EP2403635A2 - Dispositifs et procédés de production de billes de glace à partir d'un mélange aqueux - Google Patents

Dispositifs et procédés de production de billes de glace à partir d'un mélange aqueux

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Publication number
EP2403635A2
EP2403635A2 EP10706939A EP10706939A EP2403635A2 EP 2403635 A2 EP2403635 A2 EP 2403635A2 EP 10706939 A EP10706939 A EP 10706939A EP 10706939 A EP10706939 A EP 10706939A EP 2403635 A2 EP2403635 A2 EP 2403635A2
Authority
EP
European Patent Office
Prior art keywords
liquid
hydrophobic liquid
ice
vessel
flow
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP10706939A
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German (de)
English (en)
Inventor
Wolfgang Folger
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Individual
Original Assignee
Individual
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Publication of EP2403635A2 publication Critical patent/EP2403635A2/fr
Withdrawn legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/02—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops

Definitions

  • the present invention relates to devices and to an executable by means of these devices method for producing ice beads from an aqueous mixture, in particular of active ingredient-containing ice beads, and on the ice beads themselves.
  • the present invention relates on the one hand substances that are to be applied as active ingredients such as insecticides or herbicides in larger areas of the environment and are applied to the ideal distribution from the air to the ground or water surfaces.
  • active ingredients can be distributed in a suitable manner and can be applied from the air specifically at the destination, it is known to deploy the active ingredient on a carrier medium, which is distributed accordingly.
  • the production of ice beads from the carrier medium with the active ingredient has been found to achieve this purpose as suitable.
  • liquid nitrogen also leads to very rapid freezing of the ice and therefore conglomerate the ice spheres or the occurrence of imperfect, for example, hollow or otherwise not ideally shaped particles, as well as an unsatisfactory particle size distribution which complicates the homogeneous spreading of the ice particles accordingly.
  • An improvement of the ice quality using the known methods with the nitrogen freezing agent could be achieved by a drastic reduction of the discharge rate with the same nitrogen supply of the plant, which is unfavorable, especially taking into account the associated cost increase and because of the unsatisfactory production rate.
  • An embodiment of the device according to the invention for producing the ice pearls from an aqueous mixture comprises a device with a cooling device which is suitable for cooling down a hydrophobic liquid to a temperature which ensures the freezing of the material to be introduced in the desired time and to a desired degree allows, as well as a receptacle for the cooled hydrophobic liquid, as well as a receptacle on the receptacle arranged pipetting device.
  • This pipetting device essentially consists of a vessel for the aqueous mixture which is to be frozen into pearls; it has in a sidewall or in the bottom outlet tube, via which the aqueous mixture is dropped into the hydrophobic liquid: The dripping is achieved by the pipetting device so far into the receptacle protruding - such as by means of a holder - that the ends of the outlet in the region of 10 cm above a surface of the hydrophobic liquid or immerse up to 0.5 cm deep in this.
  • the device is such or has an additional device that either the hydrophobic liquid flows while entraining dripping droplets, or that the pipetting device is moved relative to the container or vice versa, the container with the hydrophobic liquid under the pipetting device so that the droplets tear off the end of the outlet tube and fall into the still cold fluid.
  • an ideal droplet shape is obtained when the dripping liquid, which is thus driven at least because of the hydrostatic pressure from the outlet tube, falls into the cryogenic hydrophobic liquid, whereby ideally shaped ice pearls are obtained evenly frozen when they have a predetermined flow or sinking distance have traveled in the hydrophobic liquid.
  • the hydrophobic liquid for freezing aqueous mixtures has a temperature of less than 0 0 C, advantageously lower temperatures of the hydrophobic medium can be selected to achieve an improved production rate.
  • the pipetting device may be made of a cast, such as metal or plastic, it is also possible to provide any suitable vessels with a plurality of passages and to fit cannulas.
  • the product which is ideally suited for the application of active substances from the air, can be taken up in suitably insulated containers in a large mass of solid frozen, dimensionally stable ice balls and Devices are distributed from the air.
  • hydrophobic liquid in terms of their viscosity in the corresponding temperature range may be, for example, a petroleum fraction such as kerosene and petroleum, or a vegetable oil, the harmless from a toxicological point of view also suitable for application in agricultural or fish farming areas such as linseed oil, linseed oil or rapeseed oil. All oils may be used in admixture, with rapeseed oil only being suitably used in admixture with other oils, such as those mentioned above.
  • the liquid can be at a sufficiently low temperature to continuously freeze through an aqueous mixture of active ingredients without taking a viscosity due to low temperatures, which prevents the formation of the spherical shape of the introduced liquid to be frozen, or which causes the freezing process even before the formation of the spherical shape progresses so far that shapeless ice is formed.
  • a liquid dissolved in water, emulsified or present in the form of water in the form of suspended particles, which acts as an insecticide, herbicide, fungicide, fertilizer, soil and / or water-improving agent, is suitable as fluid to be frozen into ice beads.
  • Known insecticides which are suitable for this purpose are BTI or BS endotoxin.
  • the cooling device will be connected to the receptacle for the active ingredient mixture by means of a pump.
  • the vessel in which the hydrophobic liquid is contained has a receiving portion via which it is filled and, correspondingly, an outlet portion in which a removal device is provided, which advantageously serves to discharge the hydrophobic liquid and ice beads. It is possible to easily provide an outlet opening, so that the product flows off with the hydrophobic liquid, however, it is also possible to suck the resulting ice beads with a corresponding suction pump or skim it with a creator.
