which is likewise supplied via the valve 13 and the conduit 16 from the compressor 10. When valve 6 is closed, pneumatic valve 12 is opened, which also derives its air pressure from conduit 16 and compressor 10. The perforated tube 12a distributes the air pressure evenly over the mixture of substances present in the pressure chamber 4 to be ground. When a predetermined air pressure is achieved in the pressure chamber 4, the valve 7 opens and at high velocity the homogeneous mixture rushes into the chamber 5, which is initially pressureless and in which the valve 8 is closed. In this way, the cells of the substance mixture that instantaneously flows into the pressureless chamber 5 and are under internal pressure burst from the inside toward the defective side due to the internal pressure, forming a slurry. When all of the substance mixture has fallen from pressure chamber 4 into chamber 5, valve r is connected to valve 15, conduit 1
6 and compressed air supplied via compressor 10. At the same time, valve 6 is opened and released for filling with the next substance mixture to be ground.

As soon as the valve T is closed, the pressure valve 14 is opened and a certain compressed air is supplied from the compressor 10 via the conduit 16, which compressed air passes through the perforated pipe 14a.
Chamber 5, which has already been transferred once from pressure chamber 4 into chamber 5 as described above and transformed into a pulverized slurry.
Acts on the object to be treated inside. In the pressure chamber 5, the same process as in the pressure chamber 4 is repeated, i.e. once a predetermined pressure is achieved in the second pressure chamber 5, the valve 8 is opened and the slurry under pressure is transferred to a high velocity. can be released into a pressure relief chamber 9 located below. During this second ejection and momentary release of pressure, the cells that have not yet been pulverized successively rupture and release the liquid component contained within. At intermediate points in time, pressure chamber 4 can be refilled and optionally the process can be repeated between pressure chambers 4 and 5.

The pulverized slurry can then be fed from the pressure release chamber 9 to the screw pump 18 via the connecting tube 1T in the direction of the arrow 1b.

Via a subsequent control valve 19, conduit 20 and feed hopper 21, the slurry is fed to a first separation and cleaning device 22. In this separation and cleaning device 22, solids and liquid components are first separated by centrifugal force, and in this case, it is also possible to simultaneously clean the oil-water mixture supplied via the conduit 40 and the three-way tank 26.

This oil-enriched mixture is conducted through an opening 35 in the device 22 via a conduit 36 to a collection vessel 37. The solids, from which oil and other liquid contents have been removed by centrifugal force, are fed in the direction of arrow 38 via the discharge hopper 23 to the feed hopper 24 of the second separation and cleaning device 25 . The separation and cleaning process described above is now repeated, except that in this case the separation and cleaning device 25 is internally separated into three processing sections. Processing sections 53 and 54 carry out a two-stage separation and washing of the material to be treated that has reached separation and washing device 25, while processing section 55 serves for the discharge of solid residues. The original separation and cleaning process proceeds as follows. The solids separated in the O device 22 fall into the second device 25 via the discharge hopper 23 and the supply hopper 24.

In the process of solid content flowing in, the branch pipe 32 passes through the conduit 28.
and fresh water is introduced into the treatment section 54 via the valve 30. The solids falling into this treatment section are washed and enriched with remaining oil components. This component is contained in the opening 41, the conduit 42
and via the three-way kettle 29, it reaches the processing section 53. There, this component is combined with the workpiece falling through the feed hopper. Once again the solid residue is now washed and enriched with oil, and the mixture is then passed through the opening 39.
, the conduit 40 and the three-way tank 26 to the first separation device. The cleaning fluid thus enriched with oil is mixed with the main amount of oil in the cleaning process and the concentrated oil/
The water mixture passes through the opening 35 and the conduit 36 into the collection container 3r.
be guided by.

The oil/water mixture present in the collection vessel 37 is led via a pump 56 and a line 45 to the inlet connection piece 46 of the special separator 4T and is supplied with control water via a valve 48, line 49 and main valve 33. be done. Separator 4r separates the whole fruit water and free solid particles from each other and sends pure anhydrous oil via opening 52 to a storage tank, not shown. Via the opening 50, the fruit juice water is returned to the water chamber of the separator 4T in a circulation system, while through the opening 5
1, the slurry-containing fruit juice water concentrate is transferred to a separator drum 47.
flows out from the nozzle. The solid residue that falls into the processing section 55 and is washed and freed of all oil residues is shown by arrow 4.
3, the discharge hopper leads via a conduit 44 to a conveying device, not shown, by means of which it can be discharged. FIG. 2 shows another embodiment of the device according to the invention, which is particularly suitable for obtaining grape juice from grape vines.

