Method for treating a fluid, in particular a beverage
09670441 · 2017-06-06
Assignee
Inventors
- Martin Zeiler (Schwäbisch Gmünd, DE)
- Ralf Ascher (Alfdorf, DE)
- Roland Müller (Waldstetten, DE)
- Harry Frison (Schwäbisch Gmünd, DE)
Cpc classification
International classification
Abstract
A method for treating a fluid is provided using a particulate material in the form of a deposited layer having an upstream side and a downstream side wherein a flow of the fluid is directed through the deposited layer from the upstream to the downstream side at a first temperature. The method includes reconditioning the deposited layer and then resuming treatment of the fluid, wherein reconditioning comprises heating the deposited layer to a second temperature; and cooling the deposited layer to a third temperature at an average cooling rate in the range of up to about 20 C./min.
Claims
1. A method for treating a fluid, the method comprising: providing a particulate material in the form of a deposited layer having an upstream side and a downstream side; starting treatment of the fluid by directing a flow of the fluid through the deposited layer from the upstream side to the downstream side at a first temperature; reconditioning the deposited layer; resuming treatment of the fluid; wherein the reconditioning comprises heating the deposited layer to a second temperature; and cooling the deposited layer to a third temperature at an average cooling rate in the range of up to about 20 C./min.
2. The method of claim 1, wherein the reconditioning comprises directing a flow of a reconditioning fluid through the deposited layer.
3. The method of claim 2, wherein the reconditioning fluid serves as a coolant while cooling the deposited layer, the reconditioning fluid being optionally circulated through a cooling device.
4. The method of claim 3, wherein the cooling rate is determined as the temperature of the reconditioning fluid serving as a coolant exits the deposited layer at the downstream side thereof.
5. The method of claim 2, wherein the reconditioning fluid serves as a heating medium for the deposited layer when heated to the second temperature, the reconditioning fluid being optionally circulated through a heating device.
6. The method of claim 1, wherein the reconditioning of the deposited layer comprises incorporating an additive into the deposited layer.
7. The method of claim 1, comprising packing the particulate material into a cartridge with a density higher than the bulk density of the particulate material in the wet state to form the deposited layer.
8. The method of claim 1, wherein the particulate material comprises particles with a particle size of less than 25 m in an amount of about 15% by weight or less.
9. The method of claim 1, wherein the particulate material comprises particles which are swellable in the fluid to be treated.
10. The method of claim 1, wherein the particulate material comprises particles in the form of beads.
11. The method of claim 1, wherein the particulate material comprises particles selected from agarose, PVPP, PA, zeolite, activated carbon, and/or diatomaceous earth.
12. The method of claim 1, wherein the particles of the particulate material are selected from compressible particles.
13. The method of claim 1, wherein the treatment comprises adsorption, filtration, doping and/or subjecting the fluid to a reaction.
14. The method of claim 1, wherein a multiplicity of deposited layers is provided in a common housing having an inlet communicating with the upstream sides of the deposited layers and an outlet communicating with the downstream sides of the deposited layers.
15. The method of claim 14, wherein heating the deposited layer comprises introducing the reconditioning fluid into the housing at its bottom end and/or wherein cooling the deposited layer comprises introducing the reconditioning fluid into the housing at its top end.
16. The method of claim 3, wherein the reconditioning fluid serves as a heating medium for the deposited layer when heated to the second temperature, the reconditioning fluid being optionally circulated through a heating device.
17. The method of claim 4, wherein the reconditioning fluid serves as a heating medium for the deposited layer when heated to the second temperature, the reconditioning fluid being optionally circulated through a heating device.
18. The method of claim 7, wherein the initial density of the packed particulate material of the deposited layer corresponds to up to about 120% of the bulk density in the wet state.
