DE1298969B - Application of a process to obtain coarsely crystalline salts from a solution in several stages with constant classification - Google Patents

Application of a process to obtain coarsely crystalline salts from a solution in several stages with constant classification

Info

Publication number
DE1298969B
DE1298969B DEW43674A DEW0043674A DE1298969B DE 1298969 B DE1298969 B DE 1298969B DE W43674 A DEW43674 A DE W43674A DE W0043674 A DEW0043674 A DE W0043674A DE 1298969 B DE1298969 B DE 1298969B
Authority
DE
Germany
Prior art keywords
solution
stage
crystallizer
discharged
double cone
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.)
Pending
Application number
DEW43674A
Other languages
German (de)
Inventor
Domning
Dipl-Ing Hans
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.)
Wintershall AG
Original Assignee
Wintershall AG
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 Wintershall AG filed Critical Wintershall AG
Priority to DEW43674A priority Critical patent/DE1298969B/en
Priority to NL6802832A priority patent/NL135394C/xx
Priority to US709477A priority patent/US3530924A/en
Priority to ES351087A priority patent/ES351087A1/en
Priority to DK85268A priority patent/DK128368B/en
Priority to GB00185/68A priority patent/GB1224671A/en
Priority to IL29557A priority patent/IL29557A/en
Priority to JP1320668A priority patent/JPS535272B1/ja
Priority to FR1580875D priority patent/FR1580875A/fr
Priority to SE08397/72A priority patent/SE366660B/xx
Priority to OA53234A priority patent/OA02784A/en
Publication of DE1298969B publication Critical patent/DE1298969B/en
Priority to DK489871AA priority patent/DK135098B/en
Priority to NL7113886.A priority patent/NL159287B/en
Pending legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
    • C05D1/00—Fertilisers containing potassium
    • C05D1/005—Fertilisers containing potassium post-treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/0018—Evaporation of components of the mixture to be separated
    • B01D9/0022—Evaporation of components of the mixture to be separated by reducing pressure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/0036—Crystallisation on to a bed of product crystals; Seeding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/004—Fractional crystallisation; Fractionating or rectifying columns
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00—Ammonia; Compounds thereof
    • C01C1/24—Sulfates of ammonium
    • C01C1/248—Preventing coalescing or controlling form or size of the crystals
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D3/00—Halides of sodium, potassium or alkali metals in general
    • C01D3/22—Preparation in the form of granules, pieces, or other shaped products

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Description

Zum nicht vorveröffentlichten Stand der Technik gehört ein Verfahren und eine Vorrichtung zur Gewinnung grobkristalliner Salze durch Vakuumkühlung aus einer Lösung in mehreren Stufen unter ständiger Klassierung, derart, daß die in jeder Stufe klassierten und ausgetragenen Salzkristalle in die vorhergehende wärmere Stufe geführt und aus der ersten Stufe, in welche die heiße Lösung eingeführt wird, ausgetragen werden, wobei die heißgesättigte Lösung tangential am größten Durchmesser eines den Fuß eines Kristallisators bildenden Doppelkonus eingeleitet, von da in den unteren Teil des darüberliegenden konischen Kristallisierraumes geführt, mit der im Kristallisator befindlichen, bereits abgekühlten Lösung, in welche auch die aus der nächst kälteren Stufe ausgetragenen Salzkristalle mit Transportlösung aus dem heißeren Kristallisator eingeführt werden, vermischt, an die Oberfläche geführt, abgekühlt, die Salzkristalle, deren Sinkgeschwindigkeit größer als die Anströmgeschwindigkeit in der Sichterstrecke ist, in dem Doppelkonus von Transportlösung erfaßt und mittels Pumpe der nächst heißeren Stufe zugeführt und in der heißesten Stufe abgezogen werden, und die gekühlte, feststoffreie Lösung aus dem Kristallisator über ein Überlaufrohr zur nächst kälteren Stufe abgeführt wird, wobei a) die Lösung nach dem Eintritt in den Doppelkonus in kreisender Bewegung in einer in den Doppelkonus hineinragenden Sichterstrecke hochgeführt wird, b) die Mischung der Lösungen durch Ansaugöffnungen in den Förderstrom der Umwälzorgane eingesaugt wird, c) in dem Knstallisierraum eine Feststoffkonzentration in dem Bereich von etwa 5 bis etwa 40 Gewichtsprozent durch Einstellung einer bestimmten Anströmgeschwindigkeit in der Sichterstrecke aufgebaut wird. The state of the art, which has not been previously published, includes a method and a device for obtaining coarsely crystalline salts by vacuum cooling a solution in several stages with constant classification, such that the in of each stage classified and discharged salt crystals into the previous warmer one Stage and from the first stage, into which the hot solution is introduced, be discharged, the hot saturated solution tangentially at the largest diameter initiated a double cone forming the base of a crystallizer, from there in the lower part of the conical crystallization room above, with the already cooled solution in the crystallizer, in which the Salt crystals discharged from the next colder stage with transport solution introduced into the hotter crystallizer, mixed, brought to the surface, cooled down, the salt crystals, whose sinking speed is greater than the inflow speed in the sifter line is captured in the double cone of transport solution and by means of Pump to the next hotter stage and withdrawn in the hottest stage, and the cooled, solids-free solution from the crystallizer via an overflow pipe is discharged to the next colder stage, with a) the solution after entry in the double cone in a circular motion in a protruding into the double cone Sifter line is raised, b) the mixture of the solutions through suction openings is sucked into the flow of the circulating elements, c) in the Knstallisierraum a solids concentration in the range of about 5 to about 40 percent by weight by setting a certain flow velocity in the classifier section is being built.