In this case, the pressure crushing process is the same as the process described in FIG. The substance mixture in this case consists primarily of grape tufts or tuft slurry. The parts of the apparatus in FIG. 2 which operate in the same manner as in FIG.
The same symbols are used as in the figure. After the pulverized slurry under pressure flows into the pressure relief chamber 9, this slurry passes through the screw pump 18, and then passes through the control valve 19 and the conduit 2.
0 to the feed hopper 21 of the separation device.

The three-way pot 26 remains closed and the liquid (grape juice) is separated from the solids by centrifugal force and the opening 3
5 and the conduit 36 into the collection container 31. The solids from which all liquid has been separated are led in the direction of the arrow 38 through the discharge hopper 23 and the opening 41 via a conduit 44 to a conveying system (not shown) and discharged therefrom. From the collecting vessel 37, the grape juice is led by a pump 56 through a conduit 45 to a separator 41 which sends the pure grape juice, free of all impurities, via an opening 52 to further processing.
On the other hand, the solid content is extruded through the opening 51.

According to the invention, the processes and treatments described above can also be used to obtain sugar from sugar-containing fruits or plants.

The sugar-containing fruits and plants, which have been washed in a conventional manner, are ground or pre-shredded in a crusher.

According to FIG. 1, the crushed material thus obtained is fed via a metering device to the collection chamber of the pressure cylinder 2. The process of grinding the sugar-containing fruits or seeds is the same as described in connection with FIG. The workpiece that has fallen into the pressure relief chamber 9 is
The solids are washed on a counter-current principle in one or more multi-stage washing and separation devices 22, 25 (FIG. 1) for further processing via a control valve 19 and a conduit 20 by means of a screw pump. is separated from the liquid. In this case, the liquid content is collected in the collection container 37. The separated and desugarized solids fall onto a conveying system connected to conduit 44, which conveys the solids from the apparatus. Sugar can be produced from the sugar-containing liquid thus obtained in various forms and manners. In the case of processing hard seeds or grains or in order to enhance the crushing effect, a buffling device 57 as shown in FIG. 3 is connected, which is adapted to the object to be processed.

This buffling device can be installed below the outflow valve r below one or more pressure chambers. FIG. 3 shows an embodiment of the buffling device 5T of the present invention as described above, which device 51 connects itself and the outflow valve r of any chamber 2 to the flange 58.
It has a connecting member 59 that connects through. This connecting member has a hopper shape 60 in its interior that is more or less conical depending on the object to be treated. The wide diameter 61 of the hopper-shaped conical recess corresponds to the inner diameter of any outlet valve r of the pressure chamber 4 of the pressure cylinder 2. The outlet 62 of the connecting member 59 has a small diameter corresponding to the material to be treated, thereby creating a nozzle effect, converging the pulverized material flowing out and delivering it to the buffling head 63 at a higher speed. make it collide. The baffle head 63 consists of a steel cylinder screwed into a frame 64, which is advantageously provided with an open thread. The frame 64 is fixed within a hopper-like hood 65 by horizontal reinforcing members 66. A recess 63a is formed at a predetermined angle at one end of the baffle head 63 to change the collision angle at the center position.
is provided. At its opposite end, the baffle head 63 has an adjustment disc 67 with a larger diameter.
The buffle head 63 may optionally be threaded and screwed into its frame 64, thereby making it possible to adjust the distance between the outflow nozzle 62 and the buffle head 63. If a flat impact surface is desired, the baffle head 63 can be removed from the frame, turned over 180 degrees and screwed in again from above, so that the adjustment disc 6r faces the nozzle opening 62 and thereby provides another You can get a full effect.

The above-mentioned grinding process and the equipment for carrying out the process are suitable for obtaining fruit juices of all kinds, in particular grape juice, or for producing edible oil from oil-containing fruits and seeds, but are also costly and involve large expenditures. There is no need to use mechanical or hydraulic screw presses or filter presses in conjunction with.

Furthermore, the danger of explosion during the recovery of cooking oil and additives is eliminated. FIG. 4 shows another embodiment of the invention, which is a further improvement on the apparatus shown in FIG.