19. The method of claim 18, wherein the initial density is about 101% or more of the bulk density in the wet state.
20. The method of claim 13, wherein the treatment comprises subjecting the fluid to a catalytic reaction.
21. The method of claim 1, wherein the fluid being treated comprises a beverage.
22. The method of claim 21, wherein the beverage comprises beer, wine, or fruit juice.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
(1) In the Figures
(2)
(3)
(4)
(5)
(6)
(7)
(8)
DETAILED DESCRIPTION OF THE INVENTION
(9)
(10) The arrangement 10 includes a housing 12 accommodating a cartridge 14 in which a layer of particulate material (not shown) has been deposited. The housing 12 comprises a fluid inlet 16 at the top and a fluid outlet 18 at the bottom thereof.
(11) Of course, housing 12 may be provided with larger dimensions such that it may accommodate a stack of a multiplicity of cartridges 14.
(12) The fluid inlet 16 is connected to a pipe 20 which provides a fluid flow path from inlet 16 to a pump 22, e.g., a flow-controlled centrifugal pump.
(13) Pipe 20 is preferably equipped with a flow-meter 24, a temperature sensor 26 and a pressure sensor 28 which allow monitoring the temperature, pressure and flow rate of the fluid fed via pump 22 and pipe 20 to inlet 16 and the upstream side of the deposited layer of particulate material accommodated in cartridge 14.
(14) The outlet 18 is connected to a pipe 30 which leads to a heat exchanger 32 which is connected via a pipe 34 to the inlet of pump 22 thereby forming a closed loop.
(15) Pipe 30 connecting the outlet 18 with the heat exchanger 32 is equipped with a temperature sensor 36 and a pressure sensor 38 which allow monitoring of the downstream pressure of the reconditioning fluid circulated through cartridge 14 as well as its downstream temperature.
(16) Once cartridge 14 has been placed into housing 12, the same is closed and the closed loop constituted by pump 22, pipe 20, housing 12 with cartridge 14, pipe 30 and the heat exchanger 32 and tube 34 is filled with a reconditioning fluid which preferably has already an elevated temperature via valve V1.
(17) Pipe 20 includes close to inlet 16 a branch 40 which can be connected to pipe 20 and inlet 16 or shut off via valve V5. Upstream of branch 40 pipe 20 includes a shut-off valve V3 and a further branch 42 connectable to pipe 20 via a valve V4.
(18) Pipe 30 may be shut off by a valve V7. Upstream of valve V7 pipe 30 may be connected to a branch pipe 44 via a shut-off valve V6.
(19) When filling the closed loop with the hot water, at the beginning of the reconditioning, valves V1, V3, V4 and V5 are open so that air contained in the closed loop may be withdrawn and an initial amount of reconditioning fluid may be dumped through branch pipe 44 while valve V6 is open. Subsequently, valve V7 is opened and the loop completely filled. The valves V4 and V5 will be closed and the heating step by passing the reconditioning fluid through a deposited layer in cartridge 14 may start.
(20) During an initial phase of the heating step, valve V6 may remain open to discharge a fraction of the recycling reconditioning fluid which is replaced by fresh fluid supplied via valve V1 into the loop. This procedure allows to dump fractions of reconditioning fluid which may at the beginning of the reconditioning of the deposited layer be heavily loaded with matter desorbed from the particulate material in cartridge 14.
(21) Thereafter, valves V1, V2, V5 and V6 remain or are closed whereas valves V3 and V7 are open.
(22) The pressure and temperature sensors 36 and 38 monitor the condition of the reconditioning fluid when exiting housing 12. The fluid is then fed into heat exchanger 32 where the fluid is again heated to a pre-set temperature.
(23) To that effect, the heat-exchanger is connected via valves VVL2 and VRL2 to a heating device (not shown) for circulating a heating medium (e.g., hot water) through the heat exchanger 32 and its heat exchange pipe 33. Once the temperature sensor 36 indicates that the deposited layer has been heated to the targeted second temperature, the valves VVL2 and VRL2 are eventually closed and reopened as necessary to maintain the temperature of the reconditioning fluid at the second temperature.
