JPS605341B2 - How to perform ion exchange - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to an ion exchange method and apparatus, and more particularly to a method and apparatus for ion exchange between a fibrous ion exchange medium and a protein-containing solution.

Typically such liquids are effluents from food and beverage plants, such as milk formula from milk processing plants. This effluent can be processed to recover useful proteins,
Or simply treat the effluent to make it less harmful to a point where it can be discharged into a river or recycled in some way. In this specification, the term "protein" shall mean a substance that can undergo ion exchange in a fibrous ion exchange medium, such as proteins and substances related thereto, and enzymes and substances related thereto.

GB 1,436,547 and GB 1,387,265 disclose such a process and a method for producing the fibrous media used therein. However, the practical application of such treatment is still at a very rudimentary stage, and large-scale plants are not yet in operation in any country.
We submit that the practical application of such a process requires a plant with novel and inventive features that enable it to meet certain basic three criteria, and a method of operating such a plant. The inventor of has discovered.

The main criteria are as follows.

3'1} Ion-exchange media are highly specialized in all respects compared to common ion-exchange materials of the resin type or of the natural or synthetic zeolite type. The economical operation of large-scale plants requires a highly efficient separation of the ion exchange medium in several process steps from the liquid 4 that forms the slurry during the various processes.
The inventors have devised a method that allows for highly efficient dewatering or other liquid removal. This method simultaneously dewaters and reduces wastage of the very expensive and finely disposed ion exchange media. Severe wear can cover the separator and result in loss of ion exchange media.
The method according to the invention allows optimal reformation of the active slurry following the preceding separation process. ■ In practice, it is necessary to have a large processing capacity, to avoid an excessively large external size of the plant, and to keep the initial equipment cost and operating cost low. Therefore, the highly efficient and simple separation technique of the present invention is extremely advantageous. {3' In practice, it is necessary to be able to reliably reproduce each processing step.

The present invention overcomes the shortcomings of conventional methods and apparatus, particularly for the separation of liquids from ion exchange media during various processing steps.

In the ion exchange method of the present invention, a fibrous ion exchange medium is internally mixed with a liquid containing a protein substance, reacts with the liquid, mixed with a cleaning liquid for cleaning, mixed with a regenerating liquid, and the regenerated liquid. A container is used that reacts with the protein to generate an eluate containing the protein, that is, in which these three processing steps are performed.

In all vessels the separation of the ion exchange medium from the liquid is
This is done with the aid of an air pressure differential applied to both sides of the furnace in the vessel. This method is similar to other types of separation equipment, where many extra accessories are used and many extra processing steps have to be performed for a given output. This eliminates the drawbacks associated with the use of liquids (which cannot be mixed with liquids). Therefore, using such a separation device
Totally impractical in commercial plants. Apparatus for carrying out the method of the invention includes a container.

Each container includes therein a sieve and a furnace provided under the sieve. A tanker is provided for storing the ion exchange medium and liquid mixture and for storing the liquid at each stage of the process. A device for supplying air, protein-containing liquid, washing water, and regeneration liquid to containers as necessary, and for supplying acid and alkaline solutions to maintain the correct pH value at each stage of processing. is also provided. Hereinafter, the present invention will be explained in detail with reference to the drawings.

FIG. 1 shows a vertical cylindrical container 10.
It is designed to withstand internal pressures of up to 2 atmospheres during use.

However, it is unlikely that normal pressures above about 1.5 atmospheres will be required during use. This container is made of stainless steel or reinforced plastic, even if the liquid is treated by interaction with a fine fibrous ion exchange medium.
For example suitable for processing milk tests. The container 10 has a shaft 14
It includes a hawk holder 12 that can be rotated by a hawk. The fly lamp 12 may also be a vibrating lamp that can vibrate vertically by means of a vibration agitation mechanism (not shown) connected to the upper end of the shaft 14. The shaft 14 is rotated by a motor mounted on the top of the container 10. The container 101 also includes a furnace 16.

