KR20150081297A

KR20150081297A - Method for granulating meltable materials

Info

Publication number: KR20150081297A
Application number: KR1020157013478A
Authority: KR
Inventors: 악셀 고트; 파스칼 트리볼레트
Original assignee: 베르트람스 헤미안라겐 아게
Priority date: 2012-10-25
Filing date: 2013-10-25
Publication date: 2015-07-13
Also published as: AT513566B1; CN104884154A; CN104884154B; WO2014064239A1; AT513566A1

Abstract

The present invention relates to a method for granulating a molten material, wherein spherical prills (2) are produced in a molten material. The molten material 3 flows into the injection system including a cup-shaped spray head 12 rotating about a vertical axis, while the spray cage 10 rotates about its longitudinal axis and the droplets flow into the casing of the spray cage 10 And the droplets fall in the direction of the bottom side outlet of the solidification tower 11 between the casing of the spray cage 10 and the inner wall of the solidification tower 11. The frills 2 are conveyed through the gaseous refrigerant flowing in the longitudinal direction of the solidification tower 11. At the same time, the outer surface of the frills 2 is cooled to a temperature which is lower than or equal to the solidification temperature. The rotational velocity of the jet cage 10 and the flow velocity of the gaseous refrigerant are such that the trajectory of at least a plurality of droplets or frills 2 has a substantially smaller diameter than the diameter of the inner casing of the solidification tower 11, And is limited upwardly in such a manner as to extend inside the casing. In the heat exchanger 18, the frills 2 are further cooled.

Description

[0001] METHOD FOR GRANULATING MELTABLE MATERIALS [0002]

The present invention relates to a method for granulating a meltable material, wherein spherical prills are produced from the molten material to form a gaseous refrigerant streaming in the longitudinal direction of the solidifying tower And the outer surface of the spherical frills is cooled to a temperature that is less than or equal to the solidification temperature, followed by further cooling of the spherical frills within the heat exchanger.

In addition, the present invention relates to a solidification tower for granulating a molten material which is cooled through a gas phase medium in which spherical frills are produced and transported in the molten material while being conveyed in a longitudinal direction, a belt conveyor and a heat exchanger disposed downstream for the frills, and a vibrating transfer member and bucket elevator for the prills directed to the transfer device, in particular the prill silo, Loop or closed-loop control device including one or more sensors for detecting one or more of the measured values, such as the temperature, volume and flow rate of the media and / or air and / or frills, closed-loop control device).

The granular phase produced through the injection of molten mass is also referred to as small pearl or prill. In order to granulate the product in the melt, it is generally injected at the top of the solidification tower through a distributor formed as a sprinkler, cage, or rotary perforated plate. In these devices, drops of somewhat similar size fall into the tower, where droplets are solidified as they are cooled through co-current flow or counter-current air, Which are collected at the bottom of the tower and then cooled.

EP1243316A2 discloses a palletizing device for petroleum residues which is treated in a prilling process in the molten state. In this case, a prilling head is used which rotates about a vertical axis including the outlet openings, and through the outlet openings the molten material is centrifuged radially outwards. In this case, the liquid phase particles of the material that are centrifuged outward are solidified into a substantially spherical shape. The prilling head is placed inside a vertically upright tank. The spherical particles fall downward into a water bath located on the lower end of the tank. In this tank, cooling of the solidified pellets is performed, after which the pellets are extracted from the tank in an additional order.

US2714224A1 discloses an apparatus for granulating chemicals, especially fertilizers. In this case, the molten material flows into a sieving device or a vibration device. The individual droplets fall downward in the tank through the sieve due to gravity and solidify during the drop. At the bottom of the tank, the particles are collected and discharged. For the cooling of the particles during the drop, the cooling air is transported through the tank in the direction of backflow of the falling particles.

DE2409695 describes a method and apparatus for granulating a molten or highly concentrated material, especially when producing granules of the same particle size, such as fertilizers, sodium hydroxide and potassium hydroxide. Disadvantages of the above method according to DE2409695 are that the prill formation is not uniform, the temperature distribution in the solidification tower is not constant, the easy cleaning is impossible, and the recycling of the frills, which does not correspond to the specification during the process, have.

It is therefore an object of the present invention to achieve an apparatus and a method which enable uniform prill formation, a constant temperature distribution in the solidification tower, easy cleaning of the solidification tower, and suitable recycling of the frills that does not correspond to the specification.

This object is achieved by a method of the type mentioned at the outset, according to the invention, through the following steps, i.e. into the injection system which includes a cup-shaped spray head in which molten material is rotated about a vertical axis, And the droplets are radially discharged through the through-holes in the casing of the spray cage to fall in the direction of the bottom side outlet of the solidification tower between the casing of the spray cage and the inner wall of the solidification tower, And the flow velocity of the gaseous refrigerant are such that the trajectory of at least a plurality of droplets or frills extends upwardly in a virtual cylindrical envelope casing having a diameter slightly smaller than the diameter of the inner casing And is thus limited.

The present invention also enables the production of KOH prills having uniform morphology and structure. This is also assisted by a constant and uniform cooling of the frills falling from the spray cage, either in air flow countercurrent to the drop direction or in conjunction with it. Likewise, in such a manufacturing process, the dissolved frills are diluted with fresh water and the resulting solutions are then completely fed back to the manufacturing process, so that reusing of the frills that do not correspond to the specifications is also performed. The solidification tower is washed with "wash water" contaminated with KOH / K ₂ CO ₃ in the first wash step and rinsed with fresh water in the second step. The wash water should contain up to 40% by weight of KOH / K ₂ CO ₃ .