Regarding components that are the same or have the same function, the first
The same symbols are used throughout the figures. The embodiment of FIG. 4, like the devices of FIGS. 1 and 2, is based on the recognition that plant products, such as seeds and fruits, are composed of small cells. Each cell contains a liquid component,
For example, it contains fruit juice or oil. These liquid components are surrounded by cell walls. Cell fluid is normally under atmospheric pressure. When these plant products are placed under increased pressure in a pressure vessel, the liquid present inside the cells is not compressed because it is incompressible, but rather increases inside the cell and acts on the cell wall. Equilibration of the liquid pressure with respect to the applied external pressure takes place. By the way, in reality, if the external pressure is removed momentarily, or if compressed gas is released at high speed, the cell wall will rupture from the inside to the outside, and the liquid contained within the cell will burst. It was discovered that it releases . In this case, the rupture of the cell wall is due to the fact that the cell internal pressure cannot be reduced or compensated for in a short release time of the column pressure. In the above-mentioned processes of the invention which carry out two or more stages of depressurization and depressurization, the respective depressurization of the compressed gas is carried out until atmospheric pressure, generally atmospheric pressure, is reached.

The device shown in FIG. 4 and the method that can be carried out with it are improved in that they allow significantly increased efficiency and, at the same time, significantly higher speeds of operation. By depressurizing and releasing the compressed gas to a partial pressure significantly higher than atmospheric pressure and by supplying the substance mixture to be comminuted at least under said partial pressure, on the one hand, high rates of depressurization result in cell wall rupture and The liquid is released (but at the same time the pressure is released and the new increased pressure is achieved by waiting until atmospheric pressure is achieved during the release and the desired increased pressure is achieved). In this case, the invention shows that the rupture of the cell wall does not depend on the absolute pressure difference between the elevated pressure and the atmospheric pressure, but rather on the absolute pressure difference between the elevated pressure and the atmospheric pressure. Rather, it is based on the recognition that the increased pressure range depends on the pressure range.

Relief in the range of high pressure differentials and also the achievement of elevated working pressures can be carried out in a generally shorter time than the above-mentioned depressurization to atmospheric pressure and pressure rise to the desired working pressure. . The efficiency increase that can be achieved results not only from significant time savings, but also from significantly reduced energy costs. This is because the pressure only needs to be increased in the increased pressure difference range. Next, in the same format as in FIG.
The apparatus shown in the figure will be explained. The substance mixture to be ground, for example fruit or seeds, is first washed in the customary manner and, after appropriate pretreatment, is fed by metering device 1 to collection chamber 3 .

During this process, valve 5 is opened, while valve 6 remains closed for the time being. Valve 5 is then closed again and a partial pressure is created in collection chamber 3 by means of compressor 10 via line 16 after opening of pneumatic valve 2. This partial pressure has a height approximately equal to , corresponds to the pressure present in the pressure chamber 4 at the time of transfer of the substance mixture from the collection chamber 3 to the first pressure chamber 4 of the pressure cylinder 2. For the transfer, the valve 6 is opened, thus The substance mixture under said partial pressure can fall unhindered in the direction of the arrow 1a into the first pressure chamber 4 of the pressure cylinder 2. During this transition process, valves 5 and r are closed; The valve is operable by pneumatic pressure supplied from the compressor via the control valve 22', the conduit 16 and the compressor 10. When the pressure chamber 4 is filled with the substance mixture, the valve 6 is automatically activated by the pneumatic control. It is closed by means of a mechanism, in particular via the valve 13, the conduit 16 and the compressor 10. When the valve 6 is closed, the pneumatic valve 12 is opened, which likewise has a common conduit 16 and the compressor 10. By means of the perforated tube 12a, the pressure is evenly distributed over the substance mixture present in the pressure chamber 4.The increase in air pressure from the initial partial pressure to the required high pressure is rapid. A predetermined air pressure is applied to the pressure chamber 4.
As soon as this is achieved, valve r is opened by control valve 15, while valve 6 is kept closed. Thereby, the substance mixture can rush at high speed into the underlying second pressure chamber 4a of the common pressure cylinder 2. In the lower pressure chamber 4a a partial pressure is created which is clearly higher than the atmospheric pressure, in particular atmospheric pressure, but significantly lower than the high pressure previously obtained in the pressure chamber 4. While the material mixture is forced in at high speed, the internal pressure of the cells, already described, acts, causing the cells to rupture from the inside out and form a slurry. Preferably, the valve 7 is closed before the entire substance mixture reaches the other pressure chamber 4a from the pressure chamber 4, so that a portion of the substance mixture still remains in the lower part of the pressure chamber 4, where one species , so that a partial pressure still remains in the pressure chamber 4 after the pressure relief has been completed.