  • the hydrophobic liquid is intended to flow away from the remaining outlet tubes or cannula tips, or a relative velocity is provided between the hydrophobic liquid and the cannula tips by either the cannula tips or the container with the stent hydrophobic liquid to be moved.
  • the relative movement ensures that the droplets of the liquid to be frozen enter separated into the hydrophobic liquid and a combination of droplets is excluded to larger entities, and freeze the drops into individual ice beads.
  • the diameter of the cannula determines.
  • Pressure and the size and shape of the tear-off surface at the cannula tips over the diameter of the drops.
  • the globular form itself assumes the drop as a function of the surface tension of natural law, if it does not z. B. by too high viscosity of the hydrophobic liquid or by excessive shear forces in the vicinity of the container walls in a moving hydrophobic fluid is prevented
  • the one reactor consists essentially of a vertically orientated th flow tube, which may be advantageously isolated or which is cooled by means of a cooling device.
  • a second reactor form provides the design as a flow channel.
  • the flow channel along its main extension direction may have a slope.
  • the orientation of the vertical flow reactor or the inclined flow channel already causes the hydrophobic liquid to flow; the corresponding means for accelerating the hydrophobic liquid can be seen in the case of the vertical flow reactor in the flow rate, in the case of the flow channel decides at a given flow rate, the slope of the channel on the thickness of the flow cross-section of the hydrophobic liquid in the channel, and thus on the flow rate.
  • An advantageous form of supplying the hydrophobic liquid in a reactor with a vertically oriented flow tube can be realized via a distribution device, in which the feed device for the cooled hydrophobic liquid flows.
  • This distributor device extends horizontally in the receiving section in the region of the surface of the hydrophobic liquid formed in the flow tube.
  • a hollow profile can be selected which is not closed along a length of one side - the "upper side” and thus has a slit-shaped outlet opening for the hydrophobic liquid If the sidewalls of the hollow profile are advantageously curved rounded towards the exit slit, the liquid may flow slowly past the rounded shoulder it passes into the vertical flow section in the flow tube.
  • the slot-shaped outlet opening extends below the pipetting device, and it is advantageous that it has two parallel rows of outlet tubes, each extending down to one of the sections adjacent to the outlet slot. Accordingly, those from the drops of each In this case, the beads of ice formed on the outlet tube rows are entrained on both sides of the hollow profile with the flow of the hydrophobic liquid into the flow section and from there into the outlet section.
  • the pipetting device in the vertically arranged flow reactor, it is possible to provide the pipetting device directly in an upper portion serving as a receiving portion for the hydrophobic fluid to be supplied.
  • a shoulder may hereby be provided at the upper end of the tube which leads to a transition to a widened tube section as a receiving section.
  • reactors with polygonal cross sections in this widened pipe section, the pipetting device can now be introduced, wherein the pipetting device is adapted to the contour of the receiving portion of the flow channel with respect to its outer contour.
  • the tube cross-section widened at its receiving portion leaps and bounds, according to a pipetting device can also be used with a cylindrical shape.
  • the cannulas can be inserted into the wall of the cylindrical vessel so that they are substantially transverse to the longitudinal axis of the flow reactor. It is possible to provide several rows of needles circumferentially and one above the other, corresponding to gap, on the wall of Pipettiervoriquessgefäßes.
  • the wall of the cylindrical vessel which contains the aqueous active substance mixture, is spaced apart from the outer wall of the flow reactor so far that a ring can be arranged as a separating ring to the cylindrical water-active ingredient vessel.
  • the ring is supported on the shoulder of the flow reactor, leaving an annular gap.
  • the frozen hydrophobic fluid can now be filled between the wall of the separating ring and the outer wall in the resulting loading space of the flow reactor, and it flows under the annular gap along the shoulder until it at the tapered portion of the flow reactor in the direction of the removal device flows.
  • the pipetting device used in the receiving section of the flow reactor is supported with its bottom, if necessary by spacers, at least so far above the shoulder that the hydrophobic fluid flowing under the annular gap can underflow the vessel with the water-active substance mixture unhindered.
  • the substantially horizontally oriented cannula tips thus allow the emerging from the cannula tips water-active ingredient mixture, first a distance of about 3 to 7 cm to fall into the air gap before they hit the oil.
  • the air-mat is provided between the outer wall of the cylindrical vessel and the annular separating liner.
  • the droplets impinging on the hydrophobic fluid stream which may be an oil stream, cause the flow reactor, which can advantageously taper in a funnel shape at its lower end, to pass through an outlet nozzle.
  • the stream containing the ice pearls is sent for further treatment.
  • a separating device for separating the ice bead product from the hydrophobic liquid is connected directly to the removal device.
  • Trained as a flow channel embodiment of the device according to the invention may have a straight shape or a ring shape.
  • the straight shape can be designed as a simple, open-topped channel, but it can also be designed as a belt conveyor.
  • the flow channel may also be insulated for economic reasons or its wall may be coupled to a cooling device.
  • a cooling device By a corresponding inclination of the flow channel, a flow of the hydrophobic liquid and thus the desired relative velocity between hydrophobic liquid and cannula tips are already achieved here.
  • the flow channel is cooled at one end with ice-cooled acted upon rophoben liquids on which the pipetting device is arranged.