Preferably, further, the through-holes are formed in the shape of a circle, an ellipse, a polygon or a slit so that the discharge of the droplets can be simply matched to the desired volume.

In addition, furthermore, the wall portions of the casing of the rotating spray cage may be manufactured with through-holes having an area of at least 0.007 mm < 2 >. As a result, frills of the desired shape and size are formed.

In addition, the wall portions of the casing of the rotating spray cage may be manufactured with through-holes having an area of up to 3.2 mm < 2 >. As a result, frills of the desired shape and size are formed.

In a preferred embodiment, when producing KOH prills with a KOH concentration above 85%, particularly with a starting material having a KOH concentration of 90% to 95%, the area of the through-holes in the casing of the spray cage is between 0.007 mm < 2 & And preferably 0.032 mm 2 to 3.2 mm 2. As a result, not only can frills of a desired size be produced, but also the solidification process after ejection from the ejection head is improved, because between the surface stress through the desired size of the through-holes and other mass forces acting on the droplets An optimal relationship is achieved, which contributes to the optimal spherical shape of the frills being formed. According to a further approach, the rotational speed is controlled such that the balance between the mass of molten substance and the mass of droplets is dependent on the mass of the molten material being fed, the diameter of the ejection head, and the volume of droplets discharged in a pre- Loop or closed-loop controlled in a manner that is achieved. Optimization of the manufacturing process is achieved by limiting the rotational speed of the injection head 12 to up to 1500 rpm. Frills of uniform shape and size at the number of revolutions are achieved.

Also, in accordance with the proved point, the rotation speed of the injection head is limited downward to the extent that it exceeds 200 revolutions per minute. Frills of uniform shape and size at the number of revolutions are achieved.

Further preferably, the loci of the plurality of droplets are spaced apart from the casing of the solidification tower by a spacing of 0.1 mm or more. As a result, it is prevented that the frills can contact the wall of the solidification tower and thus adhere to or adhere to the wall, before the outer surface of the frills is cooled below at least the freezing point. As a result, the duration of use of the solidification tower is further increased since the number of cleaning procedures can be reduced.

Additionally, during the practice of the method, suitably, the outer diameter of the jetting cage is determined as a ratio of 1 to 20 to 1 to 200 relative to the inner diameter of the casing of the solidification tower, whereby the frills consistently have a uniform shape and size . &Lt; / RTI >

In a preferred embodiment, when manufacturing KOH frills with a KOH concentration of greater than 85%, particularly with a starting material having a KOH concentration of between 90% and 95%, the outer diameter of the spray cage is preferably less than the ratio of the solidification tower to the inner diameter of the casing 1 to 20 to 1 to 50. As determined, this measure is an optimal measure for the solidification process of KOH droplets after they have been discharged from the spray cage and optimally takes into account the characteristics of KOH, especially density and viscosity.

In a particularly preferred embodiment involving the preparation of KOH prills with a KOH concentration above 85%, in particular with a starting KOH concentration of 90% to 95%, the following process parameters are used. At a temperature of 200 to 350 ° C and a concentration of 90% to 95%, the density of KOH is 1750 to 1850 kg / m 3 and the viscosity thereof is 2.5 to 3.5 mPa · s. In addition to these conditions, the area (pore size) of the through-holes in the casing of the spray cage is from 0.007 mm 2 to 3.2 mm 2 and the spray cage speed is from 100 to 1000 revolutions per minute. As a result, sufficiently small KOH frills can be produced that are rapidly cooled and simultaneously hardened and stabilized.

According to a further preferred method step, the closed loop control device is used to continuously control the rotational speed of the jet cage through the drive. With this rapid closure or open loop control of the injection cage, a rapid reconditioning can be performed when the temperature of the caustic calibers fluctuates, so that the volume of droplets discharged from the spray cage is relatively longer with relatively small tolerances Can be maintained over the operating period.

In addition, in addition, the rotation speed of the spray cage may be controlled from open loop to closed loop depending on the supplied mass of the molten material and / or the viscosity of the mass. As a result, frills of uniform shape and size are produced.

Also, rapid matching of the volume of droplets discharged can be facilitated by the rotational velocity of the spray cage being varied in the same direction when the viscosity of the molten material is varied.

If the mass of the molten material supplied varies, further preferably, the rotational speed of the spray cage is varied in the same direction. Accordingly, suitably the size and shape of the frills can be kept stable.

According to a further preferred approach, an air guide is performed in cocurrent with the falling direction of the frills in the solidification tower, and a uniform and controlled cooling of the falling frills is carried out.

In addition, in various applications, it may be provided, suitably, in such a manner that the air guide is performed in the reverse direction of the falling of the frills within the solidification tower. A uniform and controlled cooling of the falling frills is thus carried out.

Preferably, the open loop and closed loop control of the amount or the temperature of the gaseous medium formed through the air when guided by the direction of movement of the prills in the solidification tower, preferably through air, , The amount of the supplied medium is increased when the temperature rises, and / or the temperature is adjusted to be decreased. As a result, a uniform and controlled cooling of the falling frills is performed.