The filter 16 may be a wedge-shaped wire screen, a metal grid, a filter cloth, a perforated metal plate, or other types of filters. The filter 16 has holes sized, shaped and contoured to efficiently separate the liquid from the ion exchange medium without clogging. The filter 16 extends over the entire diameter of the vessel 10. As shown, the furnace 16 includes a retaining ring 100, a gasket 102 made of a material such as neoprene, a sheet 104 of IN316 grade furnace wire mesh material, a support grid 106, and a A sheet 108 of furnace-filtered wire mesh material with holes about 1.27 inches (0.5 inches) spaced about 11 to 15 inches apart.
3 skin (1'4 inch) thick plate 110 and inner flange 1
14 and a neoprene gasket 112 placed on top of the gasket 14. The furnaces 16 are fixed to each other by bolts. The vessel 10' has an upper inlet and outlet 18 controlled by valves (not shown) for admitting liquid and air, a vent (not shown) communicating with the atmosphere, and a furnace 16 below the furnace 16. It has a discharge port 30 for discharging the liquid.

If necessary, an outlet for the ion exchange medium is provided in the vessel 10 immediately above the furnace 16.

Container 10} is also provided with a PH probe 118. Second
The figure shows the apparatus in which the reaction vessel 10 is used. This device includes a large lactic acid storage tank 200 connected to a container 101 by a pump 202 and a valve 204, a water supply pump 206,
It consists of an air supply pipe 208 and a holding tank 210 having a lower outlet connected via a valve 212 to the upper end of the container 10 and to a pump 214 . Pump 214 is coupled to product tank 216. An outlet 30 is provided at the bottom of the container 10.

This outlet 30 is connected to valve 218. One outlet of this valve is connected to the upper end of the container 10 via a circulation pump 220 and also connected to valves 222 and 224.
Valve 224 is connected to the upper end of holding tank 210. An air supply pipe 226 is connected to the rising portion of the holding tank 210. An acid conditioning tank 228 is connected to the vessel 10 via an acid supply pump 230.

Further, an alkali adjustment tank 232 is connected to the container via a pump 234. The device shown in Figure 2 is (1・1
・1) It can operate according to this mode.

This (1.1.1) mode consists of one step of loading the ion exchange medium with protein material, one step of washing the ion exchange medium with water, and one step of purchasing the protein from the ion exchange medium in solution in the regeneration liquid. One step is to remove materials and regenerate the ion exchange medium. Figures 3a-3g show a complete cycle of each step of the method of the invention. FIG. 3a shows lactic acid delivered from tank 200.

The fibrous material is shown stationary at position 201. Figure 3b shows the pH adjustment performed using hydrochloric acid delivered from tank 228 and the absorption of protein material by the ion exchange medium when the ion exchange medium and milk curd are mixed in a vortex. The fibrous ion exchange medium becomes loaded with protein material from the lactic acid and when the concentration is stopped, a slurry of the milk powder, which has been removed from the protein material, and the ion exchange medium loaded with the protein material. Compressed air is blown over the lactic acid (FIG. 3c) to help drain the proteinaceous lactic acid through the filter 16.

The protein-removed liquid is placed into a drain. In this way, the ion exchange medium is separated from the liquid and the wash water is then introduced into the container 10 from the water line. Then, the evaporator 12 is operated to mix the ion exchange medium and washing water to wash the ion exchange medium (FIG. 3d). Then, compressed air is again blown from the top of the container 10,
It helps separate the ion exchange medium and wash water (this step is not shown) and directs the wash water to a drain or separate water storage tank (not shown).

The compressed air is then sent to the holding tank 210 and the water therein is sent to the tank 10 (Figure 3e).

The caustic soda solution is then added to provide the correct regeneration solution and the mulch 12 is activated to thoroughly mix the ion exchange medium and regeneration solution (Figure 3f). The ion exchange medium then loses its protein-purchasing substance and is regenerated. The regeneration solution then becomes rich in protein substances. Compressed air is then admitted into vessel 10 to assist in separating the regenerant from the ion exchange medium.