(24) After a pre-set time which preferably ensures that the deposited layer is in a sterile condition, the heat exchanger is connected to a cooling device (not shown) and the valves VVL1 and VRL1 are opened in order to circulate a cooling medium through the heat exchange pipe 33 of heat exchanger 32.
(25) Subsequently, the cooled reconditioning fluid is circulated in a closed loop constituted by pump 22, pipe 20, housing 12 with cartridge 14, pipe 30, heat exchanger 32 and pipe 34. The cooling rate is monitored via temperature sensor 26.
(26) The cooling rate of the deposited layer furthermore is monitored by temperature sensor 36 connected to pipe 30 close to the outlet 18 of housing 12. This temperature sensor 36 indicates the cooling rate of the deposited layer within cartridge 14.
(27)
(28)
(29) At the outer periphery of bottom wall 60, a side wall 66 is attached, e.g., in a welding step.
(30) The side wall 66 is running around the whole of the periphery of bottom wall 60 so as to define a chamber 70 which accommodates the particulate material in the form of a deposited layer.
(31) The bottom portion of the volume 70 is covered by a mesh material 72 having openings small enough to retain the particulate material of the deposited layer and being nevertheless pervious for the fluid to be treated and for the reconditioning fluid or fluids to be used upon reconditioning of the deposited layer.
(32) The mesh material 72 covers essentially all of bottom wall 60 and extends to the central opening 62. When mounting the hub 64 on the bottom wall 60, the mesh material 72 is clamped in between the hub 64 and the bottom wall 60, thereby allowing drainage of volume 70 into the central channel defined within hub 64.
(33) The top surface of cartridge 14 may be left open, in case the cartridge is filled and operated in a horizontal position. For practical reasons it is preferred to close the top of cartridge 14 with a disk-shaped cover made of a mesh material 76 which is fixed to the side wall 66, e.g., by welding so as to close the upper end of volume 70 and to retain the particulate matter within volume 70. The mesh material 76 is attached to an upper portion of hub 64 so as to avoid a fluid flow directly from the uppermost portion of volume 70 into the central channel of hub 64. The mesh material 76 may be removably attached to sidewall 66 and the hub 64.
(34) The side wall 66 of cartridge 14 is provided with an inlet 80 which is closed by a plug 82 once the volume 70 of cartridge 14 has been filled to the desired extent with particulate material.
(35) The central hub 64 not only serves as an outlet for cartridge 14, but also to fix the mesh material 72 and 76 in the central portion of cartridge 14. In addition, it may be designed at its upper and lower surface portions so as to accommodate corresponding cartridges when the cartridges are stacked on top of one another to form a multi-cartridge stack as described before.
(36) While the cartridge 14 and its various parts may be made of metal and may be used in multiple cycles with the particulate material replaced in volume 70, it is also conceivable to make the cartridge 14 from plastic parts which are filled once and are discarded together with the consumed particulate material at the end of its life cycle.
(37) The dimensions of the cartridges used in the examples described in connection with the invention have an inner diameter of about 540 mm and a filling height of about 30 mm, the inner diameter of the hub 64 is about 65 mm, the outer diameter of the hub is about 116 mm. Volume 70 provided by such cartridge amounts to about 6.5 I.
(38)
(39) To that extent, the arrangement 100 comprises a tank 102 equipped in its upper portion with an inlet 104 and in its bottom part with an outlet 106. Furthermore, in the bottom portion of tank 102, an agitator 108 is provided which allows stirring the contents of tank 102, e.g., a suspension of a particulate material to be filled into the cartridges 14.
(40) The cartridges 14 are positioned in a vertical standing position and connected with their inlet openings 80 to a filling pipe 110 which receives the suspension contained in tank 102 via centrifugal pump 112.
(41) Filling pipe 110 is equipped with one or more pressure sensors in order to monitor the inlet pressure during filling of the cartridges 14. The inlet pressure monitored by the sensors 112 determines the degree of packaging of the particulate material within the cartridges 14.