Preferably, open loop and closed loop control of the amount or the temperature of the gaseous medium, which is preferably formed through the air when guided countercurrently with respect to the direction of movement of the frills in the solidification tower, Depending on the temperature of the air, when the temperature rises, the amount of medium or air supplied is increased and / or the temperature is adjusted to decrease. As a result, a uniform and controlled cooling of the falling frills is performed.

In addition, preferably the medium or air for cooling spherical frills can be made to circulate in a closed system. As a result, independence from ambient air is realized.

Also suitably, the frills having a size and / or shape and / or weight different from the product specification, and / or the melts containing a high content of nickel or nickel oxide that have been formed during the prill manufacturing process are separated. As a result, frills with high purity are formed. Also, preferably, the separated frills are dissolved, reprocessed, optionally purified, and re-introduced into the manufacturing process as caustic. As a result, the material that has been lost during the manufacturing process can be used again.

In addition, the preferred sequence of the method is characterized in that the parts which are parts of the spray cage, the deflection position and the collecting tank and which are in contact with the alkali solution are contacted with oxygen and the adhesion of the frills, To prevent this, it is covered with nitrogen.

Preferably, the nitrogen addition can be carried out continuously, or periodically, to prevent contact with oxygen.

According to a preferred approach, the solidification tower is washed, wherein the wash water is pumped from the wash water tank to the top of the solidification tower, and the funnel-shaped outlet of the solidification tower and its walls are washed with wash water and subsequently with fresh water. The wash water may be purged again and then flowed back into the wash water circuit. Fresh water is also purified and flows into the circuit. As a result, high utilization of wash water and fresh water and therefore less water consumption than in conventional installations is achieved.

According to the method of the invention, preferably, the washing water is used for cleaning up to the lower or the same concentration of the KOH / K ₂ CO ₃ 40% than being played back can be used for cleaning again.

The long service life of the equipment is suitably achieved by removing the spray cage and spray head from the solidification tower for cleaning, heating at a maximum of 200 ° C in a steam bath for several hours, and then preheating to a maximum of 400 ° C The spray cage and spray head can be accomplished through being mounted on the solidification tower again. During the cleaning process outside of the solidification tower, the already heated second injection cage is mounted at the location of the contaminated portion to stop the operation of the solidification tower for as short as possible.

Further preferably, the cleaning process is performed according to the determined degree of contamination or periodically. As a result, it can be ensured that the solidification tower is only shut down for a short time.

Preferably, according to an additional method step, the inner surface of the funnel-shaped outlet of the solidification tower is heated via an electric trace heating system. This prevents the high temperatures of the frills from sticking to the inner surface and thereby prevents clogging of the outlet funnel.

Also, in the method sequence, preferably the inner surface of the outlet funnel is heated to a maximum temperature of 180 ° C, preferably to a maximum temperature of 100 ° C. This prevents the high temperatures of the frills from sticking to the inner surface and thereby prevents clogging of the outlet funnel.

In addition, the object of the invention is also achieved, independently, by a device of the type mentioned at the beginning, in which the supply line for the molten material in the solidification tower is a cup-shaped spray head with a spray cage having a substantially cylindrical, Wherein the spray head is rotatably mounted about an axis of rotation extending parallel to the longitudinal axis and connected to the rotational drive device, the casing of the spray cage discharging the droplets of molten material in a radial direction And a plurality of through-holes distributed over the surface of the spray cage for the purpose of preventing the spray cage from being damaged.

In a preferred embodiment, the through-holes in the spray cage are formed in a circular, elliptical, polygonal, or slit shape so that frills with different shapes can be produced.

In addition, a suitable use of the method can also be achieved when the through-holes in the casing of the rotating spray cage are formed with a surface of at most 0.007 mm2 to 3.2 mm2. As a result, frills of the desired shape and size are formed.

According to a preferred refinement, the outer diameter of the spray cage is 1 to 20 to 1 to 200 in relation to the inner diameter of the casing of the solidification tower. In this case, preferably, depending on the amount of the outwardly projecting mass of the prills to be produced, and the amount thereof, the caustic collar of a suitable mass is located in the injection cage, respectively, so that the highest possible temperature uniformity is achieved The size and shape of the frills can be optimally predetermined even when the requirements are different from each other.

BRIEF DESCRIPTION OF THE DRAWINGS For a better understanding of the present invention, the invention will be described in more detail with reference to the following drawings.

BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a schematic diagram showing a very simplified process drawing of equipment for the production of KOH prills.
Fig. 2 is a schematic circuit diagram showing the apparatus of Fig. 1 in a very simplified manner. Fig.
Figure 3 is a side view that greatly simplifies and schematically illustrates the injection head of the plant shown in Figure 1, including a corresponding drive system.
Figure 4 is an enlarged view, partially cut away, of the injection cage of the injection head shown in Figure 2, including through-holes disposed in a portion of the cylindrical casing of the injection cage.
Figure 5 is a schematic diagram showing a very simplified process drawing of a plant for the production of KOH prills.

