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WO2008113387A1 - Procédé pour séparer un mélange contenant du sel - Google Patents

Procédé pour séparer un mélange contenant du sel Download PDF

Info

Publication number
WO2008113387A1
WO2008113387A1 PCT/EP2007/002467 EP2007002467W WO2008113387A1 WO 2008113387 A1 WO2008113387 A1 WO 2008113387A1 EP 2007002467 W EP2007002467 W EP 2007002467W WO 2008113387 A1 WO2008113387 A1 WO 2008113387A1
Authority
WO
WIPO (PCT)
Prior art keywords
salt
slurry
ice
belt filter
crystallizer
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.)
Ceased
Application number
PCT/EP2007/002467
Other languages
English (en)
Inventor
J. A. Evers
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.)
Metso Finland Oy
Original Assignee
Larox Oyj
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 Larox Oyj filed Critical Larox Oyj
Priority to PCT/EP2007/002467 priority Critical patent/WO2008113387A1/fr
Priority to PCT/EP2007/005686 priority patent/WO2008113395A1/fr
Publication of WO2008113387A1 publication Critical patent/WO2008113387A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • 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
    • B01D9/0004—Crystallisation cooling by heat exchange
    • 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
    • B01D9/00—Crystallisation
    • B01D9/02—Crystallisation from solutions
    • B01D9/04—Crystallisation from solutions concentrating solutions by removing frozen solvent therefrom
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/22—Treatment of water, waste water, or sewage by freezing
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F11/00—Treatment of sludge; Devices therefor
    • C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
    • C02F11/121—Treatment of sludge; Devices therefor by de-watering, drying or thickening by mechanical de-watering
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F11/00—Treatment of sludge; Devices therefor
    • C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
    • C02F11/16—Treatment of sludge; Devices therefor by de-watering, drying or thickening using drying or composting beds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F9/00—Multistage treatment of water, waste water or sewage