  • the flow channel has an outlet opening, which may be correspondingly connected to a separation device, such as a centrifuge or a sieve. Due to this embodiment, the separated in the separation device hydrophobic medium can be recovered and recycled after appropriate cooling back into the process.
  • a plate rotatable about its longitudinal axis can be arranged as a stowage device in the fluid path between the pipetting device and the outlet device.
  • This rotatable plate causes the incoming freeze-water mixed drug drops to submerge beneath the surface of the hydrophobic liquid. Due to the hydrodynamic effects, the drops do not touch the plate and are not damaged, but the passage down to a greater depth of the hydrophobic liquid promotes further freezing.
  • the executable with the embodiments of the device according to the invention method provides in principle that a hydrophobic liquid by means of a corresponding cooling device to a suitable depending on the properties of the selected hydrophobic liquid and the liquid to be frozen and the desired process time temperature, in each case below 0 0 C, is cooled before it is filled into the receiving vessel, which may be a corresponding flow reactor or a flow channel.
  • the energy required for cooling the hydrophobic liquid is low, compared to the energy expenditure for the provision of nitrogen for processes for the production of similar products.
  • the aqueous active substance is preferably added to the pipetting vessel, wherein, since the cannulas are not blocked, the aqueous active ingredient mixture can be transferred dropwise via the cannulas into the hydrophobic liquid by the sole action of gravity.
  • the dripping speed can be determined via the outlet opening and / or the hydrostatic pressure.
  • the drops deposit a fall path in the air. As the drops touch the fluid, they begin to freeze and begin to float or float on the surface of the hydrophobic medium because, depending on the temperature thereof, the specific gravity can be very close to that of the freezing material.
  • the drops in the horizontally oriented reactors remain on the cold hydrophobic medium and initially freeze only on their underside.
  • the device which provides the rotatably mounted plate they are forced under the surface, whereas in the case of a vertically oriented flow tube, a suction which results from the continuous flow through the reactor draws the droplets downwards that the further freezing takes place.
  • a suction which results from the continuous flow through the reactor draws the droplets downwards that the further freezing takes place.
  • the formation of a bead-shaped ice product from the aqueous active substance mixture is completed.
  • spherically frozen drops leave the reactor together with the hydrophobic medium, respectively with the oil, through the outlet opening.
  • the mixture of hydrophobic liquid and the ice beads can be removed either by a discharge from the channel or the flow reactor takes place, or by what concerns only the flow channel, which can also be designed annular, a skimming or suction with appropriate Devices takes place.
  • the separated ice beads can be fed to their use, while the separated supernatant hydrophobic liquid is cooled down again to process temperature and fed to the receiving section of the receptacle.
  • the resulting ice bead products are spherical, homogeneously frozen through and can be broken down depending on the inner diameter of the cannula. adjust their size.
  • the ice bead manufacturing apparatus of the present invention can provide a flow of the hydrophobic liquid by appropriately providing a tilt of the receptacles, but it is also possible for the hydrophobic liquid container to be operably coupled to drive means such that the receptacle itself is in Movement is moved, is moved past the pipetting device, whereby the drops emerging from the cannulae drop individually into the hydrophobic liquid and allowed to freeze. Shearing forces in the region of the container walls can advantageously be avoided by the quiescent liquid, and drops are applied to the entire width of the container.
  • FIG. 1a is a frontal longitudinal section of a vertical flow reactor
  • Fig. 1b is a perspective longitudinal section of the reactor of Fig. 1a
  • Fig. 1c schematically shows a detail of the pipetting, which is arranged in the receiving region of the flow reactor of Fig. 1a
  • Fig. 2a is a perspective side view 2b shows the flow behavior of the fluids of the device from FIG. 2a
  • FIG. 3 shows a perspective plan view of a device designed as a ring flow channel for generating the ice pearls according to the invention
  • FIG. 5 a shows a perspective front view of a further embodiment of a device designed as a vertical flow reactor
  • FIG. 5 b shows a longitudinal sectional view of the flow reactor from FIG. 5 a
  • FIG. 5 c shows a frontal longitudinal section of the flow reactor from FIG. 5 a
  • FIG. 5 d shows a frontal longitudinal section from FIG 5a of the receiving section with the Distribution device
  • FIG. 5e is a perspective longitudinal section of the distributor device of Fig. 5a
  • FIG. 5f is a perspective top view of the distributor device of Fig. 5a.
  • reactor is to be understood in the following as a vessel in which a reaction such as the change of a state of aggregation of a liquid occurs.
  • Appropriate reactors comprise a ducted flow reactor, which is described in US Pat inclined channel or "chute", as a conveyor belt or as a rotating ring reactor, so to speak as a “carousel.”
  • Another suitable reactor is a vertical flow tube.
  • the aqueous mixture of active substances is understood to mean either an active-ingredient-containing aqueous liquid which contains a substance which acts as an insecticide, herbicide, fungicide, fertilizer, soil conditioner or water-improving agent dissolved in water.
  • Active substances of particular interest in the present case are insecticides contained in Bacillus thuringiensis Israelensis (BTI) or Bacillus sphaericus (BS endotoxin); or it's a food meant like a fruit juice.
  • the liquid to be frozen is water or water with substances dissolved or emulsified therein or floating or floating in water, which do not substantially alter the freezing properties of the water, so that the hydrophobic liquid is used as a freezing medium for the aqueous active ingredient mixture, a temperature may have as little as possible below 0 0 C to provide the desired ice-cream product.