As soon as the valve 7 is closed, the previously described filling process of the collection chamber 3 and the first pressure chamber 4 can be repeated.

The second lower pressure chamber 4a serves for repeating the grinding process, especially in difficult-to-grind substance mixtures. For this,
Both valves 1 and 8 are closed and the second
A partial pressure exists in the lower pressure chamber 4a. By opening the pneumatic valve 14, air under high pressure is forced into the second pressure chamber 4a from the compressor 10 via the conduit 16 and the perforated pipe 14a. Once the desired predetermined pressure has been achieved in the pressure chamber, the valve 8 is opened, so that the slurry under pressure is forced into the pressure release chamber 9 at high speed, with the slurry still uncomminuted and uncomminuted. The cells are ruptured and pulverized by the action of internal pressure. During this process, pressure chamber 4 is also filled and the process is repeated stepwise and selectively between pressure chambers 4 and 4a. The milled slurry material mixture can be delivered via the connecting tube 11 by means of a suitable conveying device. The pressure relief chamber is preferably similar to the previously described chamber in which the pulverized substance mixture is
It is maintained under the partial pressure generated during the transition from the pressure chamber 4a to the pressure relief chamber 9. This partial pressure is advantageously used to convey the treated substance mixture via control valve 19 and line 20 to a subsequent separation and cleaning device, not shown. With this method of operation, the illustrated screw pump 18 can generally be omitted. However, the transport of the selectively ground substance mixture from the pressure relief chamber 9 to the subsequent processing location can also be carried out under vacuum or negative pressure. For this purpose, the pressure relief chamber may be provided with a suitable vacuum connection. The type of grinding of the material mixture according to the invention is as described in connection with FIGS. 1-4.

After grinding, a slurry-like substance mixture is obtained, which consists of the liquid fraction to be obtained and the solid fraction.

In the case of some plant products, such as, for example, grape vines, it is possible to carry out the separation of the mixed components by means of a separator as described above, thereby obtaining at least a portion of the liquid component. However, this separation of mixed components is associated with high equipment costs, high energy costs and long processing times. This also applies to the known type of separation of mixture components by extraction. Next, another treatment method of the invention will be described in order to achieve consistent quality of the obtained material with low equipment costs and good economy.

This method is based on the recognition that liquefied gases, or gases brought into a supercritical state by increased pressure and/or temperature, have the property of acting particularly strongly as solvents. That is,
A liquefied gas in a supercritical state, ie above a critical temperature and pressure, can absorb soluble substances from a mixture of substances and form a supercritical liquid. The amount of material that can be dissolved in the liquefied gas is several times the amount that would be expected based on the vapor pressure at a given temperature. In this case, inert gas,
That is, it is appropriate to use a substance that is neutral and does not pose a health hazard. For this purpose, carbon dioxide is advantageously used in practice, the supercritical range of which is a pressure above about 73 bar and a temperature above about 33°C. However, in special cases it is also possible to use other gases, such as ethylene. The process proceeds roughly as follows.

First, a high-pressure vessel is filled with the substance to be separated.

After filling, a supercritical gas is introduced, which acts on the substance mixture and forms a supercritical liquid. This supercritical liquid, ie, the liquid consisting of supercritical gas and dissolved material, is sent to a demixing vessel after a certain residence time. In this demixing vessel, the supercritical state of the liquid is released by lowering the pressure and/or temperature. This results in a spontaneous demixing of the gas on the one hand and of the dissolved substances on the other hand. The material separated from this initial material mixture settles in the lower part of the demixing vessel as the desired product obtained and can be removed for further processing. The gas, which has been freed of previously dissolved substances, rises and can therefore be removed from the upper part of the demixing vessel and returned to the high-pressure vessel for reuse in the circulation system. 5 and 6, a preferred embodiment of the device for carrying out the method and the mode of operation of the device will now be described.

In the embodiment shown in FIG.
Equipped with 03d.

These vessels are configured as high-pressure vessels. The number of high-pressure vessels depends on the length of the total residence time or extraction time, which in turn depends on the substance mixture and the gas selected. If the extraction time is 4 hours, it is advantageous to use four receiving vessels, as in this example, the volumes of the receiving vessels corresponding to the desired time efficiency of the device. A common supply device 102 is preferably connected to the four receiving containers 103 .