(42) In case a swellable particulate material like PVPP is used the particles first of all are allowed to absorb the surrounding fluid, e.g., water. For PVPP particles a swelling time of about 4 h is sufficient, more preferable are swelling times of about 10 h. The suspension comprises preferably about 2 to 10% by weight, more preferably about 3 to about 5% by weight of PVPP particles. The suspension is then stirred in the tank 102 and subsequently circulated in the loop by the centrifugal pump 112 for about 15 min without filling the cartridges at a flow rate of about 4 m.sup.3/h. Depending on the particulate material and the specific equipment used fine-tuning of the flow rate may be advisable so as to avoid deposition and/or fractionating of particles in the loop. Subsequently the cartridges may be connected to the loop via the ball valves 118 and feed lines 120.
(43) In the beginning of filling of the cartridges 14, the fluid suspending the particulate material exits the cartridges 14 via their top wall 76 and hub 64. Upon successive filling of the cartridges 14, the amount of fluid exiting the cartridges 14 becomes smaller until it nearly stops at the end of the filling procedure when a sort of plug of particulate material has been created at the inlet 80 of the cartridges 14.
(44) Downstream of the filling pipe, a valve 116 is provided in the loop which may be used to adjust the filling pressure which is sensed at the filling pipe 110 at one or several positions. The pressure sensors 112 indicate the pressure under which the cartridges are filled and determine the filling degree or packing of the individual cartridges. Preferably, the pressure differential for filling the cartridges 14 is about 0.3 bar.
(45) It is important to fill the cartridges 14 with the particulate material free of voids.
(46) Typical filling times may be in the range of about 20 to about 30 min for cartridges 14 as shown in
(47) The cartridges 14 are then disconnected from the filler pipe 110 and the inlets 80 in the side wall 66 of the cartridges 14 are closed with blind plugs 82.
(48) In case a pre-compressed PVPP layer is wanted within the cartridges 14, preferably PVPP and a certain amount of a filler material soluble in water is filled into the cartridges 14 in a dry state. Upon passing a flow of water through the cartridges and rinsing out the filler material, the PVPP particles will swell and generate a pre-compressed filter cake within the cartridge 14. As water-soluble filler materials, especially food-compliant materials, e.g., salts and sugars, can be used.
(49) Taking into consideration the swelling effect obtained with PVPP of about 1.4 times of its dry volume, the amount of filler has to be calculated in order to avoid inadmissible overfilling or overpacking of the cartridge 14 and the creation of a too high pressure difference during the following step, namely the use of the cartridge 14 for stabilizing the beverage.
(50) It is recommended to do some pre-tests on a laboratory scale in order to find out the optimum percentage for a certain filler material to be admixed with PVPP particles.
(51)
(52) In order to demonstrate the effect of the present invention upon reconditioning of the deposited layer, a layer made of PVPP particulate matter has been voluntarily cracked as will be described below.
(53) After filling of the cartridge 14, the deposited layer obtained has been voluntarily cracked by repeated start-stop fluid-flow cycles and additionally been damaged by introducing compressed air (cf.
(54) Thereafter the cartridge 14 comprising the damaged deposited layer 140 has been subjected to the following conditions:
(55) The top of cartridge 14 as shown in
(56) In an initial step the reconditioning arrangement is filled with cold water having a temperature of 2 C., corresponding to the first temperature at which typically a beverage like beer is stabilized. The cold water is recirculated for about 10 minutes in order to determine the pressure differential of the cracked deposited layer. The value of the pressure differential measured is 0.73 bar at 2 C. and a flow rate of the cold water of 0.59 m.sup.3/h.
(57) Thereafter the temperature of the recirculated water is increased at a rate of about 6 C./min until the temperature at the outlet of the housing 12 (as determined by temperature sensor 36) is about 70 C. (fourth temperature). The flow rate is kept constant at 0.59 m.sup.3/h.