  • the hydrophobic liquid used in the method according to the invention must always have a viscosity which allows the liquid to be frozen to assume the spherical shape. Furthermore, it is advantageous if the liquid is easy and cheap to procure.
  • the hydrophobic liquid may be petroleum fractions, such as kerosene and petroleum, or motor oil or hydraulic oil, which have low viscosity even at very low temperatures.
  • oils which can be applied in nature due to the fact that they are not toxic, or even consumable. It should be noted that oils that are already viscous or even cured at room temperature or below, such as palm oil, are not suitable, whereas camphor oil and linseed oil have been found to be particularly suitable vegetable oils. Rapeseed oil is also suitable, but only to a limited extent, since due to its viscosity it can only be used in a suitable manner in admixture with the abovementioned oils.
  • the devices according to the invention are suitable for producing active-substance ice-cream beads.
  • an active ingredient such as BTI, preferably dissolved in water, mixed or emulsified, so that the active ingredient together with the carrier liquid is frozen into beads or spherical ice particles.
  • Such ice beads which are homogenously frozen and have a desired diameter, with a batch of manufactured ice pearls being generally homogeneous with respect to ice bead diameters, are capable of being applied to the earth's surface by aircraft such as helicopters having suitable dispensing devices.
  • a food product group may contain as an aqueous mixture a fruit juice, or a fruit juice mixture, a fruit syrup or nectar mixture or a suitable for consumption as ice basic component, which then by the preparation by means of the method according to the invention and the incomplete separation of the hydrophobic liquid a film has the same; this can be exploited by using a valuable food oil in the manufacturing process, and the remainder of the product is used as a food supplement, such as omega-3 fatty acids.
  • Such ice beads can be prepared with desired sizes as homogeneously shaped and frozen particles by means of a device comprising a pipetting device, wherein in the present pipetting device is not a burette with a single pipette to understand, but a vessel that can be made in one piece and a plurality of tapered outlet tubes in a vessel wall, or made of a vessel, on the wall of which a plurality of passage openings are provided into which the cannulas have been tightly fitted.
  • a device comprising a pipetting device, wherein in the present pipetting device is not a burette with a single pipette to understand, but a vessel that can be made in one piece and a plurality of tapered outlet tubes in a vessel wall, or made of a vessel, on the wall of which a plurality of passage openings are provided into which the cannulas have been tightly fitted.
  • a liquid such as in the present case the aqueous active substance mixture, from which the ice pearls are to be produced, filled into the vessel, so get drops on a variety of cannula tips of the cannulas from the vessel.
  • the wall may be both a side wall and the bottom of the vessel; this depends on how the pipetting device is arranged with respect to another vessel.
  • This additional vessel is a receptacle for a hydrophobic liquid.
  • the pipetting device is so above the receptacle or arranged on the receptacle for the hydrophobic liquid so that the projecting from the pipette needle tips have in the direction of the receptacle for the hydrophobic liquid that they either immerse up to 0.5 cm in the liquid or up to 10 cm above the liquid surface are such that the drops traverse a distance of about 10 cm, but advantageously not more than 5 cm, in the air before they strike the surface of the hydrophobic liquid.
  • the cooling device is connected to the receptacle for the hydrophobic liquid, taking into account a possible short path via a feeding device.
  • the entire process is a continuous process in all plant variants, which is always operated using a pump that usually runs permanently during process control. There is no direct connection between the pump and the reactor, but rather the oil! during the separation of the ice continuously in an open receptacle from which also runs the oil from the centrifuge. From this container, the pump sucks the now heated by the process oil and pumps it through the heat exchanger of the chiller back into the reactor.
  • the point at which the hydrophobic liquid is supplied in the receptacle is hereinafter also referred to as receiving section.
  • the receiving portion to which the hydrophobic liquid is supplied there is also an outlet portion;
  • a simple extraction device may be formed from an opening to which a nozzle or hose piece for transferring the product together with the hydrophobic liquid extends in downstream further processing devices accordingly;
  • a suction pump is provided, with which the guided by hydrophobic liquid Eisperlen apparatus is sucked, even a simple device after Machart a ladle is conceivable.
  • Between the receiving section and the Leaves section is a flow section.
  • the aqueous drug mixture from the pipetting device leaves the cannula tips in droplet form via the cannulas and, either directly or after traversing a fall path in the air, penetrates into the hydrophobic, ice-cold liquid and thus travels a fluid path, the drops begin to flow Freezing out into the hydrophobic liquid and the process of freezing is completed when traversing a flow path in the hydrophobic liquid.
  • the use of a vertical flow reactor is particularly advantageous because it can be cleverly connected to the pipetting device.
  • the vertically arranged flow reactor which may have a circular or polygonal cross-section, at its upper end have a larger opening cross-section than the pipe cross-section is in a central region.
  • the transition between the two divergent pipe sections is realized by a shoulder that runs horizontally or may have an inclination of up to 15 °.
  • the pipetting device can be arranged so that the pointing out of the pipette needle tips, which may be arranged horizontally in several rows circumferentially on the vessel wall of the pipetting vessel by at least 5 mm, more preferably up to 5 cm from the wall of the pipette Flow reactor are spaced.
  • the vessel may be supported on the shoulder of the flow reactor.
  • a separation device such as a separating ring, which may be selectively supported on the shoulder, equidistant from the flow reactor wall and circumferentially around the pipetting vessel wherein an air gap is provided between the cannula tips and the cannula tips facing side of the separation device, whereas between the separation device and the flow reactor wall a space for filling the cold fluid remains.
