WO2009095357A1 - Procédé et dispositif pour la fabrication en continu d’un produit cristallin à gros grains à base de sulfate d’ammonium - Google Patents

Procédé et dispositif pour la fabrication en continu d’un produit cristallin à gros grains à base de sulfate d’ammonium Download PDF

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Publication number
WO2009095357A1
WO2009095357A1 PCT/EP2009/050798 EP2009050798W WO2009095357A1 WO 2009095357 A1 WO2009095357 A1 WO 2009095357A1 EP 2009050798 W EP2009050798 W EP 2009050798W WO 2009095357 A1 WO2009095357 A1 WO 2009095357A1
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WO
WIPO (PCT)
Prior art keywords
solution
crystallizer
sulfuric acid
ammonia
line
Prior art date
Application number
PCT/EP2009/050798
Other languages
German (de)
English (en)
Inventor
Jan A.M.V. Van Esch
Reinhard Scholz
Original Assignee
Gea Messo Gmbh
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 Gea Messo Gmbh filed Critical Gea Messo Gmbh
Publication of WO2009095357A1 publication Critical patent/WO2009095357A1/fr

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Classifications

    • 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
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency
    • Y02P20/129—Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines

Definitions

  • the invention relates to a process for the continuous production of a coarse-grained crystalline ammonium sulfate product according to the preamble of patent claim 1 and to a plant for carrying out this process.
  • Ammonium sulfate (NH 4 ) 2 SO 4 ) is a large scale product used mainly as a fertilizer in agriculture to supply nitrogen and sulfur. In industrial terms, ammonium sulfate is by-produced in some chemical processes, particularly in the production of caprolactam. To meet the requirements as a fertilizer, that must
  • Ammonium sulfate as coarse-grained product (grain size d '(RRSB) in the range of 1 to 4 mm) are available. This is important in order to ensure a good throwing power and, in the case of mixing with other fertilizers, to suppress the tendency for segregation, which would be intensified by fines in a grain mixture.
  • coarse-grained crystallizates can be prepared from solutions in crystallizers of the type DTB (Draft Tube Baffled) or of the Oslo type.
  • DTB Double Tube Baffled
  • the problem arises that the average grain size of the product crystals produced in the crystallizer is subject to periodic fluctuations, i.
  • Phases with a high coarse grain fraction alternate with phases in which predominantly fine-grained crystals (for example, grain size less than 1 mm) are obtained. This is the result of a strong spontaneous primary nucleation with increased supersaturation in the crystallizer.
  • all nuclei formed are dissolved by the strong fine crystal dissolution due to the temperature increase in the heat exchanger of the external circuit of a DTB crystallizer or in the circulation of an Oslo crystallizer.
  • the external circuit before the heat exchanger and the feed line opens can be fed by the new concentrated ammonium sulfate solution in the crystallizer. From the bottom area, a partial stream of suspension with the proportion of solid contained in the desired particle size of the product crystallizate is continuously withdrawn. The product crystals are separated from the mother liquor in a thickener and then centrifuged, and the mother liquor is returned to the DTB crystallizer.
  • the temperature of the fed suspension must not exceed the operating temperature in the crystallizer.
  • the suspension must be 6 - 24 Vol .-% Contain crystals, wherein at least 35% of the crystals are greater than 1, 2 mm, and the feed of the suspension should be such that the weight of the crystals in the fed suspension in the range of 4-25% of the weight of the crystals in the the suspension withdrawn from the bottom region of the crystallizer with the product crystals.
  • This targeted feeding of crystal suspension in a crystallizer to influence the grain size is also referred to as seeding.
  • WO 00/56416 a method for controlling the grain size in the continuous mass crystallization is known, which is also intended for the production of coarse ammonium sulfate crystals in an Oslo crystallizer or DTB crystallizer and in which similar to the method according to EP 0632738 B1 an inoculation is carried out with externally supplied crystal suspension.
  • the inoculum is a crystallizate, which is manufactured in its parameters independent of the current crystallization process and which has a mean grain diameter of 0.1 - 1, 0 mm.
  • the temperature of the seed product during the addition must not be in this process above the operating temperature in the crystallizer, but must be up to 40 0 C, preferably 10 - 30 0 C, lower.