(58) The temperature is further increased at a gradually lowered rate to the second temperature of 85 C. The treatment of the deposited layer at a temperature of 80 C. or more is continued for about 20 min at still the same flow rate of the recirculated water of 0.59 m.sup.3/h. Subsequently the deposited layer is cooled at a controlled cooling rate of about 5.5 C./min to a third temperature of about 20 C.
(59)
(60)
(61) During the first step of recirculating cold water in the closed loop of arrangement 10 the pressure differential arrives at a plateau value of 0.73 bar within a few minutes. Upon heating the deposited layer 140 in cartridge 14 the particulate PVPP material expands resulting in a less dense structure and the pressure differential drops to about 0.15 bar.
(62) Upon controlled cooling of the deposited layer 140 the structure thereof becomes again more dense and the pressure differential steadily increases up to a level of 0.77 bar or more, i.e., significantly above the value determined at the beginning for the cracked deposited layer (0.73 bar) indicating curing of the cracks 142.
(63) When the cartridge is removed from housing 12 and the mesh cover 76 has been removed the reconditioned deposited layer 140 can be visually evaluated. As is shown in
(64) Damages as severe as shown in
(65) The importance of selecting a suitable particulate material for forming the deposited layer in cartridge 14 has been explained above in some detail.
(66) In the case of PVPP, a typical particle size distribution of commercially available PVPP regenerable food grade particulate material is shown in
(67) Upon suspending of the original PVPP particulate material available on the market in an amount of about 5% by weight one or several times in water and decanting the supernatant after a settling time of about 4 h, a particle size distribution according to curve B can be obtained. In contrast to the particle distribution according to curve A, the particle distribution according to curve B shows a significantly improved behavior with regard to pressure drop.
(68) Other particle distributions which will work well are demonstrated in curves C and D, the particle distribution according to curve C having a slightly higher content of small particles than the particulate material corresponding to curve B and D.
(69) The particulate material of the various samples B, C and D may be further characterized by the parameters contained in Table 1.
(70) TABLE-US-00001 TABLE 1 Fraction with Particle Size < 25 m Sample [vol %] d.sub.10 Value d.sub.50 Value d.sub.90 Value Curve B 6.2 44.6 m 104.9 m 239.0 m Curve C 1.38 39.6 m 91.3 m 204.6 m Curve D 2.03 45.4 m 108.6 m 244.2 m
(71)
(72) The arrangement 200 includes a cylindrical housing 202 accommodating a stack 204 of cartridges 14 which are aligned with their central hub portions 64 in order to form a continuous channel 206.
(73) The cartridges 14 have been filled with PVPP particulate material as described in connection with
(74) The housing 202 has an upper removable cover 208 comprising a fluid inlet 210 through which the beverage to be stabilized is introduced into the housing 202.
(75) The beverage then fills all of the volume of the housing 202 and enters into the various cartridges 14 in parallel via their respective upper mesh surface 76 (cf.
(76) In order to provide a continuous flow of beer, a centrifugal pump 218 is used which is pressure and flow controlled via pressure and flow rate sensors 220 and 222, respectively. The temperature of the beer is typically in the range of 0 C. to about 10 C. and is regarded as the first temperature.
(77) The pressure of the stabilized beer when exiting the housing via outlet 212 is monitored via pressure sensor 224.
(78) The rest of the equipment of arrangement 200 remains inoperative during the stabilization treatment of the beer.
(79) After approximately 6 to 10 hours, the capacity of the particulate material contained in the cartridges 14 is exhausted and a regeneration of the particulate material is needed.
(80) The regeneration step is typically performed by flushing the cartridges 14 and the deposited layers contained therein with a caustic and an acidic fluid, e.g., aqueous NaOH and aqueous HNO.sub.3, respectively.
(81) In a first regeneration step, the stack of cartridges 14 and housing 202 is rinsed with water in order to remove residual beer.