  • the drops impinging upon the hydrophobic fluid stream which may be an oil stream, initially tend to fall but becomes specifically lighter with the onset of freezing. Regardless of whether they would float or rise depending on the temperature and thus the density of the hydrophobic liquid in the medium, they are pulled in the vertical reactor with the oil flow in the depth, while they freeze further. They leave the flow reactor, which can taper at its lower end advantageous funnel-shaped, through an outlet.
  • a hose or a pipe can be connected with which one can supply the power containing the ice beads of the further treatment. With the length of the tube or tube, one can extend the residence time of the ice beads in the hydrophobic medium, for example, to achieve a better freezing.
  • these devices can be realized with cylindrical elements, so that the partition wall is designed as a ring around the pipetting vessel around.
  • the pipette tips of the likewise cylindrical pipetting vessel point radially in the direction of the separating ring.
  • the temperature of the hydrophobic liquid is suitably chosen: If the medium is too cold, the freezing process begins immediately upon impact of the drops on the medium, and the deformation is preserved.
  • the temperature range of -12 0 C to -14 0 C has proven to be the ideal temperature.
  • an overflow line is attached to the vertical outer wall of the reactor in the area of the task of the hydrophobic liquid and the drops, which leads to the suction vessel, from which the pump takes the oil and feeds the heat exchanger. This relieves the need for a very precise balance between the task quantity and the discharge volume.
  • the cooled to the desired temperature oil is introduced into the gap between the flow reactor and partition, so that it passes under the gap of the partition, respectively the annular gap and over the shoulder in the direction the tapered tube cross section flows.
  • an air space remains between the openings of the cannula tips and the surface of the hydrophobic liquid, so that the drops in the gap, which forms between the Pipettiergefäßwand and the partition can fall down and impinge on the hydrophobic liquid surface, wherein the immediately freezing water-drug mixture drops be entrained by the flowing hydrophobic liquid and guided along the vertical flow path of the flow reactor.
  • a suitable embodiment of the flow reactor provides that this is funnel-shaped tapered at its outlet and the funnel opens into an outlet.
  • This funnel-shaped rejuvenation is See flow reactors as possible as in flow reactors, which have a polygonal cross-section.
  • the outlet cross section of the outlet opening can be selected to be correspondingly small, and it is possible to guide the nozzle adjoining the outlet opening horizontally or otherwise bent or bent.
  • a comparable result with respect to the achievement of the desired ice bead products can be achieved with a receptacle which is designed as a flow channel, wherein the flow channel can have an inclination along its main extension direction.
  • the channel can be designed as a simple half pipe, even simple box-shaped versions are possible.
  • a pump is always arranged on the device and the oil is already running off by the continuous feed, even if the chute is mounted horizontally.
  • the relative speed of oil to cannulas has proved to be ideal at 5 cm per second, a tilt is then not absolutely necessary.
  • the band represents by its co-rotating side walls (corrugated), the reactor vessel.
  • Band speed and feed amount of oil are balanced so that the film thickness or thickness remains the same, and the oil after the task at the head in relation to the band not moved.
  • the pipetting device can be designed as a box, wherein the cannulas are arranged in a bottom side of the box which is at least partially open and connected to corresponding storage containers, such that the pipette tips are perpendicular to the liquid surface and either immerse in this or about 3 cm to 10 cm, preferably 5 cm above the liquid surface are arranged.
  • the cannulas may also be designed so that the cannula tips are slightly bent so that the line that forms between the kink of the cannula and the cannula tip opening joins the fluid surface Angle from 0 to 30 °, advantageously formed by about 15 °.
  • the out of the pipette vessel via the cannulas and emerging from the cannula tips drop now a few inches through the air and then encounter the flow of hydrophobic liquid. There they are entrained until they are removed at the end of the flow channel via a sampling device, which is essentially connected to the discharge of a corresponding proportion of hydrophobic liquid.
  • the flow channel can have both a straight shape and a ring shape, wherein the ring shape is not suitable to be inclined with respect to the horizontal and insofar requires the arrangement of a pumping device for moving the hydrophobic liquid or a device for moving the flow channel or the pipetting device, and the removal device can be designed differently depending on the shape of the flow channel: it may prove sufficient in the removal device, in particular in the straight, inclined shape of the flow channel, only provide a discharge nozzle at the end of the channel through which the hydrophobic liquid is discharged together with the entrained ice bead product. However, it may also be suitable, especially in the annular embodiment, to scoop off the ice beads from the hydrophobic liquid or to suck them off by means of a corresponding suction device.
  • the flow rate and thickness of the hydrophobic medium in the channel can be controlled by the feed rate of the medium per unit time, by damming, by tilting of the channel (positive and negative), and by the combination of these methods.
  • the necessary residence time of the drops in the cold transfer medium must be made possible by the corresponding length of the channel.
  • deformation can be prevented by dipping the outlet ends of the cannulas a few millimeters deep into the hydrophobic medium, and also by spacing the marginal cannulas at least 3 cm from the flow channel wall; furthermore, it should choose a thickness of the transmission medium in the channel, which ensures that the droplets do not sink into the depth range or even touch the channel bottom before they have a stabilizing ice casing, where the shearing forces lead to deformations.