The matters to be ascertained prior to the description of the contents are that the same members in the differently described embodiments each have the same reference numeral and the same part name, and the disclosures included in the entire specification have the same reference numerals and the same And can also be dedicated to members having respective component names. Also, positional indications selected in the specification, such as top, bottom, side, and the like, are directly related to the drawings and shown in the drawings, and are also transferred to the new position in accordance with the meaning of the position change. In addition, individual features or feature combinations in the illustrated and described embodiments may themselves be indicative of independent, inventive, or inventive solutions.

It should be understood that all instructions for value ranges in the context of the specification are intended to include the ranges of values, including any and all subranges. For example, the indication of 1 to 10 indicates that starting from lower limit 1 and upper limit 10, all subranges are included together, that is, all subranges start at one or more lower bounds and end at an upper bound of 10 or less , Such as from 1 to 1.7, or from 3.2 to 8.1 or from 5.5 to 10.

The embodiments illustrate possible variations of the process in the example for obtaining KOH prills and it should be noted that the present invention is not limited to the specifically illustrated variants of the invention, Various combinations of these are also possible and these variations are based on the skill of the ordinary technician working in the art based on the teaching of the handling of the technology through specific inventions. In addition, all modifications that may be considered as possible through combinations of the individual details of the illustrated and described variants are also included in the scope of protection.

In Figure 1, an independent embodiment by itself is shown in the case of a process for obtaining a KOH prill, wherein the same reference numerals and parts names as in all figures are used for the same members, respectively. In order to avoid unnecessary repetition in the subsequent figures, the detailed description of preceding figures is referenced and utilized.

Finally, it should be noted that for the sake of a better understanding of the method of the present application, the components of the members or members thereof are shown to be different and / or enlarged and / or reduced in part from a constant scale factor It is a point.

The subject matter underlying specific inventive solutions can be found in the specification of the present application.

Figure 1 shows a facility 1 for producing KOH prills 2 with concentrated caustic.

To this end, the liquid caustic potash 3 is fed to the collection tank 7 via a line 4 and a deflection position 5 and a line 6 connected to this deflection position. In the region of the deflection position 5, it is further possible to provide a heat exchanger 8 for heating the caustic pots to a temperature lower than or equal to 400 캜. To this end, the heat exchanger is heated to a high temperature medium, such as steam, via schematically illustrated lines.

It is also conceivable to guide the line upward from the bottom, for example from the bottom of the solidification tower, instead of feeding the caustic collar 3 through the line 6 from above with the use of gravity as shown in Fig. In this case, the transfer of the molten material 3 towards the upper region of the tower is carried out by a pump arranged in the line, thereby ensuring a continuous and controllable supply of the starting material for the prilling process as well. For example, the line starting from the bottom may be switched directly to the line 9 shown in Fig. 1 below the outlet of the collection tank 7, or may be in the line.

The heated caustic potash 3 is then fed into the spray cage 10 of the spray head 12 located inside the solidification tower 11 via line 9.

The function of the ejection head, which can be rotated through a driving device, for example an electric motor, is described below with reference to Fig.

The concentrated caustic droplets discharged through the jetting head are cooled in the interior of the solidification tower 11, that is to say in the solidification tower at least the outer surface is cooled below the solidification temperature of the liquid caustic potash, In particular, ball-shaped KOH frills 2 are formed.

Cooling of the droplets for the formation of the KOH frills 2 is carried out in this embodiment via the transfer device 13, for example a blower, or a condenser for vapor phase media, preferably air, Is carried out through the air supplied via line 14 in the region, which air flows through the solidification tower 11 in the vertical direction and in the direction of the bottom side outlet. The air flow is used for cooling the frills 2.

In an alternative embodiment shown in Fig. 5, the gaseous medium is sucked through the solidification tower 11 by a negative pressure. The fan 55 produces a preferably adjustable negative pressure within the negative pressure tank 54. Vapor medium is sucked from the solidification tower 11 through the line 53. Vapor media, through one or more inlets 52, preferably through a plurality of inlets, reaches the solidification tower 11 in the upper region. As a result, a cooling flow parallel to the direction of the falling frills 2 is also produced.

The solidified prills 2 at least in the region of the outer surface are fed to a conveying device, in particular a belt conveyor 17, via a line 16 connected to the bottom side outlet 15 of the solidification tower 11. The frills from this belt conveyor are conveyed to a heat exchanger 18 and are further cooled while being pierced through the heat exchanger. For this purpose, the heat exchanger 18 may be perfused through the lines 19 into vapor or liquid refrigerant.

In the heat exchanger 18 the frills 2 are cooled to a temperature of up to 80 ° C and preferably to a temperature of up to 70 ° C and fed to the conveying device 21 through the connected oscillating conveying member 20, For example, to a bucket elevator that stores frills in a frills silo 22.

The inner surfaces of the deflection position 5 and / or the collection tank 7 and / or the solidification tower 11 and / or the spray cage 10 are connected via lines as schematically illustrated to prevent contact with oxygen It can be washed with nitrogen. It is also preferable to provide a heating device 23 in the region of the bottom side outlet 15 which is connected to the outlet 15 in the form of a funnel for example at a temperature of from 50 to 180 DEG C, Particularly preferably up to 150 ° C, very particularly preferably up to 100 ° C, or maintained at this temperature.

Since the caustic potash 3 and prills 2 are very highly hygroscopic, it is preferred that the entire facility 1, in particular the caustic potash 3 and the prills 2, May also be covered with dry gas, especially dry air, or with inert gas.