This compressed air forces the regenerated liquid out of the vessel 10 through the furnace 16. The regenerant or product solution is sent directly to an ultrafurnace to separate the useful protein material.
Alternatively, it is sent to storage tank 210. Product solution in tank 2
10 may optionally be followed by a second absorption step by mixing the product solution with fully regenerated ion exchange media in vessel 10 to further enrich the product solution with protein. It is shown simply to show that it is possible to do this. Such an operation mode is (2.1
・1) Mode. If desired, it is also possible to perform the (2.1.2) mode using two stages of reproduction. The protein-enriched product solution is pumped into tank 210 and then pumped from tank 210 to product storage tank 216 by pump 2.
Send immediately on 14. At that time, valve 212 is also opened. 3rd b
3d and 3f, the pump 220 is shown open to return liquid from the lower part of the furnace 16 to the upper portion of the furnace 16 of the vessel 10.

This is for optimal treatment of the liquid during absorption of protein substances in ion exchange media, optimal utilization of wash water during washing and optimal enrichment of the product solution during regeneration of ion exchange media. be. The illustrated container is of the type having a sufficiently concave bottom to withstand internal pressure. It is also possible to use flat bottom containers. In that case, the furnace can be installed near the bottom if the bottom has sufficient strength. In that case, forced circulation is not necessary since the amount of the furnace under the furnace is small. The interaction between the liquid and the ion exchange medium is enhanced by natural circulation through the furnace. All processing takes place inside the vessel 10, and the ion exchange medium remains contained within the vessel for the entire duration of the process. In this way a particularly simple device is obtained which has the advantage that the energy required is reduced, since the ion exchange medium is not transferred from one container to another. 0 The device shown in FIGS. 2 and 3 uses the container shown in FIG. 1 and represents the simplest single module device.

Due to the lid air pressure applied to the furnace 16 and the throughput requirements, the basic dimensions of the vessel are approximately 8 feet in diameter and height. A basic module of such size can, for example, process about 46 kiloliters (about 10,000 gallons) of milk bran per day. A typical plant uses six modules, resulting in a throughput of about 60,000 gallons per day. Washing subsequent to loading the ion exchange medium with protein material is important to wash out protein material that is not absorbed by the ion exchange medium.

These protein substances are usually latactose and crude protein substances. Also, any untreated liquid that has adhered to it is washed away at this stage. In another example of this device (not shown), the furnace can be used only in part of the bottom of the vessel, for example in the middle part. In addition, the upper end of the furnace is flat.
It can be in the form of a cylindrical low vertical annular filter screen closed with a flat horizontal filter screen. This cylinder extends a height of no more than about 10 to 15 inches (about a few inches) or about 30 inches (about 1 foot) from the overall height of the bottom of the container. In this case, the bottom of the container can be flattened as a whole. FIG. 4 shows a reaction vessel 250.

The reaction vessel 25 includes a water lamp 251, a furnace 252, a liquid level controller or load cell 253, and a probe 254 for monitoring the pH value of the liquid within the vessel. The upper end of the container 250 has a liquid supply port 260 controlled by a valve 262, a compressed air supply port 264 controlled by a valve 266, a wash water supply port 268 controlled by a valve 270', and a wash water supply port 268 controlled by a valve 2741. an acid supply port 272 controlled by a valve 278, an alkali supply port 276 controlled by a valve 278, and a discharge liquid supply port 2 controlled by a valve 282.
80 are provided. An upper discharge valve 284 is also provided on the vessel 25 for discharging compressed air after each liquid discharge stage. The lower part of the vessel 250 is provided with a wash water circulation outlet 286 controlled by a valve 288, a valve 290 for draining to a drain, and a valve 292 for recycling the discharged eluate or protein-rich regenerant. .

Tanks 293, 294, and 295 are respective storage tanks.

All processing takes place inside container 250.

The order of this processing is as follows. First, assume that the container 250 contains a fine fibrous ion exchange medium that is ready to maximize protein absorption from lactic acid. Untreated liquid lactic acid is pumped from tank 293 by pump 400 to container 250 to the level of the upper level controller.