The feeding device 102 is preferably constructed as a screw conveyor driven by a motor 102a, which is surrounded on all sides by jackets and at the same time functions as a metering device. The material mixture to be treated, which has been ground and optionally after-treated in the device shown in FIGS. and dispensed into one of four receiving containers. A common feeding device for this purpose is the receiving vessel 1
A drawer connection piece 10 that communicates with the upper end of the receiving container
2b, 102c, 102d and 102e.
Each drawer connection piece has a filling valve 124, 125, 12.
Equipped with 6 and 12r. In order to meter the substance mixture to be treated, for example into the receiving container 103a, the filling valve 1 is activated.
24 is opened, while the other filling valves 125, 126
and 12r remain closed. During this filling process,
Further, the discharge valve 134 of the receiving container 103a is closed. The feed substance mixture should be considered previously purified and suitably pretreated. Advantageously, the substance mixture to be extracted is ground or coarsely ground before being fed. The filling of the further receiving containers takes place correspondingly in a fixed time cycle. Receiving containers 103a, 103b, 103c
and 103d are conduits 109a, 109b at the lower end of the container.
, t) via 109c, 109d and 143, 144, 145 and at the upper end of the container conduits 110, 111, 112, 1
13 and 136, 137, 138, and 139, they are mutually connected in parallel.

These conduits connect valves 118-123, 149 and 128.
~133,135 can be selectively blocked. Furthermore, the lower ends of the receiving containers 103b, 103c and 103d are
via conduits 146, 14r and 148 and isolation valve 12.
Upper common connecting conduit 1 via 8, 129 and 131
10, 136, 13r, 138 and 139. Finally, as can be seen in FIG. 5, the husband's receiving vessel is connected via the line to a common gas circulation system and can be shut off from this circulation system by means of the valve. In particular, a shutoff valve 133 serves to shut off the common gas circulation system. From this valve 133, a conduit 141 leads to a heat exchanger 114, which is connected to the conduit 14.
2 to the pressure release and demixing container 11r.

This pressure relief vessel 11r has at its lower end an outlet 115 for the substance to be collected. Gas flows from the upper end of pressure relief vessel 11r via conduit 116 into gas storage vessel 104, via another conduit 105 and heat exchanger 106 to compressor 10r or other suitable liquefied gas pump, and finally It flows into another heat exchanger 108 via conduit 107a. The gas circulation system is then closed via conduit 109, which advantageously ends at the connection between the two conduits 109a and 143. The mode of operation of the apparatus shown in FIG. 5 is generally as follows.

When the receiving container 103a is filled with the substance mixture to be treated,
The filling valve 124 is closed and after opening the valve 118, a neutral inert gas, for example carbon dioxide, enters the receiving vessel 103a in the form of supercritical gas via the heat exchanger 106 and the compressor 10γ and another heat exchanger 108. , in particular until the entire substance mixture is covered. The liquefied gas remains in this receiving container 103 until a predetermined residence time elapses.
stay at a. During this residence time, the second receiving vessel 10
3b is filled from the supply device 102 after opening of the filling valve 125, with the discharge valve 134 being closed.

As soon as this receiving container 103b is filled, the filling valve 1
25 is closed. After the residence time in the receiving vessel 103a, the valve 128 is opened, but the valve 135 remains closed. Therefore, the liquefied gas flows from the container 103a to the conduit 1.
10 and 146 in a supercritical state.
It is possible to move to b. During the duration of the residence time in the receiving vessel 103a, the supercritical gas is enriched with constituents of the substance to be separated, so that these constituents reach the receiving vessel 103b together. As soon as this enriched gas has completely transferred to the receiving vessel 103b, the valve 128 is closed. At this time, the filling valve 125 is also closed. Valve 118 is then opened, so that fresh gas from gas receiving vessel 104 can flow in a supercritical state into receiving vessel 103a until the substance mixture to be treated contained therein is again completely covered. . During this operating time, the container 103c is filled with the substance mixture from the supply device 102 via the open filling valve 126, in particular with the valve 134 closed.

Furthermore, the transfer of the enriched gas again from the receiving vessel 103b to the receiving vessel 103c and further from the receiving vessel 103a to the receiving vessel 103b takes place in the same manner as described above. The receiving vessel 103a is then filled with fresh supercritical gas via the valve 118 which is opened again. During the residence time in the three receiving vessels 103a, 103b and 103c, the receiving vessel 103d is finally filled with the substance mixture from the supply device 102 via the open filling valve 127 and the filling valve 127 is closed.