(82) Afterwards, the cartridges 14 are heated by circulating the water contained in the arrangement 200 up to a second temperature of 85 C. The second temperature of 85 C. is determined in order to provide a sterilization of the cartridges and their deposited layers as well as housing 202 and the pipes of arrangement 200 before the stack of cartridges 14 is again charged with beer to be stabilized.
(83) The process for regenerating the particulate PVPP material contained in the cartridges 14 may be modified to achieve reconditioning of the deposited layers within the cartridges 14 according to the present invention such that eventually formed cracks or other damages or inhomogeneities in the particle distribution within the deposited layers will be cured so that again the deposited layers of PVPP particulate material are in a state corresponding essentially to an original filling (cf.
(84) In order to provide for a smooth heating of the particulate material in the cartridges 14, the temperature of the recirculated water is controlled by heat exchanger 226 such that it is at most 20 to 30 C. higher than the temperature at the outlet of housing 202 (temperature sensor 228).
(85) The flow rate of the heated water is controlled such that the temperature increase per minute is about 5 to 7 C.
(86) During heating of the circulating water and heating of the stack of cartridges 14 in housing 202 or after the second temperature of 85 C. has been achieved, caustic soda is fed from supply 230 by feed pump 232 into the recirculated water until a 1% by weight concentration is obtained.
(87) Circulating of the water containing 1% by weight of caustic soda is continued for 10 min during which time the caustic soda medium is drained from the arrangement 200 via branch pipe 240 and valve 242 in order to remove the desorbed polyphenol contained in the caustic soda solution. The drained portion of the reconditioning/regenerating fluid is replaced by fresh water from water supply 234 via valve 236. The hot water containing caustic soda in the amount of about 1% by weight is then recirculated for another 20 min in a closed loop (valves 236 and 242 closed).
(88) Thereafter, the removal of previously adsorbed polyphenols from the particulate PVPP material has been completed and the alkali fluid is withdrawn from the arrangement 200 through pipe 240 and valve 242 and replaced by fresh hot water from water supply 234 preferably heated to the same temperature as the caustic material previously recirculated when passing through heat exchanger 226. The arrangement 200 is purged with fresh water until the electrical conductivity of the water exciting the housing 202 is below 0.5 mS.
(89) Thereafter, carefully controlled cooling of the stack of cartridges 14 and the deposited layers therein is initiated. According to the present invention, it is most important, that the cooling step is performed under close control of temperature such that no temperature shock is exerted on the deposited layers within the cartridges 14 in order to retain their integrity.
(90) Here, the inlet temperature is controlled to about 10 to 15 C. less than the temperature of the recirculating fluid at the outlet 212 of housing 202. The heat exchanger 226 is now operating as a cooling device.
(91) During the same time, acid, e.g., HNO.sub.3, may be dosed into the circuit from supply 238 and feed pump 232 until the amount of acid within the recirculating water reaches about 0.5% by weight.
(92) During recirculating the acidic water, a third temperature is maintained at a level of 20 to 25 C.
(93) This procedure is followed by cold water (from water supply 234) rinsing for another 3 min and the effect of rinsing is controlled by measuring the electric conductivity of the water until it is below the upper limit of 0.5 mS.
(94) The temperature of the fluid used for rinsing may be maintained at about 20 C.
(95) After that step has been completed, the stack of cartridges 14 and their deposited layers are fit for a new cycle of stabilization of a beverage, e.g., beer.
(96) The above procedure has the advantage that the cartridges 14 and the deposited layers of PVPP material may remain within the housing 202 and may be immediately re-used for stabilizing beer.
(97) Likewise, the time typically needed for regenerating the particulate matter by desorbing the adsorbed polyphenol material in a caustic liquid environment may be used at the same time to heat the deposited layers so that both the treatment of the particulate material in order to desorb the polyphenols and heating of the particles in the deposited layer for reconditioning the same may be effected at the same time. Likewise, rinsing of the cartridges and the deposited layers therein and cooling of the same may be effected at the same time so that the reconditioning according to the present invention may be incorporated in the typical regeneration process performed in a regular stabilization process.