  • a suspension with a solids content in the desired particle size is continuously withdrawn and separated by centrifugation in product and mother liquor, wherein the mother liquor is conveyed to an intermediate container and fed back from there into the circulation line of the external circuit of the crystallizer.
  • the seed product is preferably added in an amount whose solids content is 5 to 30% by weight of the from the crystallizer respectively discharged solid.
  • the solids content of the seed product can be generated, for example, by mechanically comminuting a portion of the product crystals and / or by a separate crystallization stage.
  • a third discharge line is connected, can be deducted in the case of need, an excess of crystallization nuclei and ultrafine crystals and fed into a collection container.
  • Solvent is added to the receiver to dissolve the solids. From there, the resulting solution is passed into a neutralization tank in which it is treated with sulfuric acid and ammonia and heated by the associated neutralization reaction. The heated solution is then fed to the crystallizer.
  • the object of the present invention is to improve a generic process in such a way that the production of coarse-grained ammonium sulfate with relatively low investment costs and the lowest possible requirement for externally supplied thermal energy and with the lowest possible periodic Schwankun- conditions of medium grain size can be done.
  • a system for carrying out this method should be specified.
  • This object is achieved by a method for the continuous production of a coarse crystalline ammonium sulfate product by crystallization from a supersaturated ammonium sulfate solution in a DTB crystallization stage, - wherein a suspension of supersaturated ammonium sulfate solution and crystals formed in the crystallization stage circulated in an internal circuit becomes,
  • At least the essential part of the sulfuric acid is mixed with at least part of the clarified solution in the external circuit and heated back into the crystallization stage.
  • feedstock is at least predominantly formed by the reaction of sulfuric acid and ammonia
  • a relatively small portion of the feed (less than 25%, more preferably less than 10%) can be fed to the process in a conventional manner as a concentrated ammonium sulfate solution. If the vast majority, ie at least 75%, preferably at least 90%, especially 100% of the feedstock in the form of concentrated sulfuric acid and ammonia is introduced separately into the DTB crystallizer, the released heat of reaction is sufficient to re-dissolution of by increasing the temperature To ensure fine fractions in the circulated in the external circuit of the crystallizer solution.
  • the invention provides for its introduction into the part of the process sequence in which the dissolution of fine crystals and crystallization nuclei is to take place, namely into the external circulation of the solvent recirculation. If in a preferred manner, the ammonia is fed into the external circuit, expediently downstream of the feed of sulfuric acid, then there is also the heat released by the formation of ammonium sulfate for solids dissolution available.
  • the feed of the Reactants in the external circuit has the advantage that it ensures a particularly intense and uniform mixing, since the circulating amount of material of the external circuit is considerably smaller than that of the internal circuit, and the entire heat released is used for solids dissolution, so that a subsaturated Solution is returned from the external circuit in the crystallization stage.
  • the high circulation rate of the inner circuit enables a low supersaturation operation ( ⁇ c less than 3 g / l, preferably less than 1.5 g / l), which is required to form a coarse-grained crystal.
  • the inventive method of feeding the feedstock has the great advantage that an indirect heat exchanger can be omitted both within the external solution circuit and for preheating the feedstock for a sufficient evaporation of solvent. This reduces the equipment costs and also the costs for externally supplied process energy accordingly.
  • the supply of sulfuric acid which is a function of the controlled supply of ammonia, pH controlled, wherein in the crystallization stage always a slight excess of free sulfuric acid is maintained. This ensures that no free ammonia remains in circulation, but is completely converted.
  • the pH is expediently measured in the external circuit.
  • the supply of ammonia which is usually supplied in liquid form, preferably takes place in the gaseous state.
