WO2014187690A1 - Unité de séparation et procédé pour séparer des sels d'une substance détergente - Google Patents

Unité de séparation et procédé pour séparer des sels d'une substance détergente Download PDF

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Publication number
WO2014187690A1
WO2014187690A1 PCT/EP2014/059622 EP2014059622W WO2014187690A1 WO 2014187690 A1 WO2014187690 A1 WO 2014187690A1 EP 2014059622 W EP2014059622 W EP 2014059622W WO 2014187690 A1 WO2014187690 A1 WO 2014187690A1
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WIPO (PCT)
Prior art keywords
crystallizer
hydrocyclone
salt crystals
separation
separating
Prior art date
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PCT/EP2014/059622
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German (de)
English (en)
Inventor
Ansgar Kursawe
Markus Kinzl
Ralph Joh
Rüdiger Schneider
Original Assignee
Siemens Aktiengesellschaft
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Filing date
Publication date
Application filed by Siemens Aktiengesellschaft filed Critical Siemens Aktiengesellschaft
Publication of WO2014187690A1 publication Critical patent/WO2014187690A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/0059—General arrangements of crystallisation plant, e.g. flow sheets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/50—Carbon oxides
    • B01D2257/504—Carbon dioxide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
    • B01D53/1425—Regeneration of liquid absorbents

Definitions

  • the invention relates to a separation unit for the separation of salts from a washing medium, comprising a crystallizer with a crystallization chamber for the formation of salt crystals and with a classifier for separating the salt crystals according to their particle size. Furthermore, the invention relates to a process for the separation of salts from a washing medium.
  • amines with large alkyl groups, cyclic amines, amino acids or amino acid salts used.
  • the amines used form either carbamates with carbon dioxide, or the carbon dioxide reacts in the wash medium indirectly to bicarbonate and a protonated amine.
  • the temperature-resistant salts optionally promote corrosion and change the flow properties of the washing medium negative.
  • the salts crystallize out of control and cause turbulence, for example, in the absorber or lead to blockages in the pipes or pumps.
  • a disadvantage resulting from the low solids content and the associated low surface area of the salt crystals is an insufficient performance of the crystallizer.
  • the particle growth and thus the separation from the liquid phase take place on the surface of the crystals.
  • Small crystals have a high specific surface, but are difficult to separate.
  • a classifying crystallizer which provides a high mass of particles per volume, allows the growth of large and easily separable particles while providing a high absolute surface area for high separation efficiency.
  • An essential aspect in the design of the crystallizer is therefore the classification of the particles.
  • the classification serves both to increase the particle density through an enrichment of the particles in the crystallizer, as well as a simpler separation of solids. By crystallizers used so far, this can not be guaranteed.
  • a first object of the invention to provide a separation unit, by means of which the salts formed by reaction in the washing medium can be effectively separated from this with recovery of the washing medium.
  • a second object is to provide a corresponding method for the separation of salts from a washing medium.
  • the first object of the invention is achieved by a separation unit for the separation of salts from a washing medium, comprising a crystallizer with a crystallization chamber for the formation of salt crystals and with a classifier for separating the salt crystals according to their particle size, and comprising a first pump connected to the crystallizer fluidly for drawing off a first partial stream enriched with salt crystals, and a second pump fluidically connected to the crystallizer for discharging a second partial stream depleted of salt crystals, wherein the first pump and the second pump are each fluidically connected to a separating unit.
  • the invention takes into account that the separation units previously used for the separation of salt crystals from a washing medium for the separation of salt crystals from a washing medium are only partially suitable. Due to the insufficient separation of small and large particles within the washing medium, a suspension supplied from a crystallizer to a solid-liquid separation can not be separated by means of a Separate a centrifuge. The necessary use of additional equipment, such as the use of a decanter to thicken the suspension, is associated with additional equipment and expense.
  • the invention recognizes that effective separation of the salt crystals from the washing medium is possible if two pumps are connected to the crystallizer for discharging partial streams of the suspension.