At the same time, acid is added to the lactic acid in the container 250 in order to maintain the ion exchange base value correctly at 3. Then the Fly Azusaki 25
1 to mix the liquid and ion exchange medium at the correct pH conditions.

The proteins in the liquid are then absorbed into the ion exchange medium. This processing step is the first stage of lactic acid processing. The protein content of the liquid in container 10 is then significantly reduced and can be passed to a drain via outlet 286 and valve 290, or to an intermediate tank if more than one absorption stage is required. (not shown). The compressed air is then supplied to the container 25 through the valve 266 and the supply port 264.
0 to facilitate filtration of liquid from the ion exchange medium. Then, from the tank 294, the pump 402
The cleaning water is supplied to the container 2 through the valve 270 and the supply port 268.
Put it in 50.

This wash water is water that has been previously used and stored in a tank to reduce water usage. The evaporator 251 is then operated to mix the water and ion exchange medium to dilute and wash out undesirable substances, such as lactase, from the ion exchange medium. This water is discharged from the scarlet outlet through valve 290. A portion of the drained water can be returned to tank 294 through pipe 416 and valve 288. Air pressure is applied to the liquid level inside container 250 to direct water to tank 294 . Excess water is routed to a drain through valve 290. If desired, further washing steps can be provided to bring the ion exchange medium to the desired condition. This washing step is carried out with direct flow or countercurrent flow. The partially exhausted regeneration solution is then pumped 403 from tank 295.
through the tube 404, the valve 282, and the supply port to the container 2.
Put it in 50. The condenser 251 is then activated to mix the ion exchange medium and regeneration solution, completing the first stage of ion exchange medium regeneration. The regenerant transfers the protein into solution so that the ion exchange medium loses the protein and is completely regenerated. The exhausted regeneration solution is routed through outlet 286, line 418, and valve 292 to tank 295. In this case, compressed air is blown into the container 250 to provide a moving force to the liquid level. 0 Tank 295 has an outlet 450 for passing the protein-rich regeneration solution to a later stage.

After draining some of this solution from tank 295, tank 295 is filled with fresh caustic sotada liquid to restore the concentration of regenerant in the liquid inside tank 295.
In this case, the regeneration solution will contain a relatively small amount of protein. The ion exchange medium is thus ready to interact with the raw feed coming from tank 293, as described at the beginning of the cycle, and the cycle is repeated using the same ion exchange medium. You will be able to give back. Eventually, the ion exchange medium becomes less capable of ion exchange. It is then necessary to completely remove the ion exchange medium from container 250 through outlet 452 and valve 454. Fresh ion exchange media can then be introduced into the container 250 through the capped top entrance (not shown).

In this case, it can also be pumped into the container 250 in the form of a slurry. A typical sequence of operations for the method performed by the apparatus shown in FIG. 4 is as follows, and takes approximately three hours to complete the operating cycle.

1. Mix the liquid to be treated with the ion exchange medium for 15-20 minutes.

2. Allow the liquid to drain for 5-10 minutes.

3 Inject the wash water for 5 minutes.

4 Mix the wash water and ion exchange medium for 1 minute.

5. Drain the washing water for 5 to 1 minute.

6 Inject the regenerant or release liquid for 5 minutes and add alkali to bring the pH to 9.

7. Mix the regeneration solution with the ion exchange medium to release the protein from the ion exchange medium - 15 to 2 hours.

8. Allow the regenerant to drain - 5-10 minutes.

9 Put the milk bran before treatment at pH=6 for 5 minutes.

At the same time, add acid to adjust the pH to 3. To maintain good hygiene, it takes approximately 3 hours per day to completely remove proteins from the ion exchange medium using caustic soda solution.

This is ``cleaning place''.
” is known as.

Therefore, the processing can be performed in approximately 7 cycles per mark.
FIG. 5 shows an apparatus for carrying out a second embodiment of the method of the invention.

The apparatus uses five containers RI-R5 similar to container 10 shown in FIG. 6 storage tanks HTI~HT
6 is provided, and pumps P1, P2, and P3 are attached to tanks HT1, HT2, and HT3, respectively.