  • the ice chute is therefore a device variant that is particularly suitable for the use of vegetable oils as a hydrophobic medium;
  • the advantage of the slide is its simple structure and simple process control.
  • An advantage of the vertical reactor is that there are no interfering shear forces and that there is no large exposed surface of the hydrophobic medium which, if not produced in the cold store, should be well insulated to account for the energetic aspects as well in that condensation of atmospheric moisture and thus an accumulation of water can take place on the surface of the hydrophobic medium.
  • reactors may be coupled downstream of the sampling device with a separator to separate the ice bead product from the hydrophobic liquid.
  • a separator may be a centrifuge or a sieve.
  • the separated liquid can be cooled again by being transferred directly from the separation vessel of the cooling device, from there it can be returned to the process by being fed back by means of a corresponding hose or line connection to the receiving portion of the corresponding receptacle becomes.
  • a stowage device is provided in the flow of hydrophobic liquid, wherein the stowage device in the range of about two third to half of the flow through the! Provided flow path of the hydrophobic liquid is arranged.
  • the stowage device may be a simple plate whose shape is adapted to the cross-sectional contour of the channel. The plate is fixed by means of an axle on the side walls of the channel and rotates in the flow direction. This plate is used to acts to force the flowing stream of hydrophobic liquid to submerge the droplets to be frozen entering the plate. The drops do not touch them directly due to a damming wave generated by the hydrodynamic effects on the lower edge of the plate, but are forced downwards by the damming wave, so that the freezing in spherical form is not hindered.
  • the drops are thus forced into a deeper layer of the hydrophobic liquid and can be appropriately freeze without being deformed when covering the remaining flow path.
  • the whole vessel moves with the hydrophobic medium resting therein under the outside of the vessel, for. B. attached to a tripod pipetting device, the equally arranged feed device for the hydrophobic medium and the product removal device.
  • This mode of operation applies to the carousel, which rotates about a central axis, as well as to the conveyor belt which, with its corrugated edge, constitutes a moving channel in which the hydrophobic medium rests at its outlet end footing until it exits the belt.
  • the advantage of these two variants is that no shear forces occur here because the hydrophobic medium does not move in the channel.
  • the ice beads are advantageously separated by dripping as much as possible from the oil before they are fed to the centrifuge.
  • the oil / ice mixture exiting the reactor effluent may be directed into an inclined tube which may be pierced through many slots and slowly rotate about its longitudinal axis. A large part of the oil flows through the slots and runs into the collecting container positioned below the pipe, from which the pump pumps the oil back to the reactor via the heat exchanger. Thus, the cycle is closed.
  • the ice beads enter the centrifuge after passing through the drip tube.
  • the oil thrown off here also flows into the collection container. After centrifuging, a small amount of oil sticks to the ice. On a kilo of ice pearls remain about 10 grams of oil. The so extracted from the plant amount of oil is constantly supplemented from a reservoir.
  • the product of the present invention exhibits a homogeneous and spherical structure, all of the spheres emanating from needles of the same internal diameter have substantially the same diameter, which is the product of the application by means of air transport over land or water makes it particularly suitable because it allows the scattering effect can be optimized.
  • the choice of the outlet opening of the cannula tips determines the size of the ball diameter;
  • Known cannulas are conventionally classified over their outer diameter, and in particular cannulas with outer diameters of 1 mm to 8 mm are suitable for the present method, wherein an outer diameter of 1.2 mm has proven to be ideal.
  • FIGS. 1a, 1b, 2a, 3, 4 and 5a show embodiments of the devices according to the invention.
  • 1a shows the longitudinal section of a vertically arranged flow reactor 2, which is "tapered in its middle section 2 and provides a flow section 2".
  • the flow reactor 2 extends above its flow section 2 "via a peripheral shoulder 13 into a receiving section 2 ', where the hydrophobic, ice-cooled liquid is carried out.”
  • the receiving section 2' of the cylindrically shaped flow reactor 2 is separated from the centrally arranged pipetting device 3 by a
  • the separating ring 14 is seated at a point on the shoulder 13 and is spaced from the shoulder 13 by a non-continuous annular gap 14 'This arrangement is also shown in Fig.
  • the pipetting device 3 comprising the vessel 4, in whose wall 4 'two juxtaposed, circumferential rows are arranged around needles 5, is also disposed above the shoulder 13, and, which is not shown figuratively, set on this spaced.
  • the pipetting device can also be held in the position shown by means of a holder and does not then have to be supported by the shoulder 13.
  • the flow reactor 2 tapers at its outlet end 2 "'in the funnel-shaped collector 6, which opens into an outlet connection 7. By means of a flange 21, the flow reactor can be positioned and held.
  • FIG. 1c which shows the detail A marked by a dashed line in FIG. 1a
  • the vessel 4 of the pipetting device 3 is positioned on the region 2 "of the flow reactor 2 so that an air gap 15 'is located between a bottom of the flow reactor 2 Vessel 4 and the surface 20 'of a flowing hydrophobic liquid 20.
  • the ice-cooled hydrophobic liquid 20 is, as shown by arrow b, in an annular gap 15 between the separating ring 14 and the outer reactor wall of the receiving portion 2 "filled.
  • the liquid flows into the tapered section 2 "of the flow reactor via the shoulder 13.
  • the liquid 11 filled in the pipetting device 3 exits via the cannula tips of the cannulas 5 and drops dropwise into the air gap 15 'between the outer vessel wall and the separating ring 14 and, after about 5 cm drop height, impinges on the surface 20' of the hydrophobic liquid.