  • the separation unit comprises a first pump connected fluidically to the crystallization chamber for discharging a first substream enriched with salt crystals, and a second pump fluidically connected to the crystallization chamber for discharging a second substream depleted of salt crystals.
  • the two pumps are in each case connected in terms of flow with a separating unit.
  • the solids content can be controlled in the crystallizer and its Abscheidekapaztician be adapted to the required power based on the ratio of inlet concentration to volume flow.
  • a second pump is installed in addition to one of the crystallization chamber fluidly connected first pump, the first partial flow.
  • This second pump is adjustable and leads to a largely solids-depleted, almost particle-free mother liquor to a second separating unit.
  • an enriched first partial flow can be discharged by means of the first pump, which fulfills the requirements for a centrifugable suspension both in terms of particle size and in terms of the solids content contained for the subsequent separation of the solid from the washing medium in the first separating unit.
  • a depleted partial flow can be discharged by means of the second pump, via which a solid fraction of small salt crystals possibly remaining in the washing medium is discharged. These are then separated from the washing medium in the second separating unit and returned to the crystallizer.
  • such a separation unit can be used effectively for producing a centrifugable suspension, and in particular a centrifugable potassium sulfate suspension, from a sulfate-laden washing medium.
  • the solids-rich suspension, ie the first partial stream, and the almost particle-free suspension, ie the second partial stream, are expediently removed at mutually different points of the crystallizer.
  • the desired accumulation of the particles can be achieved.
  • the amount of solids present in the crystallizer which can be achieved by the targeted control of the partial flows, a desired adaptation of the available crystal surface to the process requirements is possible. Due to particle growth in the crystallizer and the associated increase in Enrichment of particles and the available crystal surface decreases the required volume of the crystallizer. The particles in this case have a much higher residence time and thus growth time within the crystallizer than the liquid flowing through, resulting in large and easily separable crystals.
  • the specification of the volumetric flow ratio of both pumps allows the control of the withdrawal from the crystallizer and thereby control of the accumulation of solids in the crystallizer.
  • the separation unit can be integrated, for example, in a common carbon dioxide deposition apparatus.
  • a separation device usually comprises an absorption unit and a desorption unit fluidically connected to the absorption unit.
  • the separation unit can in this case be connected, for example, in the return line of the desorption unit, wherein the return line connects the desorption unit with the separation unit and this in turn with the absorption unit. In this way, the separation unit is directly in the circulating circuit of the
  • Wash medium between absorption unit and desorption unit switched. It is also possible to remove the washing medium from a separation device, to be transported separately to the separation unit and to reuse it after the separation of the salts in the separation device.
  • the crystallizer is preferably a crystallizer for continuous crystallization, that is, for continuous operation.
  • the crystallizer may comprise, for example, an agitator or a circulation pump and a device for heating and / or cooling.
  • the essential task of the agitator is to keep the particles dependent on size in the balance.
  • the circulation pump is used in combination with a heat exchanger to cool the washing medium to the desired process temperature.
  • a temperature in a range between 5 ° C and 20 ° C is advantageous.
  • the crystallizer comprises a crystallization chamber and a classifier.
  • the crystallization chamber in which the salt crystals are formed, consists of a substantially cylindrical container in which the washing medium and the growing salt crystals are located.
  • the classifier the separation of the salt crystals formed according to their particle size.
  • the large salt crystals are largely separated from the middle and small salt crystals.
  • the use of two pumps for extracting different partial streams from the crystallizer allows a targeted separation of small and large particles from each other and thus their targeted removal from the washing medium.
  • the medium and small salt crystals may remain in the crystallization chamber for further growth.
  • the washing medium is cooled prior to introduction into the crystallizer of the separation unit, whereby the crystal formation of the salts is enabled or promoted.
  • the salt crystal growth is essentially due to supersaturation in the crystallizer.
  • the supersaturation can be generated in particular by cooling the washing medium.
  • the particle size of the salt crystals can be controlled in particular via the local and average supersaturation and the distribution and the residence time of the salt crystals in the supersaturated solution.