These pumps are configured to send liquid from the tank through the pipeline and control valve CV to the upper inlet of the reaction vessel. The outlet provided at the bottom of the container is connected to the tanks HTI to HT via another pipe, a control valve CV, and a manual control valve V.
Connected to the upper entrance of 4. A water supply pipe 320 is connected to the upper inlet of the reaction vessel, and an effluent supply pipe 322 is connected to the upper inlet of the reaction vessel via a pump 324.

The tank HT6 has a water supply pipe 326 and a water level controller 32.
8,330.

The outlet from tank HT6 is connected to the upstream side of pump PI. Tank HTI has an overflow outlet into tank HT5, the bottom of which is provided with a drain for the protein-rich liquid. The outlet at the bottom of tank HT4 is discharge pipe 3.
32.

In FIG. 5, CV indicates an automatic control valve, and V indicates a manual valve used in an emergency and during setting. For ease of illustration,
An air supply pipe, an acid and alkali supply pipe for bait adjustment,
The new regenerant supply line and the complete water circulation system are not shown. Since the method carried out inside each tank is similar to that described with reference to FIG. 4, reference is only made to FIG. 6 which shows the complete operating cycle for the method.
I can understand the method.

In Figure 6, part of the liquid inside tank HTI is
It should be noted that fresh regenerating liquid, such as caustic soda liquid, is added to the remaining liquid sent to T5 before being sent from tank HTI to the reaction vessel.

If required, water from tank HT6 can be added to the liquid from tank HTI and sent to the reaction vessel. Tank HTI always contains a protein solution in the regenerant, the protein content of which is either maximum or minimum.

Tank HT2 always contains partially treated feed liquid.
Tank HT3 always contains partially exhausted regeneration liquid. Tank HT4 always contains fully treated effluent, which is intermittently drained to a drain through tube 332. Pumps P1, P2, P3 are tanks HT1, HT2
, HT3 to containers R1, R29, R3, R4, and R5 as necessary. Air pressure pumped into the space above the liquid in the container moves the liquid from the container to the tank HTI~
Used to send to HT4. FIG. 7 shows yet another embodiment of the invention.

In this example, five containers RI to R5, two storage tanks HT1 and HT2, and five feed cones CI to C5 are used. In this embodiment, the ion exchange medium is moved between the reaction vessels in a direction opposite to the flow direction of the liquid to be treated.

In Figure 7, the solid lines represent pipelines for transporting liquid from tank to container or from container to tank, and the dashed lines represent pipelines for transporting ion exchange medium and liquid slurry from container to cone or from cone to container. Represents a pipeline.
Further, the dash-dotted line represents a pipeline that sends compressed air to or discharges compressed air from the container to push the liquid out of the container. Next, the operation of this device will be explained.

First, the liquid to be treated is introduced into the container RI through the valve V6, and the liquid is mixed with the partially exhausted ion-exchange medium by means of a stirrer, so that the ion-exchange medium absorbs the proteins sufficiently. Therefore, the protein content in the input liquid is reduced (i.e., the first step of protein removal is
A step has been taken. ) The slurry of ion exchange medium and liquid is then conveyed with compressed air to cone C3.

Most of the slurry sent is immediately sent to container R3.
The protein-enriched ion exchange medium remains in container R3. The liquid is transferred with compressed air from container R3 through valve V15 to tank HTI. Then pour the liquid into container R2Z.
and where it is mixed with a fully regenerated (ie protein-free) ion exchange medium to perform the second step of protein removal from the liquid. Tank R
The compressed air in V24 is sent to the exhaust valve V24 through a pipe indicated by a dotted line. The slurry is then pneumatically delivered to cone CI.

The delivered slurry immediately enters the container RI. Then open V13 and the fully treated liquid will drain to the drain. At this time, compressed air is used to apply pressure to the slurry in the container to aid in filtration. The partially exhausted ion exchange medium, which does not contain enough protein, is retained by the furnace inside vessel R1. The protein-rich ion exchange medium remaining in vessel R3 is transferred to the reaction stage and vessel R2.
Wash with water during the second stage of protein removal from the liquid.