Also, for cleaning the solidification tower 11, a wash water tank 24 is disposed. This wash water tank 24 is connected to the bottom side outlet 15 of the solidification tower 11 via the connection line 25 and on the other hand the wash water is supplied by the transfer pump 26 Side inlet port of the solidification tower 11. The solid-

An open loop or closed loop control device 28, which may be connected to additional memories 29 and additional computers and data measurement displays and receiving devices, for open loop and / or closed loop control of the facility 1, Are schematically shown. The open loop or closed loop control device 28 is connected to the sensor 32 for measuring the air temperature in the region of the bottom side outlet 15 via line 30 and / Is preferably connected to a sensor 34 for measuring the flow rate of the refrigerant, in particular the flow rate of air, within the solidification tower 11 and is connected to the line 30 via a line 30, for example via a non-contact infrared scanner, Is connected to a sensor (32) for measuring the surface temperature of the frills (2). To the same extent, additional sensors 35, 37 and 38 may be connected to the open loop or closed loop control device 28 via lines 33 and 39.

All the lines connected to the open loop or closed loop control device 28 are connected to the sensors 32,34-38 either by the lines themselves or by the injection head 12, the conveying device, the belt conveyor 17 Regardless of whether it is the lines leading to the driving devices of the conveying device 21 or the vibrating transferring member 20 or of the transferring device 21, But may also be formed through bus lines or bus systems as are known to those of ordinary skill in the art of control. The same applies to the drive motor 40 for the injection head 12.

2, there is shown a corresponding sensor 28 for detecting the air temperature for cooling spherical frills, a sensor 32 for detecting the volume and flow rate of air, and a sensor 32 for detecting the temperature of air in the funnel- The circuit diagram of the open loop and closed loop control device 28 including the sensor 32 for detecting the temperature of the frills 2 is shown again. The temperatures are detected by thermography, in other words the temperature measurement of the frills 2 is carried out in a noncontact manner, preferably in laminar flow, and displayed in accordance with the temperature detection using the thermal sensitive sensors 34-38 do. The data is then collected in, for example, a microprocessor 28, that is, the central open-loop and closed-loop control unit 28, where all the modules of the processor are integrated on one microchip, , And in an alternative manner, memories 29 may also be provided for evaluation.

3, the injection head 12 and the drive motor 40 assigned to this injection head are shown in enlarged scale.

The drive motor 40 is connected to the injection cage 10 via a coupling and a drive shaft 41 so that the injection cage is preferably centered about the longitudinal axis 42 which is also identical to the longitudinal axis of the drive shaft 41 Can be rotated.

Here, the injection cage 10 is illustrated schematically as a one-dot chain line. Feed lines or feeders 43 and 44 are provided in the region of the drive device or drive motor 40 for the injection cage 10. [ So that the molten caustic collar 43 is supplied through the line or feeder 43 so that the caustic colli can flow into the interior of the spray cage 10 through the outlet 45. Nitrogen to cover the interior of the spray cage 10 can be supplied via the outlet 46 through the feed line or feeder 44.

The injection cage 10, shown in an enlarged view in Figure 4, is connected to the drive shaft 41 in a rotationally fixed manner and thus rotates about a longitudinal axis 42. [ The cylindrical casing of the injection cage 10 has a plurality of through-holes 47 distributed throughout the casing, and only some through-holes as an example of these through-holes are shown in Fig. The penetrating cross-section of the through-holes 47 is such that droplets having a predetermined volume according to the rotational speed of the spray cage 10 and the mass of molten caustic potash 3 supplied thereto are introduced into the cylindrical casing of the spray cage 10 48 so as to pass through the through-holes 47 of the first and second passages 48, 48.

4 shows the through holes 47 of the casing 48 of the spray cage 10 having various shapes such as elliptical through holes 49, circular through holes 50 and angular through holes 51, Respectively.

Through rotation of the spray cage 10, small droplets are centrifuged into the solidification tower, and in this solidification tower, the droplets solidify through cooling to form so-called frills 2. In this case, .

The method according to the invention for producing said frills 2 with liquefied caustic potash 3 will now be described in more detail in accordance with the equipment 1 shown in Figs.

The method for obtaining KOH frills is divided into the following four steps. - the preparation of KOH frills, - the treatment of KOH frills, - the washing of the solidification towers, - the re-supply of frills that do not correspond to the specification for the acquisition of KOH frills.

For the production of KOH frills 2, the liquid caustic potash 3 is concentrated (less than or equal to 95 weight percent) to form deflection points 4 and 6 at deflection positions Is fed into the collection tank 7 via the line 5 and from the collection tank via line 9 to the spray cage 10 which rotates with the injection head 12 arranged in the solidification tower 11, / RTI > The caustic collie flows into the collection tank 7 through the biasing position 5 through its inherent weight. However, instead of feeding the melt through the gravity to the injection cage 10, the melt may be pumped into the injection cage using a pump.

The through-holes 47 in the casing or sidewall portions of the spray cage 10 have a diameter or cross-section of up to 1 mm and through the centrifugal force exerted on the caustic collar through the rotation of the spray cage 10, Passes through the through-holes (47) and is discharged into the solidification tower (11). Through the deformation of the shape of the through-holes 47, frills having a circular, elliptical, polygonal, slit-like shape and other shapes can be formed. The through-holes 47 in the wall portions of the casing 48 of the rotating spray cage can be manufactured to include an area of 0.007 mm 2 to 3.2 mm 2.