  • the first separating unit is fluidically connected to the crystallizer and formed to separate the large salt crystals formed by the washing medium.
  • the salt crystals separated by the first separating unit are sent for storage, disposal or recycling.
  • the washing medium which as far as possible contains no salt crystals, can be fed to an absorption unit of a separation device.
  • the second separating unit is also connected fluidically to the crystallizer and serves to separate the small salt crystals from the washing medium.
  • the separated small salt crystals can be fed back to the crystallizer completely or partially to a corresponding
  • Solid concentration in the crystallizer to maintain which has a positive effect on the crystallization efficiency of the crystallizer.
  • the operation of the separation unit with two independent regulators in the form of pumps requires that a low-particle and a particle-rich suspension can be withdrawn at different points of the crystallizer.
  • This can be implemented, for example, by a countercurrent classification, a decanter, a cyclone or a centrifuge.
  • the classifier is designed as a countercurrent classifier.
  • the classifier can be formed, for example, on the bottom side of the crystallization chamber.
  • the salt crystals grow in the crystallization chamber of the crystallizer. These are separated within the classifier according to their size.
  • the classifier is flowed through by a countercurrent, which is introduced counter to the feed direction of the washing medium into the crystallization chamber of the crystallizer.
  • the rate of descent of the large salt crystals is greater than the rate of descent of the middle and small
  • Salt crystals The salt crystals, whose rate of descent is less than the speed of the countercurrent, are transported with the countercurrent in the upper part of the crystallizer. Salt crystals with a higher rate of descent accumulate at the bottom of the crystallizer or the classifier.
  • the speed of the countercurrent is set so that it is smaller than the rate of descent of the large salt crystals, but greater than the rate of descent of the medium and small salt crystals.
  • a differently configured separation unit such as a hydrocyclone may be used to achieve the separation of the salt crystals from the mother liquor.
  • separation unit is to be understood as meaning, in particular, those units which make it possible to separate the salt crystals according to their particle size.
  • separation of the particles takes place according to their particle size in a multi-stage process.
  • either the same or different separation units can be used and combined with each other.
  • a hydrocyclone can be used in a subsequent second and third separation stage.
  • a decanter can be used in a second separation stage and a hydrocyclone in a third separation stage.
  • a counterflow classifier and / or a decanter and / or a cyclone and / or a centrifuge can be used as the respective separation unit.
  • the individual separation stages are then in particular part of a combined separation unit.
  • the separation units used are expediently coupled to each other in terms of flow.
  • the first pump for discharging the enriched partial flow is arranged at the bottom of the crystallizer.
  • the large-particle suspension enriched at the bottom of the crystallizer can thus be withdrawn directly at this point and fed to a separating unit for solid-liquid separation.
  • the first separating unit preferably comprises a centrifuge.
  • a centrifuge such as a sieve centrifuge, in particular separates the large salt particles from the wash medium. Due to the use of two pumps for the separate discharge of a particle-enriched and a particle-depleted partial flow, the requirements for a centrifugable suspension, both in terms of the particle size as well as the content of solids contained, are met.
  • the first separating unit comprises, in addition to the centrifuge, a filter element which separates any small salt crystals still contained from the washing medium.
  • the first separating unit is followed by a processing device downstream of a processing device.
  • the solid obtained from the suspension ie the potassium sulfate
  • the solid obtained from the suspension ie the potassium sulfate
  • the second pump for discharging the depleted partial flow is arranged at the head of the crystallizer. Since light salt crystals are carried upwards when classifying the particles, a partial stream can be withdrawn at the upper part of the crystallizer which contains no or only a small amount of ultrafine particles. Thus, the second pump removes a thin suspension of washing medium with fine particles from the crystallizer which has been largely depleted of solids.
  • the second separating unit comprises a second hydrocyclone.
  • a hydrocyclone is a centrifugal separator for wellssiggemi- see. With a hydrocyclone solid particles contained in suspensions can be separated or classified. The discharged from the crystallizer, depleted second partial stream contains a small proportion of solids, which can be further reduced. For this purpose, the partial flow can be passed through a hydrocyclone.