  • a vertical flow section the embodiment shown in Fig. 5a of the device 1 for the production of ice beads on.
  • This device 1 is similar to an upright cuboid, over the open top of the pipetting device 3 is arranged.
  • the vessel 4, which contains the aqueous active ingredient mixture 11 is also formed with a rectangular cross-section, the Longitudinal extent corresponds substantially to the longitudinal extent of the rectangular surface of the flow reactor 2, while the width of the vessel 4 in the illustrated embodiment is less than the width of the flow reactor.
  • Fig. 5b the arrangement of the distribution device 30 is illustrated in the flow reactor 2.
  • the distributor device 30 is formed by a hollow profile, on whose side pointing upwards, in the direction of the pipetting device 3, a gap 31 extends, through which the hydrophobic liquid 20 passes into the flow reactor 2 (arrow c).
  • the fluid path b of the hydrophobic liquid thus extends from the feed line 19 through the hollow profile 30 and its exit slit 31, from where the fluid path divides on both sides, vertically down through the flow reactor 2 to the outlet port 7.
  • the two rows of cannulas 5 of the pipetting device 3 are arranged offset parallel to the exit slit 31, so that a path a, the respective half of the drops of drug solution 11 traced, starting from the source gap 31 to the right and left of the distributor device 30 passes according to the fluid paths b passes.
  • the "fluid mountain” 20 "formed by the source gap 31 can be clearly seen in FIG. 5c.
  • a floating arrangement of the Verteiiervoriques 30 in the receiving portion 2 'of the flow reactor 2 results in the illustrated gradient of the formed on the hollow profile on both sides of the gap 31 fluid film:
  • the surface 20' of the hydrophobic liquid proceeds from the “Fluidberg” 20 " on both sides over the rounded edges of the hollow profile 30 up to the surface level, which is held in the reactor 20.
  • the floating arrangement of the distributor device 30 is realized by a respective buoyant body 32 at the longitudinal ends of the hollow profile 30, which can be seen more clearly in Fig. 5e and 5f.
  • the dripped-in active substance beads freeze, so that the removal in the outlet section 2 '" can take place through the connection 7.
  • the receiving portion of the reactor 2 with the supply of the cooled, hydrophobic liquid 20 and the task of the drug solution 11-containing droplets is shown in detail in Fig. 5d. Drops of the drug solution 11 fall from the vessel 4 through the cannulas 5 on both sides of the outlet gap 31 of the distributor device
  • FIG. 5e A longitudinal section shown in FIG. 5e in the region of the feed line 19 through the distributor device 30, which is provided by a hollow profile slotted on top, again illustrates the fluid path b, which the cooled, hydrophobic liquid takes through the outlet gap 31.
  • the floating arrangement of the distributor device 30 in the reactor is provided by the buoyancy of the buoyancy bodies 32 (shown in FIG. 5e as one of the buoyant bodies 32) attached to the end faces of the hollow profile.
  • the arrangement of two buoyancy or float 32 at the two end faces of the hollow profile 30 are shown in FIG. 5f.
  • the buoyant bodies 32 form end seals, so that the liquid supplied through the supply line 19 can only escape through the outlet gap 31.
  • the supply line 19 is here at the center of the hollow profile
  • a simple box-shaped channel is used as the flow channel 102
  • a belt conveyor is shown, which represents a device in which the hydrophobic medium rests, while the wave edge is a moving channel.
  • Fig. 3 shows the flow channel in an annular embodiment, there moves the whole vessel with the therein hydrophobic medium of the outside of the vessel arranged pipetting away.
  • FIGS. 2 a, 4 and 3 have a receiving section 102 'of the receiving vessel, on which by means of a feed line 19, see FIGS. 3 and 4, corresponding cooling devices reach the approximately -5 to approx. 30 0 C cooled hydrophobic fluid is filled into the receptacle.
  • the supply line is not shown in Fig. 2a.
  • the pipetting device 3 is arranged, which in the present case consists of a box-shaped vessel 4, from whose bottom side, which is understood in the present case as a wall, a plurality of arranged in rows of needles 5 extend.
  • the cannulas 5 are attached at an angle of inclination to the surface of the hydrophobic liquid.
  • Fig. 2b The principle shown in the devices of Figs. 2a, 4 and 3, which is the basis of the method of the present invention, is illustrated in Fig. 2b in a simple manner:
  • the pipetting device 3 has arranged on its bottom side cannulas 5 and is filled with an aqueous active substance mixture 11. If too much aqueous active substance mixture 11 was added to the vessel 4, the excess can run off via the outlet connection 19 '.
  • the aqueous active substance mixture is dispensed into droplets 11 'and falls onto the surface 20' of the hydrophobic liquid, not illustrated here in more detail. Change the drops immediately after touching the surface 20 'with freezing their state of aggregation and gradually form ice beads 10, which are guided by the current, see arrow b.
  • Fig. 2b also illustrates the principle of the baffle plate 17, which, as shown in Fig. 2a, along its longitudinal axis A-A by a rotation axis 17 'on the side walls of the flow channel 102 is fixed so that it protrudes into the hydrophobic liquid.
  • the surface 20 ' is lowered by the rotating baffle plate by the liquid is pressed under the baffle plate 17.
  • the resulting surge wave With the resulting surge wave, the not yet completely frozen ice beads 10 are forced into the depth and below the surface 20 'of the hydrophobic liquid, so that they continue to freeze out homogeneously.