Dieses Klistallisationsverfahren versagt aber bei solchen Salzen, deren Löslichkeit weitgehend von der Temperatur abhängig ist, wie Natriumchlorid. Diese können nur dann zur Kristallisation kommen, wenn die Lösung eingeengt, d. h. das Lösungsmittel ganz oder teilweise durch Verdampfung entzogen wird. However, this clistallization process fails with such salts whose solubility is largely dependent on temperature, like sodium chloride. These can only crystallize if the solution is concentrated, i. H. the solvent is completely or partially removed by evaporation.

Es wurde nun die Anwendung des Verfahrens der eingangs bezeichneten Art zur Verdampfungskristallisation in mehreren Stufen gefunden, wobei eine Lösungsmenge, welche etwa der stündlichen Durchsatzmenge entspricht, aus dem Ringraum zwischen der Kristallisatorwand und der Tauchglocke entnommen, mit einer Pumpe 13 über einen Wärmeaustauscher 14 geleitet und an den Stellen 15 am unteren Teil des sich hosenförmig gabelnden zentralen Leitrohres (3) wieder eingeführt wird, wobei der Wärmeaustauscher der ersten Stufe mit Frischdampf, die Wärmeaustauscher der folgenden Stufe je mit dem Brüden der jeweils vorausgehenden Stufe beheizt werden. It was now the application of the method described at the outset Type of evaporative crystallization found in several stages, with a quantity of solution, which corresponds approximately to the hourly throughput, from the annular space between taken from the crystallizer wall and the immersion bell, with a pump 13 via a Heat exchanger 14 passed and at the points 15 on the lower part of the trousers-shaped bifurcating central guide tube (3) is reinserted, the heat exchanger the first stage with live steam, the heat exchangers of the following stage each with to the Vapors from the previous stage are heated.

Claims (1)