  • the use of a second hydrocyclone is advantageous here, since it consists of a container without moving parts and has a small volume due to the short residence time of the partial flow.
  • the use of other separation units, such as an edge gap filter, a decanter or a centrifuge for the separation of any remaining in the second depleted partial flow solids content is possible.
  • the second separating unit for returning salt crystals separated from the washing medium is connected via a return line to the crystallization chamber of the crystallizer.
  • the second separating unit returns the crystals remaining in the aspirated suspension to the crystallizer, which are available there as nucleation nuclei.
  • a first hydrocyclone is fluidically interposed between the crystallizer and the second separating unit.
  • the first hydrocyclone is here in particular formed as a separation unit as part of a separation stage in a multi-stage separation process.
  • the crystallizer and the second separating unit may additionally or alternatively be interposed, for example, a decanter and / or a centrifuge, which are preferably coupled to one another in terms of flow technology.
  • the first hydrocyclone is preferably a larger hydrocyclone than the second hydrocyclone connected downstream of the first hydrocyclone in the second separating unit.
  • the second separator unit for separating smaller crystals and the intermediate hydrocyclone for separating large to medium crystals is provided.
  • the second separating unit is preferably a hydrocyclone, to which a first hydrocyclone is fluidically interposed.
  • the first hydrocyclone is a larger hydrocyclone than the one provided in the second separating unit, the first hydrocyclone downstream hydrocyclone.
  • the first hydrocyclone is an annular arrangement of a plurality of parallelized small hydrocyclones
  • the classifying zone of the crystallizer can be reduced or even dispensed with the classifying zone in the crystallizer.
  • the crystallizer can therefore be carried out as a simple stirred container.
  • the two-stage hydrocyclones used are small, inexpensive apparatuses. They are combined with a simple stirred tank.
  • the wall of the crystallizer becomes available for heat removal due to the absence of the classifying zone.
  • This combination is characterized by a high degree of flexibility, because hydrocyclones can be adapted to changed operating conditions with very little effort, in particular in the case of a numbering-up, by connecting or disconnecting individual apparatuses.
  • the crystallizer no longer needs to be designed in a conservative manner to meet all conceivable operating conditions.
  • the investment cost of the crystallizer can be more than halved in large volumes.
  • the two-stage hydrocyclone has a small footprint.
  • the classifying device for separating the salt crystals is formed according to its particle size in the form of a classifying zone within the crystallizer. It is therefore an internal classification zone, which is expediently provided in the edge region of the crystallizer.
  • the classifying zone is preferably formed as a concentric annular gap, which is formed for separating the classifying zone, in particular by a partition wall drawn into the crystallizer on its inner circumference.
  • At least one baffle is preferably used in the classifying zone.
  • the or each baffle is integrated in the classifying zone designed as a concentric annular gap.
  • the second depleted partial flow is withdrawn at several points within the concentric annular gap.
  • the removal of the second depleted partial flow from the annular gap is preferably carried out via an annular intake pipe with a plurality of uniformly distributed openings formed on the circumference of the intake pipe.
  • the cross-section of the intake openings is preferably much smaller than the inner diameter of the annular intake pipe. In this case, the pressure loss at the holes dominates over the
  • Pressure loss in the intake manifold is at all Openings of the intake pipe equal, so that adjusts the same volume flow at all openings.
  • the feed stream fed to the crystallizer must be cooled accordingly.
  • the crystallization energy and the energy introduced by the stirring and the circulation pump must be dissipated. Since the outer wall surface of the crystallizer is small in comparison to the internal volume, in particular on an industrial scale, external wall cooling for tempering the crystallizer is not sufficient.
  • a combined cooling is used for temperature control of the crystallizer.
  • a separating wall drawn in to separate the classifying zone in the crystallizer can be provided with a cooling structure, for example a pipe coil.
  • the temperature control can be enhanced by an external cooler, which is preferably integrated into the circulation, that is, into the return line coming from the second separation unit and connected to the crystallizer.