  • the ice bead product contained in the hydrophobic liquid can be withdrawn from the flow channel 102 through the outlet port 7.
  • Fig. 4 makes the further work clearly.
  • the liquid stream contained in the ice beads is guided into a centrifuge 16 serving as a separating device, which is surrounded by a receptacle 16 '.
  • the separated hydrophobic liquid is returned by means of a supply line 15 directly into the cooling device 18, where it is given after further, or renewed cooling to the desired temperature by means of the feed line 19 at the receiving portion 2 'in the receptacle.
  • a post-separation can take place in a second centrifuge 16.
  • FIG. 3 shows the annular flow passage 102, at the receiving portion 2 'also a device for acting on the receiving vessel, here the circular groove, with ice-cooled hydrophobic liquid.
  • the liquid is brought to the desired temperature in the cooling device 18 and transferred via the supply line 19 into the receiving portion.
  • a pipetting device 3 which is likewise of a box-shaped design, is arranged which, as can be seen, is open at the top.
  • the ring-shaped designed flow channel is moved while hydrophobic medium rests until after covering a circle of the device, the hydrophobic liquid with the meantime resulting ice beads passes the suction and sucked off via the suction 8 and immediately transferred to a centrifuging device 16 for separating the hydrophobic liquid.
  • the inventive devices ice beads.
  • the particles are homogeneously frozen through, ideally spherical and the ice pearls produced in a batch have substantially the same diameter.
  • the product of this quality can be obtained because a relative velocity difference between the hydrophobic liquid and the cannulas which allow the aqueous drug mixture to drip is provided by agitating either the liquid or the cannulas, and therefore the freezing beads are close together detached from the cannulas and begin to sink below the surface of the liquid.
  • a hydrophobic liquid such as a petroleum fraction or a vegetable oil, since these substances will separate the ice beads by centrifuging Allow centrifuging at temperatures below 0 ° C.
  • the hydrophobic media can be handled safely at the prevailing temperatures, even kerosene and petroleum.
  • the method is particularly advantageous because after separation of the product, a recycle of the hydrophobic medium is possible, which makes the method advantageous from an ecological and economic point of view. LIST OF REFERENCE NUMBERS

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • Fats And Perfumes (AREA)
  • Confectionery (AREA)

Abstract

L'invention concerne un dispositif (1) de production de billes de glace (10), comportant au moins un dispositif de refroidissement (18) pour refroidir un liquide hydrophobe (20) à une température d'au moins -5 °C, et un réservoir (2, 102) contenant le liquide hydrophobe (20). Le dispositif (1) comporte également un dispositif de pipetage (3) disposé sur le réservoir (2, 102), comprenant un récipient (4) pour un mélange aqueux (11). Une pluralité de tubulures de sortie (5) qui s'amincissent, disposées dans une paroi du récipient (4'), s'étendent dans le réservoir (2, 102) depuis le récipient. Une extrémité de sortie d'une tubulure de sortie (5) est espacée de 3 à 10 cm d'une surface (20') du liquide hydrophobe (20). Le dispositif (1) comporte également au moins un appareil destiné à produire une vitesse relative entre le dispositif de pipetage (3) et le liquide hydrophobe (20). Le mélange aqueux (11) parcourt un trajet fluidique (a) du récipient (4) du dispositif de pipetage (3), à travers les tubulures de sortie (5), vers le liquide hydrophobe (20), et y forme des billes de glace (10). L'invention concerne également un procédé de production de billes de glace (10) au moyen du dispositif (1), et les billes de glace (10) produites au moyen de ce procédé.
EP10706939A 2009-03-06 2010-02-25 Dispositifs et procédés de production de billes de glace à partir d'un mélange aqueux Withdrawn EP2403635A2 (fr)

Applications Claiming Priority (2)

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DE102009011521A DE102009011521A1 (de) 2009-03-06 2009-03-06 Vorrichtung und Verfahren zur Herstellung von Eisperlen aus einem wässrigen Gemisch
PCT/EP2010/001161 WO2010099893A2 (fr) 2009-03-06 2010-02-25 Dispositifs et procédés de production de billes de glace à partir d'un mélange aqueux

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US (1) US8720211B2 (fr)
EP (1) EP2403635A2 (fr)
CA (1) CA2753653C (fr)
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WO (1) WO2010099893A2 (fr)

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DE102015000238A1 (de) * 2015-01-08 2016-07-14 Optimize Gmbh Latentwärmespeicher und Verfahren zu dessen Betrieb
CN105597622B (zh) * 2016-03-09 2017-11-21 苏州大学 结冰温度可控的用于制备微米级冰球颗粒的喷雾冷冻塔
WO2019195581A1 (fr) 2018-04-04 2019-10-10 Active Energy Systems Système d'échange de chaleur destiné à congeler un matériau à changement de phase, et procédés associés
DE102019133385B4 (de) * 2019-12-06 2022-01-27 Wolfgang Folger Vorrichtung und Verfahren zur Herstellung von Eispartikeln

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DE102009011521A1 (de) 2010-09-16
WO2010099893A3 (fr) 2010-11-18
US20120036871A1 (en) 2012-02-16
CA2753653C (fr) 2017-06-13
US8720211B2 (en) 2014-05-13
WO2010099893A2 (fr) 2010-09-10
CA2753653A1 (fr) 2010-09-10

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