Definitions

  • Eutectic freeze crystallization is a technique to separate salt from salt bearing aqueous solutions producing pure ice as by product.
  • the output from the crystallizer is a salt slurry and an ice slurry.
  • the present invention provides a process for separating a mixture containing salt, into an ice slurry and a salt slurry, comprising the steps of feeding the mixture to a crystallizer having a first output for the ice slurry and a second output for the salt slurry, treating the salt slurry, so that a liquid part is recycled to the crystallizer, the salt remaining, and washing the ice slurry on the belt filter, whereby purified ice is outputted from the belt filter, as well a liquid which can be recycled to the crystallizer.
  • the de-watered ice crystals (filter cake) are washed on the belt filter, increasing the wash efficiency, viz. using less water and/or producing more purified ice crystals.
  • Preferred applications for the process of the present invention relate to MgSO 4 , CaCO 3 , HNO 3 among others.
  • the salt slurry is treated on a belt filter, preferably in three stages, so that purified salt is obtained at the end of the belt filter.
  • the de-watered salt crystals are washed with a saturated salt solution, producing more purified salt crystal .
  • the aqueous solution can be pre-concentrated in a conventional freeze crystallization, operating at a higher temperature than the eutectic temperature to produce ice crystals only.
  • a conventional freeze crystallizer can operate at higher cooling transfer rates than in a eutectic freeze crystallizer, resulting in a use of less cooling surface area and reduced capital cost.
  • In the pre-concentrated ice solution can be fed to a belt filter, which can either be the same belt filter receiving ice suspension from the eutectic freeze crystallizer or a separate belt filter.
  • Figure 1 a flow diagram of a preferred embodiment of the process according to the present invention
  • Figure 2 a side view of a preferred embodiment of an apparatus to be used with the process according to the present invention
  • Figure 3 a sectional view of the embodiment shown in Figure 2;
  • Figure 4 a sectional view of the embodiment shown in Figures 2 and 3 ; and Figure 5 a more detailed sectional view of the embodiment shown in Figures 2, 3 and 4.
  • a solution comprising CaCO 3 is fed to a buffer tank 12.
  • a solution is fed to a precooler 14 for cooling the solution.
  • the precooled solution is fed from the precooler to a crystallizer 16 from which the ice slurry goes to an ice slurry buffer 18 and into a first gravitation separator 20 from which a salt slurry is fed back to the crystallizer 16.
  • An ice slurry is fed to an ice slurry buffer 22, from which the ice slurry is fed to a belt filter 24, having two stages 26 and 28 resp.
  • liquid is sucked off and fed back to the buffer tank 12, while on the second stage 28 the slurry is washed with ice water from an ice water buffer 30, which is supplied with clean water from a tank 32 and the washing liquid being sucked off and fed back to the ice water buffer.
  • the washed and cleaned ice is output into ice buffer 34.
  • a second output is output to a second gravitation separator 36, having an ice output which is fed back to the buffer tank 12 and a salt output being output to a belt filter 38, showing three stages 40, 42 and 44 resp.
  • the output from the first stage being fed back to stage 12.
  • saturated soda is added from a buffer 46 from which second stage the output is drained to a spent wash buffer 48.
  • the salt is dried in the third stage 44 by purging hot air indicated by arrow 50, so that pure salt is available at the end of the belt filter, which can be sold for commercial purposes.
  • a preferred embodiment 110 of the apparatus according to the present invention ( Figure 2) comprises a lower hopper 112 which is supported by a steel construction comprising legs 113, 114 and 115, as well as intermediate modular parts 120, 122, 124 as well as a top part 126.
  • Each of the modules 120, 122, 124 is provided with an inlet 121, 123, 125 for introducing a mixture or solution into the interior of the modules, of which interiors are in open connection with the interiors of the modules below and above.
  • Each of the intermediate modules is also provided with a manhole 127 for inspection and reparation thereof.
  • the top part 126 is provided with an discharge 127 for discharging ice crystals.
  • the top part 126 includes a variable speed electric motor 128 (see also Figure 3) , driving a central shaft 129 extending through the module to a scraper 130 in the lower part 112. In the top part, the electric motor also drives a propeller 132 to press the ice
  • a clutch mechanism 133 is provided for driving the propeller 132.
  • each of the intermediate modules 120, 122, 124 is provided with arms 136, 137, 138, 139 coupled to the central shaft 129 for supportingO scrapers 146 to scrape ice from two cylindrical walls 140, 145 and 141, 144.
  • Each of the intermediate modules is provided with a connection 142 for cooling fluid for flowing in and out of helical line 143 which are provided in annular spaces between walls 140, 145 and 141, 144.
  • the above described apparatus can easily be used for recover of crystallized material including MgSO 4 from aqueous solutions. Of course, it will also be possible to use it for salts, such as HNO 3 or Ca(NO 3 ) 2 .
  • the overall temperature of the solution can be e.g. within 2.0 0 C, preferably 0.5 0 C or 0.1 0 C of the eutectic point of such medium, e.g. around -12°C for MgSO 4 .
  • the overall height of the apparatus can be a 1-10 metres.

Landscapes

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

Abstract

L'invention concerne un procédé pour séparer un mélange contenant du sel en bouillie de glace et en bouillie de sel. Ce procédé comprend les étapes consistant à amener le mélange dans un cristalliseur qui présente une première sortie pour la bouillie de glace et une deuxième sortie pour la bouillie de sel; à traiter la bouillie de sel de sorte qu'une partie liquide soit recyclée dans le cristalliseur, le sel étant conservé; et à laver la bouillie de glace sur un filtre à bande, ledit filtre permettant d'obtenir de la glace purifiée ainsi qu'un liquide pouvant être recyclé dans le cristalliseur.
PCT/EP2007/002467 2007-03-20 2007-03-20 Procédé pour séparer un mélange contenant du sel Ceased WO2008113387A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
PCT/EP2007/002467 WO2008113387A1 (fr) 2007-03-20 2007-03-20 Procédé pour séparer un mélange contenant du sel
PCT/EP2007/005686 WO2008113395A1 (fr) 2007-03-20 2007-06-27 Procédé pour séparer un mélange contenant du sel

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/EP2007/002467 WO2008113387A1 (fr) 2007-03-20 2007-03-20 Procédé pour séparer un mélange contenant du sel

Publications (1)

Publication Number Publication Date
WO2008113387A1 true WO2008113387A1 (fr) 2008-09-25