  • the second object of the invention is achieved by a process for the separation of salts from a
  • washing medium in which the washing medium is fed to a crystallizer of a separation unit, in a crystallization chamber of the crystallizer salt crystals are formed in the washing medium, and the salt crystals formed in the crystallization chamber are separated by a classifier according to their particle size, with a salt crystal
  • An enriched first partial stream is supplied by means of a first pump to a first separating unit, and wherein a depleted of salt crystals second partial stream is fed via a second pump to a second separating unit.
  • a partial flow can be discharged by means of the first pump, which meets the requirements of the suspension both in terms of particle size and in terms of the solids content contained for subsequent separation in a centrifuge.
  • the second pump serves to extract a depleted partial flow, via which the solids content is discharged with small salt crystals.
  • the salt crystals are preferably separated by means of a countercurrent according to their particle size, so that a low-particle and a particle-rich suspension at various points of the crystallizer can be removed.
  • the enriched with salt crystals first partial stream at the bottom of the crystallizer is discharged from this.
  • the derived partial flow is then fed in particular to a separating unit for solid-liquid separation.
  • the salt particles are essentially separated from the washing medium by means of a rotating drum by utilizing the centrifugal force.
  • the washing medium can subsequently be filtered to remove as much as possible of the salt particles still contained in it.
  • the salt crystals separated from the first substream are ren of the first separating unit supplied to a preparation device.
  • the depleted of salt crystals second partial stream at the head of the crystallizer is discharged from this. Since the classification of the particles, the light salt crystals rise up, so a partial stream can be withdrawn at the top of the crystallizer, which contains a small proportion of fines.
  • the salt crystals contained in the second partial stream are separated from the depleted second partial stream by means of at least one hydrocyclone.
  • the salt crystals contained in the second partial stream are separated in a hydrocyclone as part of the second separating unit.
  • the depleted second partial stream of the second separating unit is additionally or alternatively fed to a hydrocyclone enclosed by the second separating unit.
  • a hydrocyclone enclosed by the second separating unit.
  • a portion of remaining in the second partial flow small salt crystals can be separated from the washing medium before the second separating unit.
  • the already small proportion of solids in the partial stream removed from the crystallizer can be further reduced.
  • the preferred second partial stream depleted of salt crystals already passes a hydrocyclone before it enters the second separating unit, whereby a separation of very fine particles is achieved even before entry into the second separating unit.
  • salt crystals separated from the washing medium are returned to the crystallization chamber of the crystallizer in the second separating unit, which salt crystals are then available there as nuclei of crystallization.
  • the salt crystals within the crystallizer in a classifying zone of the classifier are separated according to their particle size.
  • the classifying zone of the classifier is thus integrated into the crystallizer and expediently provided in the edge region of the crystallizer.
  • the salt crystals are separated according to their particle size in a classifying zone formed as a concentric annular gap.
  • a combined cooling is preferably used for the temperature control of the crystallizer.
  • This combined cooling comprises, in particular, outer wall cooling, inner cooling, for example in the form of a cooling structure attached to a dividing wall of the classifying zone, and external cooling, which is preferably introduced in the form of a cooler integrated into the circulation.
  • 1 shows a separation unit with a crystallizer and with two controllable pumps for withdrawing various partial streams.
  • 1 shows a separation unit 1 for separating salts from a washing medium.
  • the separation unit 1 comprises for this purpose a crystallizer 3 with a crystallization chamber 5 for the formation of salts in the washing medium, as well as a Classifying device 7 for separating the salt crystals according to their particle size.
  • the crystallization chamber 5 of the crystallizer 3 is supplied with a washing medium regenerated from a desorption unit (not shown).
  • the washing medium an amino acid salt solution
  • the washing medium must be cleaned accordingly, since in the washing medium in addition to carbon dioxide acid gases, in particular nitrogen oxides and / or sulfur oxides, are absorbed and form with the washing medium, among other temperature stable salts, such as potassium sulfate (K 2 S0 4 ).