After a suitable residence time, valve 131 is opened, in which case valve 1
32 remains closed. Thereby, the enriched gas can pass from the receiving vessel 103c to the receiving vessel 103d, in particular until the receiving vessel 103d is filled and the substance mixture contained therein is completely covered. . After closing the valve 131, the gas is transferred again step by step from the individual preceding containers. 1st
The fourth and fourth fresh inert gas is charged to the receiving vessel 103a. In this embodiment, after a residence time of one hour, the inert gas is again transferred in stages.
As soon as the gas is removed from the receiving vessel 103a, the completely extracted residue can be discharged from said vessel via the discharge valve 134. Similarly, the gas is transferred stepwise sequentially from receiving vessels 103a to 103b and from 103b to 103 as described above after a residence time of 1 hour in each case in this embodiment.
c and finally to 103d.

Thus, the gas is present in the first receiving vessel 103b by about 1/4 or 25% of the substance to be extracted, in the second receiving vessel 103b a further 1/4, i.e. about 50% in total, and in the third receiving vessel 103b.
c is further enriched to a quarter, ie to a total of approximately 75%, and thus finally the rearmost receiving vessel 103d is enriched until it is completely saturated with 100% of the substance to be extracted.
It is self-evident that in the gas transfer sequence, the receiving vessel from which the gas is transferred from the neighboring vessel must always be evacuated beforehand. The gas, now completely saturated with the contained substances, can be transferred to the depressurization or demixing vessel 117 via the heat exchanger 114 after opening the valve 133. Here, a reduction in pressure and/or temperature below the gas critical range, and thus a depressurization, takes place, so that the gas is spontaneously separated from the entrained substances. Gas is stored in gas container 1 for reuse.
Returned to 04. The harvested material can be removed via outlet 115. In this way a continuous circulation of the inert gas is ensured and a complete and exhaustive extraction of the substance to be obtained is achieved.

By suitably switching said valves, it is also possible and optionally possible to switch the operating sequence of the receiving vessels in such a way that each receiving vessel is filled with fresh supercritical gas in succession. is advantageous.

For example, if it is desired to fill the receiving container 103b with fresh gas, valves 118 and 120 are closed and valves 119 and 12 are closed.
Just open 2. If it is desired to transfer the partially saturated gas from the rearmost receiving vessel 103d to the first receiving vessel 103a, valves 128, 129, 131 and 133 may be closed and valves 135, 130 and 132 may be opened. .
However, it is also possible to provide a connecting line with a safety valve between the lines 109a and 146 and to supply the gas via the valve 128. FIG. 6 shows how the gas is enriched during the individual residence times in four successively connected receiving chambers and on the other hand how the substance mixture present in the receiving vessel is to be obtained. This indicates whether the substance is extracted from the substance.

Figure 6 clarifies the individual processes; in this case, for the sake of clarity, only the lower part of the drawing shows the four side-by-side receiving vessels, whereas the upper three 3, 2, and 1 containers have been omitted for simplicity. This is because these containers are in any case still empty at the beginning of the process and are not filled with any substance mixture or gas. However, as soon as the aforementioned process has been carried out for all four containers, the whole process is correspondingly repeated. Instead of the counter-extraction described above, another type of filling of the receiving container can be achieved by operating the valves of the device in a different manner.

For example, instead of only one container in each case, two or even all receiving containers can be filled at the same time or at intervals. The same thing applies to gas supplies. If, for example, it is not desired to obtain as continuous a material as possible, but rather to process a particularly large amount at a particular point in time, it is advisable to fill several receiving vessels simultaneously. An advantageous embodiment of the device according to the invention consists in that the receiving containers are arranged circularly relative to one another.

In this case, a central feed hopper is provided which is designed to be filled with the substance mixture one after the other at regular time intervals via a conveying device of a different type than mentioned above, which rotates in a circle. It is advantageous to configure the feeding device so that it has.
In this case, the extracted residue can also be discharged via the central collection vessel. A device of the type described above is particularly suitable for extracting vegetable oils.