Next, the slurry of water and ion exchange medium is pneumatically pumped into the cone C.
4, and from there, immediately put it in container R4 for further worship. From there, valve V16 is opened to allow the wash water to escape with compressed air, and the protein-enriched ion exchange medium is retained by the filter in vessel R4. The partially exhausted regenerant (i.e. containing some protein) is then sent from tank HT2 to vessel R4 and mixed with the ion exchange medium to completely consume the regenerant (i.e. containing some protein). completely absorb the protein present).

In this way, the first stage of protein removal from the ion exchange medium is performed and a large portion of the ion exchange medium is regenerated. The slurry of ion exchange medium and liquid is then pneumatically delivered to cone C5 and then to container R5. Valve V17 is then opened to pneumatically send the protein-rich regeneration liquid to tank 500.

Tank 50 is equipped with a bell controller 501 for controlling the level of fresh regenerated liquid, such as caustic soda liquid, and a flow pipe 502, so that the liquid containing a large amount of protein can be sent to the next stage of processing. It has become. Next, add fresh caustic soda solution to reduce the protein concentration. Next, fresh regeneration liquid from tank 300 is placed into container R5 and mixed with the ion exchange medium to perform the second stage of regeneration of the ion exchange medium, ie protein removal.

The slurry is then sent to cone C2 via valve 22;
From there it is sent to container R2.

Then, the valve V14 is opened and the partially exhausted regeneration liquid is sent to the tank HT2 by applying air pressure. In this way, the ion exchange medium is completely regenerated. The partially exhausted regeneration fluid contains the last of the proteins from the initially considered input processing fluid.

This regeneration liquid is sent from tank HT2 to vessel R2 where it is mixed with the ion exchange medium containing proteins from the next input liquid to be processed. Finally, the regenerating solution containing sufficient protein is added to the cone C5 using air pressure along with the ion exchange medium.
via to container C5. The regeneration liquid is then separated from the ion exchange medium and then passed through valve V17 to tank 5.
Send to 00. This completes the removal of proteins from the input processing solution.

FIG. 7 shows the three processing stages as follows. First stage:
Interaction takes place at this stage. That is, container RI
The first stage of protein absorption by ion exchange between the processed input process liquid and partially exhausted ion exchange medium; partially processed process liquid and fully regenerated ion exchange medium in vessel R2 a second stage of protein absorption by ion exchange between; washing the ion exchange medium in vessel R3;
A first stage of protein removal from the ion exchange medium by ion exchange with the regeneration liquid in vessel R4; a second stage of protein removal from the ion exchange medium by ion exchange with the regeneration liquid in vessel R5 are carried out sequentially. Condition 1 Cones CI, C2, C3, C4, C5 - empty.

2 Liquid tanks HT1, HT2 - filled.

3. Eluent (regenerant) supply device - filled.

motion 1 All valves are closed.

2 Valve V6, V7, V8, V9, VI0, V24 open.

3 Level controllers in vessels R1, R3, R5 determine the start of the reaction period. 4 Activate the lily pad.

5. Start of operation for reaction period.

6 All valves are closed.

The washing step removes unwanted lactose and other soluble contaminants and loose particles from the ion exchange medium.

This method is a 2:1:2 method. Stage 2: This stage transports the ion exchange media slurry from one cone to the vessel and from the vessel to the cone.

This stage consists of two parts. First partial state 1 All reaction products are in containers R1, R2, R3, R4,
Present in R5.

2 Processing liquid tanks HT1 and HT2 are empty.

operation 1 All valves are closed.

2 valves V18, VI9, V20, V21, V22, V2
Open 3.

3 Activate the hawk rig.

4 After sending all the air (P of air pipe pressure), close all valves.

Second partial state 1 All reaction products are cones C1, C2, C3, C4
exists within.

2 Processing liquid tanks HT1 and HT2 are empty.

3 Containers R1, R3, R4, and R5 are empty.

operation 1 All valves are closed.