Family

ID=38683556

Family Applications (2)

Application Number Title Priority Date Filing Date
PCT/EP2007/002467 Ceased WO2008113387A1 (fr) 2007-03-20 2007-03-20 Procédé pour séparer un mélange contenant du sel
PCT/EP2007/005686 Ceased WO2008113395A1 (fr) 2007-03-20 2007-06-27 Procédé pour séparer un mélange contenant du sel

Family Applications After (1)

Application Number Title Priority Date Filing Date
PCT/EP2007/005686 Ceased WO2008113395A1 (fr) 2007-03-20 2007-06-27 Procédé pour séparer un mélange contenant du sel

Country Status (1)

Country Link
WO (2) WO2008113387A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10246345B2 (en) 2015-12-30 2019-04-02 General Electric Company Water desalination system and method for fast cooling saline water using turbines
CN110759565A (zh) * 2019-10-15 2020-02-07 广西金川有色金属有限公司 一种去除离子液中热稳定性盐的方法

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
NL2011027C2 (en) 2013-06-24 2014-12-29 Univ Delft Tech Process for the preparation of 2,5-furandicarboxylic acid.
CN103910396B (zh) * 2014-03-19 2015-10-28 北京师范大学 一种利用微波海冰破碎排盐方法
CN104163450A (zh) * 2014-07-23 2014-11-26 云南锡业股份有限公司 一种铜电解液生产硫酸铜的脱水方法
CN106630398B (zh) * 2016-12-02 2019-07-16 自然资源部天津海水淡化与综合利用研究所 一种处理高盐有机废水的方法
CN106882890A (zh) * 2017-03-24 2017-06-23 中国石油化工股份有限公司天然气分公司 一种基于液化天然气冷能的冷冻‑微波‑离心复合海水淡化方法及装置
CN110550609A (zh) * 2019-08-23 2019-12-10 上海应用技术大学 一种浓缩酸性废水回收硫酸的方法
CN110606613A (zh) * 2019-10-09 2019-12-24 北京国电富通科技发展有限责任公司 一种高含盐废水波能结晶方法和装置

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3150499A (en) * 1961-01-23 1964-09-29 Halcon International Inc Apparatus for refrigerating saline water
US4247341A (en) * 1979-06-18 1981-01-27 Zep Pey Chen Continuous massecuite vacuum filtering system
US5623168A (en) * 1991-09-18 1997-04-22 Wasagchemie Sythen Gmbh Reduction of the grain size of crystalline explosive
EP1094047A1 (fr) * 1999-10-22 2001-04-25 Technische Universiteit Delft Crystallisation de materiau a partir de solutions aqueuses
WO2006013228A1 (fr) * 2004-08-04 2006-02-09 Kemira Growhow Oyj Procede de recuperation de composants organiques et inorganiques a partir d'un flux de dechets

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10242746B4 (de) * 2002-09-13 2010-07-01 Evonik Degussa Gmbh Waschvorrichtung, ein Verfahren zur Aufreinigung eines Waschguts sowie die Verwendung der Waschvorrichtung

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3150499A (en) * 1961-01-23 1964-09-29 Halcon International Inc Apparatus for refrigerating saline water
US4247341A (en) * 1979-06-18 1981-01-27 Zep Pey Chen Continuous massecuite vacuum filtering system
US5623168A (en) * 1991-09-18 1997-04-22 Wasagchemie Sythen Gmbh Reduction of the grain size of crystalline explosive
EP1094047A1 (fr) * 1999-10-22 2001-04-25 Technische Universiteit Delft Crystallisation de materiau a partir de solutions aqueuses
WO2006013228A1 (fr) * 2004-08-04 2006-02-09 Kemira Growhow Oyj Procede de recuperation de composants organiques et inorganiques a partir d'un flux de dechets

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10246345B2 (en) 2015-12-30 2019-04-02 General Electric Company Water desalination system and method for fast cooling saline water using turbines
CN110759565A (zh) * 2019-10-15 2020-02-07 广西金川有色金属有限公司 一种去除离子液中热稳定性盐的方法

Also Published As

Publication number Publication date
WO2008113395A1 (fr) 2008-09-25
WO2008113395A8 (fr) 2008-12-04

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