  • K 2 S0 4 potassium sulfate
  • the classifying device 7 of the crystallizer 3 is designed in the form of a classifying zone 9 in its edge region 11.
  • the classifying zone 9 is designed to separate the particles as a concentric annular gap 15, which is formed to separate the classifying zone 9, in particular by a dividing wall 19 drawn into the crystallizer 3 on its inner circumference 17.
  • baffles 21 are used in the classifying zone.
  • the baffles 21 are integrated in the concentric annular gap 15.
  • the classifier 3 uses the principle of countercurrent classification.
  • the crystallization chamber 5 is flowed through by an upward flow.
  • the salt crystals whose sinking rate is low ger than the speed of the countercurrent are transported with the countercurrent in the upper part of the crystallizer 3. Large salt crystals with higher sinking rate accumulate at the bottom of the crystallizer 3.
  • the crystallizer 3 for this purpose two pumps 27, 29 connected fluidically.
  • the first pump 27 serves for the withdrawal of a first partial stream 31 enriched with salt crystals and for this purpose is arranged on the bottom 33 of the crystallizer 3.
  • the first partial flow 31 is fed to a first separating unit 35.
  • the first comprises
  • Separator unit 35 is a centrifuge 37. After centrifuging in the first separating unit 35, the potassium sulphate thus obtained is fed to one of the first separating unit 35, downstream of the downstream processing device 39. In this processing device 39, the solid obtained from the suspension, ie the potassium sulfate, can be further processed and finally used for storage or further use, for example as a fertilizer.
  • the washing medium is returned via a return line 40 back into the crystallizer 3
  • the second pump 29 By means of the second pump 29, the second partial stream 41, which is balanced by salt crystals, is discharged from the crystallizer 3 or the classifying zone 9 of the crystalliser 3.
  • the second pump 29 is arranged on the head 43 of the crystallizer 3 for this purpose.
  • the second depleted partial flow 41 is withdrawn at several points within the concentric annular gap 15.
  • the removal of the second, reduced partial flow 41 from the annular gap 15 preferably takes place via an annular intake pipe 45, with several formed on the circumference of the intake pipe 45 equally distributed openings.
  • the separation of the particles according to their size takes place here in three separation stages 47, 49, 51.
  • the first separation stage 47 here represents the separation within the classifying zone 9 in the crystallizer 3.
  • the particles are separated for the first time according to their size.
  • the depleted second substream 41 then becomes the second
  • Separating stage 49 is supplied, which comprises one of the second pump 29 fluidly downstream first hydrocyclone 53.
  • this hydrocyclone 53 a further portion of the particles contained in the washing medium is removed from the second substream 41 already depleted in the first separation stage 47.
  • the particles are fed back to the crystallizer 3 via a return line 55.
  • the second substream 41 which is further depleted compared to its outlet from the crystallizer 3, is supplied from the second separation stage 49, by means of a further pump 57, to the third separation stage 51 via a feed line 59.
  • the third separation stage 51 also includes a second hydrocyclone 61 for separating any fine particles still contained in the partial flow 41.
  • the third separation stage 51 is part of the second separation unit 63.
  • the first hydrocyclone 53 is configured as a larger hydrocyclone or an annular arrangement of a plurality of parallelized small hydrocyclones (numbering-up), which separates the large and medium crystals 3. These are again fed to the crystallizer 3, while the remaining thin stream of the second separating unit 63, preferably designed as a smaller hydrocyclone 61, is fed. There, the separation of the small particles, which are returned as Impfgut in the inner region of the crystallizer 3, where they act as growth nuclei.
  • the classifying zone 9 of the crystallizer 3 can be reduced or even dispensed with the classifying zone 9 in the crystallizer 3.
  • the crystallizer 3 could be carried out as a simple stirred container.
  • the two-stage hydrocyclones 53, 61 used are small, inexpensive apparatuses. They are combined with a simple stirred tank.