The rotational speed of the spray cage 10 is adjusted according to the mass of the caustic pot 3 to be supplied, the diameter of the injection head 12, and the volume of droplets formed at predetermined time units. The rotational speed of the injection head 12 is 200 to 1500 rpm and the rotational speed of the injection cage 10 can be continuously adjusted by the closed loop control device through the drive device. In addition, the rotational speed of the spray cage 10 may be determined through the addition or alternatively of the mass of the caustic potash 3 supplied and / or the viscosity of the caustic potash 3.

In this case, preferably, the rotation speeds of the injection heads 12 to the injection cage 10 are set such that the loci of the individual droplets are spaced apart from each other by the spacing of the solidification towers 11 in accordance with the aforementioned physical values such as the medium, And is spaced apart from the inner wall of the solidification tower by a spacing of at least 0.1 mm.

The droplets of caustic cali are centrifuged outwardly from the spray cage 10 through the through-holes 47 of the spray cage through rotation of the spray cage 10. [

The droplets 2 to be discharged are crystallized while falling downward in the solidification tower, while being cooled with a gas flow, particularly ambient air, or with an inert gas in the solidification tower. The droplets are discharged through the funnel-shaped end of the injection tower equipped with the heating device 23 at a temperature of 50 to 180 ° C, preferably 110 to 180 ° C.

The cooling air or gas can be guided in parallel with the falling frills 2. However, the cooling and crystallization of the frills 2 can also be carried out with gas or air flowing backwash. The prills 2 exit the solidification tower 11 and fall down onto the belt conveyor 17 via line 16 and are transported towards the heat exchanger 18.

The air heated in accordance with the cooling of the frills 2 is removed from the solidification tower 11 through a ring collector connected to the exhaust blower through a cleaning tower. Through the supply and discharge of air, a constant temperature that can vary by itself can be generated in the solidification tower. As a result, undesirable water consumption can be prevented by the resulting frills. Used air is purified and sent to the atmosphere. The wash water is discharged through the overflow in the wash water tank (24).

If conventional ambient air is used as the refrigerant for the spherical frills 2, the ambient air is fed into the solidification tower, and after the air is discharged from the solidification tower, it is purged and filtered, .

Cooling and crystallization of prills using air or other vapor media can likewise be carried out in a closed system where the air to vapor medium is purified and recirculated therein.

It is also possible to adjust the ratio of the outer diameter of the spray cage to the inner diameter of the casing, preferably for the manufacture of the spherical frills 2. [ Preferably, good results are achieved when determined as a ratio of 1: 20 to 1: 200. Likewise, a crucial factor for the production of spherical frills is the mass of the caustic potash 3 and its viscosity, which is proportional to the rotational speed of the spray cage, i.e. the mass or viscosity of the spray cage 10, The rotational speed must also be increased. If the mass or viscosity decreases, preferably the rotational speed of the jet cage also has to be reduced.

When preparing KOH frills with a KOH concentration of more than 85%, in particular with a KOH concentration of 90% to 95%, preferably the area of the through-holes in the casing of the spray cage is between 0.007 mm < 2 & And preferably 0.032 mm2 to 3.2 mm2. As a result, not only can frills of a desired size be produced, but also the solidification process is improved after ejection from the ejection head, because between the surface stresses through the desired size of the through-holes and other mass forces acting on the droplets An optimal relationship is achieved, which contributes to the optimal spherical shape of the frills being formed.

Likewise preferably, when preparing KOH frills with a KOH concentration of greater than 85%, particularly with a starting material having a KOH concentration of from 90% to 95%, the outer diameter of the spray cage is preferably less than the ratio of the solidification tower to the inner diameter of the casing 1 to 20 to 1 to 50. As determined, this measure is an optimal measure for the solidification process of KOH droplets after they have been discharged from the spray cage and optimally takes into account the characteristics of KOH, especially density and viscosity.

In the heat exchanger 18, the frills are cooled to a temperature of less than or equal to 80 캜, preferably less than or equal to 50 캜, in the rotating cylinder. Air supply to the heat exchanger 18 is performed through the lines 19. The frills from the heat exchanger 18 are conveyed into the prill silo 22 via the oscillating belt conveyor 20 and the conveying device 21. [

Interfering nickel residues are introduced into the solidification tower, particularly into the spray cage 10, by the caustic colli, and clog the through-holes 47 of the spray cage 10. [ To ensure that the injection process is only briefly interrupted, two injection cages 10 are provided. In other words, the nickel-contaminated spray cage can be manually replaced with a clean spray cage, cleaned, and then cleanly reused.

For the cleaning of the spray cage, the spray cage is removed from the solidification tower with the spray head and disassembled at the spray head to heat up to a maximum of 200 占 폚 in the steam bath for several hours, and then preheated to a maximum of 400 占 폚, The cage 10, in a subsequent cleaning process, reassembles the second injection cage into the ejection head which immediately disassembled it and mounts it in the solidification tower 11. [ Therefore, only the spray cage needs to be exchanged, whereas the spray head is separated from the manufacturing process only for a short time. The cleaning process is performed according to the defined degree of contamination. However, the cleaning process can also be performed periodically.