  • the evaporation in the crystallization stage under vacuum; In principle, however, it can also be carried out at atmospheric pressure and even at a slight overpressure of up to 1 bar.
  • the suspension which is tempered by the excess heat of reaction which is not consumed, ie, not used to dissolve the finely crystallized solution, typically has a temperature in the range from 75 to 80 ° C.
  • the solvent evaporates adiabatically as it approaches the liquid level.
  • the vapor withdrawn from the crystallization stage is advantageously cooled indirectly by means of a coolant and the resulting condensate is collected.
  • the heated coolant of the condenser as a heat source for the pressure-controlled evaporation of liquid ammonia for the supply of the gaseous ammonia to be supplied.
  • the withdrawn suspension containing the product crystals is suitably subjected to a thickening still centrifugation and thereby washed with a partial stream of the collected condensate.
  • the suspension is in a freed from adhering mother solution and sulfuric acid, so pure
  • Crystalline and divided into liquid phase.
  • the washed crystals should then be subjected to drying as well as separation of fine crystals to obtain a salable coarse ammonium sulfate product.
  • the separated fine crystals can advantageously be dissolved with mixing with the separated in the thickening, fine solid fractions containing liquid phase and with the discharged from the centrifugation liquid phase and a residual partial flow of condensate and recycled to the crystallization.
  • This recycling can take place directly into the space of the crystallizer filled with suspension, but can advantageously also take place into the external circulation of the suspension or solution.
  • it may be provided to return a certain proportion of condensate directly back into the crystallization, in particular to feed this condensate fraction to increase the dissolving power and thus to support the re-dissolution of solid fractions into the external circuit.
  • the entire condensate is ultimately recycled back into the crystallization, so that apart from inevitable losses no running solvent supply must be made.
  • a waste acid originating from another process, in particular from caprolactam production is used to reduce the production costs as sulfuric acid.
  • Core of the illustrated system is a DTB crystallizer 1, the head is denoted by 4 and the bottom portion with 2.
  • Flow guide 6 is arranged inside the crystallizer 2.
  • the liquid level lies in the system in operation in the region of the upper end of the flow guide tube 6, at the lower end of which a circulating pump 5 for an internal suspension circuit is arranged.
  • the circulation pump 5, whose drive is flanged on the outside of the bottom of the crystallizer 1, is designed so that it introduces as little mechanical energy into the suspension, so it promotes particularly gentle and consequently produces little abrasion and grain breakage in the crystals. In that regard, the formation of fine solids is reduced.
  • a flow guide wall ending below the liquid level and forming an annular, downwardly open chamber is provided, which is decoupled from the internal suspension cycle in the sense of a clarification area 3 as a flow-calmed space.
  • this annular clarification chamber can also be divided by radial partitions into several sub-chambers.
  • a line 7 of an external solution circuit is provided, which is provided with a circulating pump 8 and returns to the bottom area 2 of the crystallizer 1 in the vicinity of the lower end of the flow conduit 6.
  • a sulfuric acid feed 9 and behind this an ammonia feed 10 open into the line 7.
  • the ammonia feed 10 has an ammonia evaporator 1 1 on.
  • a suspension withdrawal line 12 with a suspension pump 13 is connected to the crystallizer 1 in the bottom region 2.
  • the suspension withdrawal line 12 leads to a thickener 25 formed, for example, as a hydrocyclone.
  • a vapor discharge line 14 is connected, which leads to an indirectly cooled condenser 15.
  • the coolant used for cooling the condenser 15 can be supplied to the condenser 15 from a coolant supply line 17 through a wiring harness 17a and can be returned to a coolant outlet 18 via a wiring harness 18a and, for example, advantageously used to heat the ammonia evaporator 11 be (not shown).
  • the condenser 15 is connected via a vacuum line 19 to a vacuum generating system 20, so that the evaporation of the solvent in the crystallizer 1 can take place as a vacuum evaporation.
  • the negative pressure in the vacuum line 19 and thus the negative pressure in the vacuum evaporation can be controlled in a simple manner by means of an air inlet 21 in front of the vacuum generating system 20.