  • the wall of the crystallizer 3 is usable due to the reduction / absence of the classifying zone 9 for heat dissipation. This combination is characterized by a high degree of flexibility, because hydrocyclones, in particular in the case of a numbering-up, can be adapted to changing operating conditions by connecting or disconnecting individual apparatuses with very little effort.
  • the crystallizer 3 no longer needs to be designed to be particularly conservative, in order to meet all conceivable operating conditions.
  • the particles deposited in the third separation stage 49 are introduced into the second from the second via a return line 65
  • the feed stream fed to the crystallizer 3, ie the regenerated washing medium must be cooled accordingly.
  • the solubility of the salts in the regenerated washing medium decreases and the salts to be crystallized out are brought to supersaturation.
  • the crystal growth of the salts in the crystallization chamber 5 of the crystallizer 3 is made possible.
  • the energy of crystallization and the energy introduced by the stirrer and the pumps 29, 57 must be dissipated.
  • a combined cooling in which the separating wall 19 drawn in to separate the classifying zone 9 in the crystalliser 3 is provided with a cooling structure 67 designed as a tube coil.
  • a cooler 73 is integrated in circulation 69, that is to say in a recirculation line 71 coming from second separation stage 47, connected to crystallizer 3.
  • the cooler 73 cools in particular a feed stream taken from the feed line 59 between the second separating stage 49 and the third separating stage 51 via a branch line 75 to the desired process temperature in the crystallizer 3.
  • the regenerated washing medium which is substantially freed from salts, can finally be fed to an absorption unit of a separation device.

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  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

L'invention concerne une unité de séparation (1) pour séparer des sels d'une substance détergente, ladite unité de séparation comprenant un cristalliseur (3) présentant une chambre de cristallisation (5) pour former des cristaux de sel et un dispositif de triage (7) pour séparer les cristaux de sel en fonction de leur granulométrie, ainsi qu'une première pompe (27) raccordée fluidiquement au cristalliseur (3) et servant à évacuer un premier flux partiel (31) enrichi en cristaux de sel, de même qu'une deuxième pompe (29) raccordée fluidiquement au cristalliseur (3) et servant à évacuer un deuxième flux partiel (41) appauvri en cristaux de sel, la première pompe (27) et la deuxième pompe (29) étant reliées fluidiquement chacune à une unité de séparation (35, 63). L'invention concerne en outre un procédé pour séparer des sels d'une substance détergente.
PCT/EP2014/059622 2013-05-23 2014-05-12 Unité de séparation et procédé pour séparer des sels d'une substance détergente WO2014187690A1 (fr)

Applications Claiming Priority (4)

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DE102013209534.1 2013-05-23
DE102013209534 2013-05-23
DE102013225720.1A DE102013225720A1 (de) 2013-05-23 2013-12-12 Abtrenneinheit sowie Verfahren zur Abtrennung von Salzen aus einem Waschmedium
DE102013225720.1 2013-12-12

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3208834A (en) * 1960-01-26 1965-09-28 Hertha M Schulze Method and apparatus for crystallizing and classifying
GB1029132A (en) * 1962-05-29 1966-05-11 Power Gas Ltd Improvements in the production of crystals from solutions
US3616835A (en) * 1968-02-20 1971-11-02 Cocei Sa Evaporators having hollow platelike vertical heat transfer elements and overhead nozzles
EP0299597A2 (fr) * 1987-04-28 1989-01-18 Suntory Limited Procédé et appareil pour l'élimination des tartrates ou d'impuretés similaires

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3208834A (en) * 1960-01-26 1965-09-28 Hertha M Schulze Method and apparatus for crystallizing and classifying
GB1029132A (en) * 1962-05-29 1966-05-11 Power Gas Ltd Improvements in the production of crystals from solutions
US3616835A (en) * 1968-02-20 1971-11-02 Cocei Sa Evaporators having hollow platelike vertical heat transfer elements and overhead nozzles
EP0299597A2 (fr) * 1987-04-28 1989-01-18 Suntory Limited Procédé et appareil pour l'élimination des tartrates ou d'impuretés similaires

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