Patentanspruch: Anwendung eines Verfahrens zur Gewinnung grobkristalliner Salze aus einer Lösung in mehreren Stufen unter ständiger Klassierung derart, daß die in jeder Stufe klassierten und ausgetragenen Salzkristalle in die vorhergehende wärmere Stufe geführt und aus der ersten Stufe, in welche die heiße Lösung eingeführt wird, ausgetragen werden, wobei die heißgesättigte Lösung tangential am größten Durchmesser eines den Fuß eines Kristallisators bildenden Doppelkonus eingeleitet, von da in den unteren Teil des darüberliegenden konischen Kristallisierraumes geführt, mit der im Kristallisator befindlichen, bereits abgekühlten Lösung, in welche auch die aus der nächst kälteren Stufe ausgetragenen Salzkristalle mit Transportlösung aus dem Kristallisator eingeführt werden, vermischt, an die Oberfläche geführt, abgekühlt, die Salzkristalle, deren Sinkgeschwindigkeit größer als die Anströmgeschwindigkeit in der Sichterstrecke ist, in dem Doppelkonus von Transportlösung erfaßt und mittels Pumpe der nächst heißeren Stufe zugeführt und in der heißesten Stufe abgezogen werden, und die gekühlte, feststofffreie Lösung aus dem Kristallisator über ein Überlaufrohr zur nächst kälteren Stufe abgeführt wird, wobei a) die Lösung nach dem Eintritt in den Doppelkonus in kreisender Bewegung in einer in den Doppelkonus hineinragenden Sichterstrecke hochgeführt wird, b) die Mischung der Lösungen durch Ansaugöffnungen in den Förderstrom der Umwälzorgane eingesaugt wird, c) in dem Kristallisierraum eine Feststoffkonzentration in dem Bereich von etwa 5 bis etwa 40 Gewichtsprozent durch Einstellung einer bestimmten Anströmgeschwindigkeit in der Sichterstrecke aufgebaut wird, zur Verdampfungskristallisation in mehreren Stufen, wobei eine Lösungsmenge, welche etwa der stündlichen Durchsatzmenge entspricht, aus dem Ringraum zwischen der Kristallisatorwand und der Tauchglocke entnommen, mit einer Pumpe (13) über einen Wärmeaustauscher (14) geleitet und an den Stellen (15) am unteren Teil des sich hosenförmig gabelnden zentralen Leitrohres (3) wieder eingeführt wird, wobei der Wärmeaustauscher der ersten Stufe mit Frischdampf, die Wärmeaustauscher der folgenden Stufen je mit dem Brüden der jeweils vorausgehenden Stufe beheizt werden. Claim: Use of a process for obtaining coarsely crystalline Salts from a solution in several stages with constant classification in such a way that the salt crystals classified and discharged in each stage into the previous one warmer stage and from the first stage, in which the hot solution is introduced is discharged, with the hot saturated solution tangentially greatest Introduced the diameter of a double cone forming the base of a crystallizer, from there into the lower part of the conical crystallization room above, with the already cooled solution in the crystallizer, in which also the salt crystals discharged from the next colder stage with transport solution are introduced from the crystallizer, mixed, carried to the surface, cooled down, the salt crystals, whose sinking speed is greater than the inflow speed in the sifter line is captured in the double cone of transport solution and by means of Pump to the next hotter stage and withdrawn in the hottest stage, and the cooled, solids-free solution from the crystallizer via an overflow pipe is discharged to the next colder stage, with a) the solution after entry in the double cone in a circular motion in a protruding into the double cone Sifter line is raised, b) the mixture of the solutions through suction openings is sucked into the conveying flow of the circulating elements, c) in the crystallization space a solids concentration in the range of about 5 to about 40 percent by weight by setting a certain flow velocity in the classifier section is built up, for evaporative crystallization in several stages, whereby a quantity of solution, which corresponds approximately to the hourly throughput, from the annular space between taken from the crystallizer wall and the immersion bell, with a pump (13) over a heat exchanger (14) passed and at the points (15) at the lower part of the central guide tube (3) bifurcating in the shape of a trouser is inserted again, wherein the heat exchanger of the first stage with live steam, the heat exchangers of the The following stages can be heated with the vapor from the previous stage.
DEW43674A 1967-03-03 1967-04-01 Application of a process to obtain coarsely crystalline salts from a solution in several stages with constant classification Pending DE1298969B (en)

Priority Applications (13)

Application Number Priority Date Filing Date Title
DEW43674A DE1298969B (en) 1967-04-01 1967-04-01 Application of a process to obtain coarsely crystalline salts from a solution in several stages with constant classification
NL6802832A NL135394C (en) 1967-03-03 1968-02-28
US709477A US3530924A (en) 1967-03-03 1968-02-29 Crystallization method and device
ES351087A ES351087A1 (en) 1967-03-03 1968-02-29 Crystallization method and device
DK85268A DK128368B (en) 1967-03-03 1968-03-01 Method and apparatus for extracting and drying coarse-grained salts.
GB00185/68A GB1224671A (en) 1967-03-03 1968-03-01 Process and apparatus for the production of coarse grained salts
IL29557A IL29557A (en) 1967-03-03 1968-03-01 Process and arrangement for the production and drying of coarse salts by means of multi-step counter current crystallization
JP1320668A JPS535272B1 (en) 1967-03-03 1968-03-02
FR1580875D FR1580875A (en) 1967-03-03 1968-03-04
SE08397/72A SE366660B (en) 1967-04-01 1968-03-04
OA53234A OA02784A (en) 1967-04-01 1968-03-29 Process and device for obtaining and drying coarse-grained salts by counter-current crystallization in several stages.
DK489871AA DK135098B (en) 1967-04-01 1971-10-07 Process for the recovery and drying of coarse-grained salts by evaporative crystallization of a solution in several steps while still classifying.
NL7113886.A NL159287B (en) 1967-03-03 1971-10-08 METHOD FOR THE WINNING OF COARSE GRAINY SALT BY VACUUM EVAPORATION.

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DEW43674A DE1298969B (en) 1967-04-01 1967-04-01 Application of a process to obtain coarsely crystalline salts from a solution in several stages with constant classification

Publications (1)

Publication Number Publication Date
DE1298969B true DE1298969B (en) 1969-07-10

Family

ID=7603752

Family Applications (1)

Application Number Title Priority Date Filing Date
DEW43674A Pending DE1298969B (en) 1967-03-03 1967-04-01 Application of a process to obtain coarsely crystalline salts from a solution in several stages with constant classification

Country Status (1)

Country Link
DE (1) DE1298969B (en)

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3071447A (en) * 1958-09-09 1963-01-01 Whiting Corp Hydraulic classifier

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3071447A (en) * 1958-09-09 1963-01-01 Whiting Corp Hydraulic classifier

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Legal Events

Date Code Title Description
E77 Valid patent as to the heymanns-index 1977
8320 Willingness to grant licences declared (paragraph 23)