  • the one from the crystallisa- Tor 1 withdrawn vapor can be performed as condensate from the condenser 15 through a condensate discharge line 16 in a condensate collector 22 and collected there for subsequent reuse.
  • a coarse solids / liquid separation can be carried out, wherein the separated liquid phase with finely divided crystals introduced by a dissolution of solution 29 in a dissolving apparatus 37 and the separated solid can be passed through a crystallizate 26 into a centrifuge 27.
  • the centrifuge 27 is provided for cooling the supplied crystals with a condenser 28, which via the two strands of wire 17b and 18b of the coolant supply line 17 and the
  • Coolant discharge 18 can be supplied with coolant.
  • condensate can be introduced by means of a condensate pump 24 via the condensate lines 23 and 23a as a detergent in the centrifuge 27.
  • the solids which can be separated off in the centrifuge 27 can be fed to a dryer 32 for drying via a crystallization line 30, while the liquid phase can be introduced into the dissolving apparatus 37 by a washing liquid discharge line 31.
  • the dry crystallizate coming from the drier 32 may conveniently be fed with a dry material conveyor 33 to a sieve plant 34 in which fine crystals of an ammonium sulfate product 35 having the desired coarser particle size spectrum are separated off. The separated fine fraction can over a
  • Fine crystallization line 36 also as the liquid phases from the thickener 25 and the centrifuge 27 are conveyed into the dissolving apparatus 37. Since a condensate line 23b connected to the condensate line 23 can also be used to introduce condensate into the suitable apparatus 37 equipped with a stirring apparatus, complete dissolution of the supplied solid to a reusable solution can be achieved.
  • This solution can be supplied to a solution tank 39, which is also expediently provided with an agitator, by means of a solution line 38 designed, for example, as an overflow line, and returned from this to the crystallizer 1 by means of a solution pump 40 and a solution return line 41.
  • a condensate line 23c may be provided, through which a part of the resulting condensate from the Condensate line 23 can be fed into the line 7.
  • a DTB crystallizer comprising combining the reactants (NH 4 and H 2 SO 4 ) to form ammonium sulfate in a separate reactor and feeding the resulting warm ammonium sulphate solution into the crystallization space or directing the reactants directly into the crystallization space Crystallization be given, and implement there, the solids dissolution in the external circuit must be done solely by the addition of solvent (condensate). This results in being removed from the bottom of such a DTB crystallizer
  • Suspension is a product crystallizate having a typical particle size D50 in the range of 0.7 - 1, 0 mm.
  • the inventive method provides a crystal size D50 of at least 1, 2 mm (corresponding to a RRSB distribution with d 'in the range 1, 4 - 2.0 mm at n greater than or equal to 2).
  • a DTB crystallizer which is filled with 250 m 3 of ammonium sulfate suspension, an internal circulation takes place with a circulation rate of 10000 m 3 / h.
  • the operating temperature is 75 ° C.
  • the external circuit extracts 700 m 3 / h of clarified solution, which contains only fines as solid, from the crystallizer and after separate feed of 14.5 t / h of concentrated sulfuric acid and 4.9 t / h recycled gaseous ammonia back into the crystallizer, wherein the recycled solution is solids-free and has a temperature of 87 0 C.
  • t / h of vapor are withdrawn at a pressure of 0.7 bar, while in the bottom area, a suspension withdrawal of 90 t / h takes place.
  • This withdrawn suspension is passed into a hydrocyclone in which a first part of the liquid phase is separated in an amount of 42 t / h and then passed into a dissolving tank.
  • the remaining wet Kristallisatmasse is washed in a centrifuge with an amount of about 2 t / h of the condensate obtained from the vapors and largely from the rest of the liquid phase, which is also passed in an amount of 22.5 t / h in the dissolving tank, freed.
  • the crude crystal mixture is subdivided by sieving into a fine crystallizate of 2 t / h and an ammonium sulfate product crystallizate of 19 t / h, the product crystallizate having a particle size D50 of 1.3 mm.
  • the fine crystals are also passed together with about 3 t / h of vapor condensate in the dissolving tank and dissolved again.
  • the residual vapor condensate is fed back as a mass flow of about 13 t / h in the DTB crystallizer, in a preferred embodiment of the invention to support the solids dissolution into the external circuit.
  • the content of the dissolving tank is also recycled as a mass flow of 69.5 t / h in the DTB crystallizer.