The wash water is pumped from the wash water tank 24 to the top of the solidification tower 11 by the pump 26, in order to ensure that there is no residue in the facility 1, particularly for cleaning the solidification tower 11. [ The funnel-shaped outlet with the heating device 23 and the walls of the solidification tower are washed with wash water and then with cold water. The wash water is used until it reaches a concentration of KOH / K ₂ CO ₃ of less than 40%, and is then treated with a neutralization reaction.

The heat exchanger 18 is likewise washed with wash water, and the wash water is collected and pumped into the wash water tank 24.

1: facility 2: frills
3: Caustic Carly 4: Line
5: deflection position 6: line
7: collecting tank 8: heat exchanger
9: line 10: injection cage
11: solidification tower 12: jet head
13: blower 14: line
15: outlet 16: line
17: belt conveyor 18: heat exchanger
19: Line 20: Vibration transfer member
21: Feeding device 22: Frill silo
23: heating device 24: washing water tank
25: connection line 26: transfer pump
27: Line 28: Microprocessor
29: memory 30: line
31: Line 32: Sensor
33: Line 34: Sensor
35: sensor 36: sensor
37: sensor 38: sensor
39: line 40: drive motor
41: drive shaft 42:
43: feeder 44: feeder
45: outlet 46: outlet
47: through hole 48: casing
49: elliptical through hole 50: circular through hole
51: angular through-hole 52: inlet
53: line 54: negative pressure tank
55: Fans

Claims

A method for granulating a molten material, wherein spherical frills (2) are produced from the molten material (3) and conveyed through the gaseous coolant flowing in the longitudinal direction of the solidification tower (11) ) Is cooled to a temperature that is lower than or equal to the solidification temperature and then the spherical frills (2) are further cooled in a heat exchanger (18), wherein said molten material has a vertical axis The injection cage 10 rotates about its longitudinal axis and droplets flow into the injection system including the cup-shaped injection head 12 rotating about the center of the injection cage 10, And is dropped in the direction of the bottom side outlet of the solidification tower 11 between the casing 48 of the injection cage 10 and the inner wall of the solidification tower 11, (10) The total speed and the flow velocity of the gaseous refrigerant are such that the locus of at least a plurality of droplets or frills 2 is smaller than the diameter of the inner casing of the solidification tower 11 in the inside of a virtual cylindrical casing Wherein the molten material is confined upwardly in an extended manner.

The method of claim 1, wherein the molten material (3) is formed through KOH.

The method of claim 1 or 2, wherein the through-holes (47) are formed in a circular, elliptical, polygonal, or slit shape.

4. A device as claimed in any one of the preceding claims, characterized in that the walls of the casing (48) of the rotating spray cage (10) are manufactured with through-holes (47) having an area of at least 0.007 mm & Of the molten material.

Characterized in that the walls of the casing (48) of the rotating spray cage (10) are manufactured with through-holes (47) having an area of at most 3.2 mm < 2 > A method of granulating a material.

A method according to any of the preceding claims, wherein the rotational speed is selected such that the volume of the molten material (3) supplied, the diameter of the injection head (12) Is controlled in an open-loop or closed-loop manner in such a way that a balance is achieved between the mass of said molten material (3) and the mass of said droplets.

Characterized in that the rotational speed of the injection head (12) is limited upwards to a maximum of 1500 revolutions per minute, preferably up to 1000 revolutions per minute Granulation method.

The method of any one of the preceding claims, wherein the rotational speed of the injection head (12) is limited downward to a degree that exceeds a maximum of 200 revolutions per minute.

The method of any one of the preceding claims, wherein the loci of the plurality of droplets are spaced apart from the casing of the solidification tower by a spacing of at least 0.1 mm.

Wherein the outer diameter of the spray cage (10) is in the range of 1 to 20 to 1 to 200, preferably 1 to 20 to 1 to 50, in relation to the inner diameter of the casing of the solidification tower (11) By weight based on the weight of the molten material.

A method according to any one of the preceding claims, wherein the rotational speed of the injection cage (10) is continuously regulated by the closed loop control device via the drive device.

Characterized in that the rotational speed of the injection cage (10) is controlled in an open loop or closed loop depending on the mass of the molten material (3) supplied and / or the viscosity of the mass Of the molten material.

The method according to any one of the preceding claims, wherein the rotational speed of the spray cage (10) varies in the same direction when the viscosity of the molten material (3) is varied.

The granulation method of a molten material according to any one of the preceding claims, wherein the rotational velocity of the injection cage (10) varies in the same direction when the mass supplied of the molten material (3) fluctuates .

The method according to any one of the preceding claims, wherein the vapor phase medium flows in parallel with the falling direction of the spherical prills / droplets (2) in the solidification tower (11) .

15. The method according to any one of claims 1 to 14, characterized in that the gas phase medium is guided in the solidification tower (11) in a counterflow direction with respect to a falling direction of the spherical frills / droplets (2) A method of granulating a material.

The method according to any one of the preceding claims, wherein the amount of the gas phase medium and / or its temperature, preferably formed through air when guided in cocurrent with the direction of movement of the prills (2) in the solidification tower, Characterized in that the amount of the medium fed is increased and / or the temperature is adjusted to decrease when the temperature rises, depending on the temperature of the medium in the region of the outlet.