[Brief explanation of the drawing]

The drawings show an embodiment of the invention, and FIG. 1 is a schematic representation of an apparatus for comminution of a substance mixture, which is suitable in particular for separating off all solids and for obtaining vegetable oils or fruit juices. , FIG. 2 is a schematic illustration of an apparatus corresponding to FIG. 1, which is particularly suitable for obtaining grape juice from grape tufts, and FIG. 3 is a diagram of the apparatus shown in FIGS. a schematic longitudinal sectional view of a device configured as an auxiliary device, i.e. a buttful device;
FIG. 4 is a partial block diagram of the apparatus shown in FIGS. 1 and 2, and FIG. 5 shows a mixture component which can be connected to the apparatus shown in FIGS. and FIG. 6 is a schematic diagram illustrating a process relating to the apparatus shown in FIG. 1... Metering device, 2... Pressure cylinder, 3... Collection chamber, 4, 4a. 5...Pressure chamber, 6,7,8...combined, 9...pressure relief chamber, 10...compressor, 12...pneumatic pressure Valve, 12a...Pipe provided with a hole, 13.
...Valve, 14...Pressure valve, 14a...
... Pipe provided with holes, 15 ... Control valve, 1
6... Conduit, 17... Connection member, 18
...Screw complete pump, 19...Control valve, 20...Conduit, 21...Supply hopper, 211...Valve, 22. ...Separation and cleaning device, 22'...Valve, 23...
Discharge hopper, 24... Supply hopper, 25...
...Second separation and cleaning device, 26...Three-way pot, 28...Conduit, 29...Three-way pot, 30...Valve, 32 ... Branch pipe, 33 ... Main valve, 35 ... Opening, 36
... Collection container, 40 ... Conduit, 41.
...Opening, 42, 44, 45... Conduit,
46... Inflow connection pipe piece, 47... Special separator, 48... Conduit, 50, 51, 52.
...Opening, 53, 54, 55...Processing division, 56...Pump, 5r...Buttful device, 58...Flange, 59・・・・・・
Connection member, 60...Hopper type, 62...
・Outlet (nozzle hole), 63... Buff full head, 63a... Recess, 64... Frame, 65... Hood, 66... - Lateral reinforcing member, 6r...adjustment disc, 102...supply device, 102b, c, d, e...drawer connection tube piece, 103a, b, c, d ...Receptor container, 1
04... Gas storage container, 105... Conduit, 106... Heat exchanger, 101...
Compressor, 101a... Conduit, 108...
...Heat exchanger, 109a, b, c, d...
Conduit, 110, 111, 112... Conduit, 11
4... Heat exchanger, 115... Outlet, 116... Conduit, 11r... Pressure release and demixing container, 118, 119, 120, 121, 12
2,123...Valve, 112,125,126,
12T... Filling valve, 128, 129, 130,
131, 132, 133... Valve (shutoff valve), 1
34...Discharge valve, 135...Valve, 13
6,131,138,139,141,142,143
,144,145,146,147,148...
・Conduit, 149... Valve.

Claims (1)