2 Open valve V24.

3 Open valves V1, V2, V3, V4, and V5.

4 Operate the rope rig.

5 Close all valves after complete discharge.

Stage 3: In this stage, the liquid in the container is partially transferred to a storage tank and from there to the container. State 1 All reaction products are in containers R1, R2, R3, R4,
Present in R5.

2 Cones CI, C2, C3, C4, and C5 are empty.

Operation 1 Close all valves.

2 Open valves V13, V14, V15, V16, and V17.

3 Open valve V23.

4 Stop the hawk trunk.

5 After sending all the water (pipe pressure P), close all valves.

In FIG. 7, the storage tank is positioned higher than the container so that liquid flows from the tank by gravity. In the method described above, the ion exchange medium is handled in such a way as to minimize deterioration of the quality of the ion exchange medium due to depletion and pressure.
The ion exchange medium can either not be removed at all from the container where it reacts with the liquid, or it can be delivered to the cone using air pressure. However, the ion exchange medium remains in the cone only for a short time. Little or no sticking of the ion exchange medium occurs inside the cone, and the slurry of ion exchange medium is transferred very quickly to the next vessel, where it is again concentrated to maintain its optimal physical properties. to be maintained. This is particularly important for fibrous ion exchange media. Further information on this type of ion exchange media and its use can be found in The Viscose Development Ltd., UK.
pmentCompanyLimi can receive information from d). The company supplies this type of ion exchange media under the trade name VISTEC. Cationic and anionic ion exchange media are available, and the method described above uses intestinal ionic media to recover proteins contained in milk bran. Whether the purpose is to purify the liquid to make it possible or to recover valuable organic matter contained in the liquid, such as proteins, enzymes, or other macromolecular substances, many Can be generally applied to liquid processing. A reactor vessel as described above with a furnace at the bottom has been tested and found to operate satisfactorily for 2000 cycles using 50 mesh wire cloth.

In place of the wire cloth described above, the wedge-shaped wire sieve described above or other types of washing filters may be used. As mentioned above, no further treatment of the protein-rich liquid discharged from the product tank was described, but it is sufficient that the solution can be concentrated by ultrafiltration or evaporation.

In the case of evaporative concentration, removal of impurities by crystallization may be required prior to final evaporation and drying. Impurities can be removed from the protein in the ultra-furnace, and the product can also be washed in the ultra-furnace if necessary. If necessary, the liquid can be pretreated to remove coarse particles, fats, and other components that may reduce the efficiency of ion exchange and cleaning.

The above discussion has not addressed the periodic cleaning operations necessary to ensure that the operations and reactions are conducted in clean and sanitary conditions to ensure that the recovered proteins are safe and free from harmful contamination.

This is typically necessary in the case of factory processed lactic acid. The method described with reference to Figure 6 requires continuous monitoring or laboratory monitoring of the physical, chemical, biological and other properties of the ion exchange medium since the ion exchange medium is repeatedly removed from the reaction vessel. Another advantage is that inspection can be easily performed. This means that extremely high safety standards can be maintained. The ion exchange medium can be easily removed and replaced if necessary during operation of the device. For example, about 270 kiloliters (about 60,000 gallons) of liquid can be processed using the method described above.

It has been described that air pressure is applied above the slurry in a reaction vessel with a furnace at the bottom to facilitate drainage of liquid through the furnace. Furnace filtration can also be performed using negative pressure, that is, vacuum, instead of positive pressure. The method of the invention described above by way of example can be modified to vary the number of protein absorption steps, protein removal steps from the ion exchange medium, or washing steps of the ion exchange medium.

If necessary, the medium can also be cleaned after regeneration of the ion exchange medium. It is also possible to carry out many different operating patterns using one or more bottom-mounted furnace vessels of the type described above.