Abstract

L’invention concerne un procédé et un dispositif pour fabriquer du sulfate d’ammonium à gros grains, en prévoyant un cristalliseur DTB (1) qui présente une conduite (7) pour un circuit externe de solution. Le sulfate d’ammonium à utiliser est fourni sous la forme d’acide sulfurique (9) et d’ammoniac (10) concentrés, séparément alimentés directement dans la conduite (7). La chaleur de processus nécessaire pour le procédé est tirée de la chaleur dégagée lors de l’introduction de l’acide sulfurique et de la conversion de l’acide sulfurique et de l’ammoniac en sulfate d’ammonium.
PCT/EP2009/050798 2008-02-01 2009-01-23 Procédé et dispositif pour la fabrication en continu d’un produit cristallin à gros grains à base de sulfate d’ammonium WO2009095357A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102008007155.2A DE102008007155B4 (de) 2008-02-01 2008-02-01 Verfahren und Vorrichtung zur kontinuierlichen Herstellung eines grobkörnigen kristallinen Ammoniumsulfat-Produkts
DE102008007155.2 2008-02-01

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WO2009095357A1 true WO2009095357A1 (fr) 2009-08-06

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WO (1) WO2009095357A1 (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101734813B (zh) * 2009-12-21 2012-01-11 山东大明消毒科技有限公司 一种利用氰尿酸生产过程中的废酸液回收硫酸铵的工艺及其使用的设备
CN111498869A (zh) * 2020-04-14 2020-08-07 中石化南京工程有限公司 一种硫酸铵中和结晶方法及其装置
CN111530119A (zh) * 2020-04-14 2020-08-14 中石化南京工程有限公司 一种串联的硫酸铵结晶方法及其装置

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102014101843A1 (de) * 2014-02-13 2015-08-13 Gea Messo Gmbh Verfahren und Anlage zur Erzeugung eines Laktose-Kristallisats
CN111408157B (zh) * 2020-04-14 2021-09-14 中石化南京工程有限公司 一种硫酸铵结晶方法及其装置

Citations (4)

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Publication number Priority date Publication date Assignee Title
US2801907A (en) * 1952-01-02 1957-08-06 Phillips Petroleum Co Process for the manufacture of crystals of uniform size
EP0632738B1 (fr) * 1992-03-27 1995-11-08 AlliedSignal Inc. Processus de cristallisation dans un appareil de cristallisation a chicane de tube d'aspiration
JP2005194153A (ja) * 2004-01-09 2005-07-21 Toray Ind Inc 硫安結晶の製造方法
WO2009007577A1 (fr) * 2007-07-09 2009-01-15 Crystal-Evap Consult Appareil de cristallisation a circulation forcee

Family Cites Families (1)

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DE19912699A1 (de) 1999-03-20 2000-09-28 Domo Caproleuna Gmbh Verfahren zur Steuerung der Kristallgröße bei der kontinuierlichen Massenkristallisation

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2801907A (en) * 1952-01-02 1957-08-06 Phillips Petroleum Co Process for the manufacture of crystals of uniform size
EP0632738B1 (fr) * 1992-03-27 1995-11-08 AlliedSignal Inc. Processus de cristallisation dans un appareil de cristallisation a chicane de tube d'aspiration
JP2005194153A (ja) * 2004-01-09 2005-07-21 Toray Ind Inc 硫安結晶の製造方法
WO2009007577A1 (fr) * 2007-07-09 2009-01-15 Crystal-Evap Consult Appareil de cristallisation a circulation forcee

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101734813B (zh) * 2009-12-21 2012-01-11 山东大明消毒科技有限公司 一种利用氰尿酸生产过程中的废酸液回收硫酸铵的工艺及其使用的设备
CN111498869A (zh) * 2020-04-14 2020-08-07 中石化南京工程有限公司 一种硫酸铵中和结晶方法及其装置
CN111530119A (zh) * 2020-04-14 2020-08-14 中石化南京工程有限公司 一种串联的硫酸铵结晶方法及其装置
CN111498869B (zh) * 2020-04-14 2022-11-15 中石化南京工程有限公司 一种硫酸铵中和结晶方法及其装置

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