[Claims] 1. A method for comminuting a mixture of substances and separating the components of the mixture by extraction, in which the mixture of substances is exposed to high pressure by supplying a compressed gas, and subsequently the components of the mixture of substances are separated within the mixture. The mixture components are depressurized by releasing a compressed gas at a high velocity so as to be ruptured by the pressure generated in the mixture, and the crushed mixture components are separated by extraction into a neutral, healthy material. exposure to a gas existing in a supercritical state that does not harm the gas for a residence time until the gas is enriched with the substance to be extracted from the corresponding mixture components, and subsequently releasing the gas into the subcritical range. grinding of the substance mixture and mixing components, characterized in that the extracted substances are separated from the gases and the gases are again converted into a supercritical state and returned to the substance mixture to be separated in a circulation system. How to separate. 2. Process according to claim 1, characterized in that the pulverized substance mixture is subjected to a pretreatment by washing in co-current or counter-current before separation. 3. The depressurization and release of the compressed gas is carried out to a partial pressure significantly above atmospheric pressure, and the substance mixture to be ground is supplied at least under said partial pressure. Method. 4. A method as claimed in claim 3, in which the pulverized substance mixture is distributed in each case and transferred from the pressure chamber to the pressure relief chamber. 5. The method according to claim 4, wherein a suitable amount of the unpulverized substance mixture is charged into the pressurizing chamber. 6. A method as claimed in claim 4, in which the overpressure remaining in the pressure chamber after the transfer of the portions is utilized for conveying the comminuted substance mixture from the pressure relief chamber to a further processing position. 7. The method according to claim 4 or 5, wherein the pulverized substance mixture is transported from the pressure relief chamber to the subsequent processing device under vacuum. 8. The gas is fed in a supercritical state in a stepwise manner, with strict observance of the respective residence times, into a number of containers for receiving mixtures of similar substances separated from each other and only then released in order to separate the extracted substances. The method according to claim 1, wherein the pressure is increased. 9. A method as claimed in claim 8, in which the feeding and discharging of each individual substance mixture under pressure is carried out during the duration of the residence time of the other substance mixture. 10. A method according to claim 8 or 9, in which the substance mixture to be extracted is crushed or coarsely ground before being fed. 11. Process according to any one of claims 8 to 10, in which the pressure and/or temperature is reduced to at least a subcritical range of the gas in order to depressurize the extracted material. 12. A device for comminuting a mixture of substances and separating the components of the mixture by extraction, comprising at least one pressure chamber for comminution of the substance mixture, a pressure relief chamber arranged above the pressure chamber, and a pressure chamber arranged above the pressure chamber; and a pressure relief chamber, and a device for supplying compressed gas to the pressure chamber. It is configured as a pressure-controlled valve for releasing and discharging the pressure chamber, and is further provided with a filling device for filling the uppermost pressure chamber with the substance mixture to be ground. Furthermore, a receiving device for the comminuted substance mixture for separating the mixed components is connected, which receiving device supplies the substance mixture to be separated and a conveyor for discharging the extracted residual material. and a circulation system for neutral, non-healthy gases, with pressurization and/or heating devices and depressurization for converting the gases to a supercritical state. or a device for comminuting a substance mixture and separating the mixed components, characterized in that it is provided with a demixing vessel. 13 Two or more pressure chambers are arranged one above the other with the intervention of a blocking mechanism, and each of the above blocking mechanisms relieves and discharges pressure from the upper pressure chamber to the pressure chamber or pressure relief chamber below. 13. The device of claim 12, wherein the device is a pressure controlled valve. 14. The individual pressure chambers are selectively configured vertically in series, parallel to each other, or in a circular configuration, and each pressure chamber has a pressure relief chamber below, whereby the pressure of the first pressure chamber is Claim 12 or 13, wherein the conveying pump conveys the crushed pressure material from the pressure relief chamber to the supply hopper of the next pressure chamber, and thus performs pressure crushing in two or more stages. Device. 15. The outlets of the valves of the individual pressure chambers are each connected to a device with a baffle head, which device focuses the pulverized substance mixture exiting with a nozzle effect onto said adjustable baffle head. Claims 12-1
4. The apparatus according to any one of clauses 4 to 4. 16. Within the baffle device, the baffle head is fixed in a central position by a transverse stiffening member, is adjustably screwed into a threaded frame, and is constructed as a cylindrical body with an external thread. , an adjustment disc having a centrally located recess at one end and a larger diameter at the other end, and wherein the baffle head is provided with a centrally located recess at one end and an adjustment disc having a large diameter at the other end, and wherein the baffle head is arranged such that the recess or adjustment disc faces the outflow valve of the baffle device. Claim 1, which is selectively screwable so as to
The device according to any one of Items 2 to 15. 17 Claim 1, in which a pipe is guided through the pressure chamber of the pressure cylinder, and the pipe is provided with a hole in the center thereof for evenly distributing air or gas necessary for pressurization.
The device according to any one of Items 2 to 16. 18. Apparatus according to any one of claims 12 to 17, in which one or more separators are connected to purify and clarify the product obtained. 19. The pressure control mechanism of each valve is constructed and comminuted so that the valve is opened only during the depressurization and release process of the compressed gas, up to an adjustable partial pressure clearly above atmospheric pressure. 13. The device as claimed in claim 12, wherein the filling device is constructed in such a way that the substance mixture to be filled can be fed under at least the above partial pressure and is provided with a compressed gas connection. 20. The device according to claim 19, wherein the pressure relief chamber is provided with a vacuum connection. 21 The receiving device consists of a number of receiving vessels, each of which is connected to a supply device for the raw material, the receiving vessels are connected in series by a conduit, and the conduit can be shut off by a valve. and each receiving vessel is connected to a gas circulation system by said conduit and can be shut off from said circulation system by said valve.
Apparatus described in section. 22. Device according to claim 21, characterized in that a common supply device is provided for all receiving containers. 23. The device according to claim 21 or 22, wherein a heat exchanger is provided in the circulation system following the last container, and a pressure relief container follows the heat exchanger. 24 The pressure relief vessel includes a gas storage vessel, and the gas storage vessel is further followed by two heat exchangers, and a compressor or a liquefied gas pump is arranged between the two heat exchangers. Any 1 of Items 21 to 1, Item 23
Equipment described in Section. 25. Device according to claim 22, characterized in that the common supply device has a drawer connection tube for each receiving container leading to the upper end of the container, and each of the tubes is provided with a filling valve.