In that case, the ion exchange medium may be entirely fixed within the container, or it may be exchanged between several containers. Alternatively, the ion exchange medium may remain in one vessel for one or more stages or may be transferred to a separate vessel for each stage of operation. In the methods described above, the ion exchange medium may be separated from the liquid in the same vessel in which the interaction takes place, or the ion exchange medium may be separated from the liquid before it is sufficiently exhausted. In the method described with reference to Figure 7, the basic sequence of operations is: loading the slurry, moving the slurry, separating the liquid from the ion exchange medium, and moving the liquid into the container into which the slurry is sent. It is sending. Slurry maintenance, furnace heating in the same container to separate the liquid from the ion exchange medium, feeding the liquid into the same container,
Other methods of feeding the resulting slurry, such as pouring, and using a top layer, are also possible. In the method described above, the various control valves can be operated automatically under the control of a programmable master controller.

As mentioned above, a manually operated valve is also required, but the automatically operated valve is omitted in FIG. 7 to simplify the illustration. Although controllers for monitoring the pH value and controlling the liquid level have been described, it is possible to incorporate these controllers and other necessary controllers into the automatic controller.

[Brief explanation of drawings]

Figure 1 is partially cut away to show the internal structure.
FIG. 2 is a schematic perspective view of a typical reaction vessel-shaped apparatus used in carrying out the method of the present invention; FIG. a schematic diagram illustrating successive steps of the method carried out using the apparatus shown;
FIG. 4 is a schematic representation in flow diagram form of another embodiment of an apparatus that can be used to carry out the method of the invention; FIG. , FIG. 6 is an operating stage chart showing the relationship of operating cycles over time in the containers constituting the apparatus of FIG. 5, and FIG. 1 is a schematic diagram showing an example. 10, RI~R5... Container, 12,251...
...Taka Azusa, 16,252... Furnace, 220
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Claims (1)

[Claims] 1. Mixing a fibrous ion exchange medium and a liquid containing protein by stirring, then separating the ion exchange medium from the liquid, then mixing the ion exchange medium and a regenerant by stirring, and then A method of performing ion exchange between a fibrous ion exchange medium and a liquid containing protein, in which the ion exchange medium and the regenerating agent are separated, and the ion exchange medium and the liquid are separated and then washed with the ion exchange medium. mixing the liquid by stirring, then separating the ion exchange medium and the cleaning liquid, all mixing processes, all ion exchange processes,
The entire separation process is carried out in at least one vessel 10 comprising a filter 16 and a stirrer 12 above the filter;
An ion exchange method characterized by applying an air pressure differential on both sides of the filter 16 to aid in the separation of the ion exchange medium from one of the liquids. 2. The method according to claim 1, in which all mixing steps, all ion exchange steps, all washing steps, and all separation steps are performed in the same container. 3. The method according to claim 1, which includes a step of mixing a liquid containing protein with an ion exchange medium, an ion exchange step for enriching the ion exchange medium, and a step of mixing the liquid containing protein with an ion exchange medium, and removing the liquid from the ion exchange medium. a process of separating, a process of mixing the ion exchange medium and the cleaning liquid, a process of cleaning the ion exchange medium, a process of separating the cleaning liquid from the ion exchange medium, a process of mixing the regeneration liquid with the ion exchange medium, and a process of regeneration. A method of using several similar vessels 10 for enriching the liquid, ion-exchanging it to regenerate the ion-exchange medium, and separating the regeneration liquid from the ion-exchange medium, respectively. 4. In the method according to claim 1, several similar containers 1
0 to mix the ion exchange medium with the protein-containing raw liquid inside the first container R1, then place the fully loaded ion exchange medium into another container R3, and in this container R3. The ion exchange medium is separated and mixed with the washing liquid by stirring for washing, and then the ion exchange medium is placed in another container R4, in which the ion exchange medium is mixed with the washing liquid to separate the protein from the ion exchange medium. and then put the ion exchange medium into another container R5 in which the ion exchange medium is separated from the regeneration liquid and the fresh regenerant is mixed into the ion exchange medium by stirring. A second step of separating the proteins from the ion-exchange medium is carried out, after which the ion-exchange medium is transferred to another container R.
The liquid, which has already lost some protein in R1, is mixed with the ion exchange medium by stirring to carry out a first step of loading the ion exchange medium, and then the ion exchange medium is returned into the first container R1. How to complete the cycle.