The method of any one of the preceding claims, wherein the amount of media or air and / or its temperature when guided countercurrent to the direction of movement of the frills within the solidification tower is dependent on the temperature of the medium or air in the region of the media outlet , The amount of medium or air fed is increased, and / or the temperature is adjusted to decrease when the temperature rises.

Method according to any one of the preceding claims, characterized in that the medium for cooling the spherical frills (2) is recirculated in a closed system.

7. A method according to any one of the preceding claims, wherein the discharge air is purified and discharged to the atmosphere.

A method according to any one of the preceding claims, wherein fresh ambient air is continuously fed into the system as cooling air.

Method according to any one of the preceding claims, characterized in that the spherical frills (2) having a size and / or shape and / or weight different from the product specification, and / or a high content of nickel or nickel oxide &Lt; / RTI > wherein the molten materials are separated.

Characterized in that the separated frills (2) are dissolved, reprocessed, optionally purified and again introduced into the manufacturing process as a caustic (3). The process according to any one of the preceding claims, A method of granulating a material.

Characterized in that the parts in which the spray cage (10), the deflection position (5) and the collection tank (7) are in contact and which are in contact with the alkali solution are covered with nitrogen Of the molten material.

A method according to any one of the preceding claims wherein the nitrogen addition is carried out continuously or periodically.

Method according to one of the preceding claims, characterized in that the solidification tower (1) is washed and the washing water thus pumped from the wash water tank (24) to the top of the solidification tower (11) Characterized in that the funnel-shaped outlets (45, 46) and their wall portions are washed with wash water, and subsequently with fresh water.

A method according to any one of the preceding claims, wherein said wash water is used until a maximum concentration of 40% KOH / K2CO3 is reached.

8. A method according to any one of the preceding claims, wherein the spray cage (10) and the spray head (12) are stripped from the solidification tower (11) for cleaning and heated for up to 200 ° C in a steam bath for several hours , And then to a maximum of 400 ° C, whereby the spray cage (10) and the injection head (12) are again mounted to the solidification tower (11).

The method according to any one of the preceding claims, wherein the cleaning process is performed periodically or according to a predetermined contamination level.

A method according to any one of the preceding claims, characterized in that the inner surface of the outlet funnel of the solidification tower (11) is heated, in particular through an electric tracing heating device.

The method according to any one of the preceding claims, wherein the inner surface of the exit funnel is heated to a maximum temperature of 180 DEG C, preferably a maximum temperature of 100 DEG C.

32. A process according to any one of claims 2 to 31, wherein the KOH frills are made with starting material (3) having a KOH concentration above 85%, in particular with a KOH concentration of 90% to 95% Wherein the area of the through-holes in the casing is 0.007 mm < 2 > to 4.53 mm < 2 >, preferably 0.032 mm < 2 >

32. A process according to any one of claims 2 to 32, wherein the KOH frills are made of a starting material (3) having a KOH concentration above 85%, in particular a KOH concentration of 90% to 95% Wherein the outer diameter of the solidification tower is 1 to 20 to 1 to 50 in relation to the inner diameter of the casing of the solidification tower.

34. A process according to any one of claims 2 to 33, wherein the KOH frills are made of a starting material (3) having a KOH concentration above 85%, in particular a KOH concentration of 90% to 95% Wherein the temperature of the molten material (3) is 200 to 350 占 폚, the area of the through-holes in the casing of the injection cage is 0.007 mm2 to 3.2 mm2, and the injection cage speed is 100 to 1000 rpm. A method of granulating a substance.

A solidification tower (11) for granulating a molten material (3), wherein spherical prills (2) are produced in a molten material (3) and transported in the longitudinal direction of the solidification tower (11) And the solidification tower comprises a collection tank disposed upstream for the caustic colli 3, a belt conveyor 17 and heat exchanger 18 disposed downstream for the prills 2, a conveying device, Particularly the temperature 32 of the medium to air and / or frills, the volume 34 and the flow rate 35 of the media and air and / or frills, as well as the vibratory transfer member 20 and the bucket elevator 21 for the frills, Loop or closed-loop control device including at least one sensor for detecting one or more of the same measurement values. In the solidification tower, the supply line for the molten material is substantially cylindrical and has a vertical longitudinal axis Having a spray Type ejection head 12 having a nozzle 10 and the ejection head 12 is rotatably mounted about a rotation axis extending parallel to the longitudinal axis and connected to a rotation drive device And the casing 48 of the spray cage 10 comprises a plurality of through-holes 47 distributed over the surface of the spray cage for radially discharging droplets of the molten material 3 Solidification towers feature.

36. A solidification tower according to claim 35, wherein the solidification tower is a KOH-prilling-solidification tower for producing KOH frills through granulation of the molten material (3) formed through KOH.

37. The solidification tower according to claim 35 or 36, wherein the through-holes in the injection cage (10) are formed in a circular, elliptical, polygonal, or slit shape.

37. A device according to any one of claims 35 to 37, characterized in that the through-holes (47) in the casing (48) of the rotating spray cage (10) are formed to comprise an area of 0.007 mm2 to 3.2 mm2 Solidification tower.

41. A method as claimed in any one of claims 35 to 38, wherein the outer diameter of the spray cage (10) is from 1 to 20 to 1 to 200, preferably from 1 to 20, in relation to the inner diameter of the casing (48) One to twenty to one to fifty.