DE102009018959B4 - Process for reducing thallium concentration in mineral salt solutions - Google Patents
Process for reducing thallium concentration in mineral salt solutions Download PDFInfo
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- DE102009018959B4 DE102009018959B4 DE102009018959.9A DE102009018959A DE102009018959B4 DE 102009018959 B4 DE102009018959 B4 DE 102009018959B4 DE 102009018959 A DE102009018959 A DE 102009018959A DE 102009018959 B4 DE102009018959 B4 DE 102009018959B4
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- thallium
- mineral salt
- kcl
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- reducing
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- 229910052716 thallium Inorganic materials 0.000 title claims abstract description 45
- BKVIYDNLLOSFOA-UHFFFAOYSA-N thallium Chemical compound [Tl] BKVIYDNLLOSFOA-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 22
- 229910052500 inorganic mineral Inorganic materials 0.000 title claims abstract description 17
- 239000011707 mineral Substances 0.000 title claims abstract description 17
- 239000012266 salt solution Substances 0.000 title claims abstract description 17
- 239000000243 solution Substances 0.000 claims description 21
- 238000001704 evaporation Methods 0.000 claims description 2
- 230000008020 evaporation Effects 0.000 claims description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 40
- 239000001103 potassium chloride Substances 0.000 description 20
- 235000011164 potassium chloride Nutrition 0.000 description 20
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 6
- 235000010755 mineral Nutrition 0.000 description 6
- 239000000203 mixture Substances 0.000 description 4
- 239000011780 sodium chloride Substances 0.000 description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 3
- 229910052700 potassium Inorganic materials 0.000 description 3
- 239000011591 potassium Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000003456 ion exchange resin Substances 0.000 description 2
- 229920003303 ion-exchange polymer Polymers 0.000 description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 235000014413 iron hydroxide Nutrition 0.000 description 1
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000012047 saturated solution Substances 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- -1 thallium ions Chemical class 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
-
- 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
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
-
- 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
- C02F1/68—Treatment of water, waste water, or sewage by addition of specified substances, e.g. trace elements, for ameliorating potable water
-
- 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
- C02F2101/20—Heavy metals or heavy metal compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/02—Temperature
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Removal Of Specific Substances (AREA)
Abstract
Verfahren zur Verringerung der Thalliumkonzentration in Mineralsalzlösungen, dadurch gekennzeichnet, dass eine Übersättigung an KCl in der Mineralsalzlösung nach allgemein üblichen Methoden herbeigeführt wird, sodass KCl kristallisiert und dabei Thallium aus der Mineralsalzlösung extrahiert wird.A process for reducing the concentration of thallium in mineral salt solutions, characterized in that a supersaturation of KCl in the mineral salt solution is brought about by generally customary methods, so that KCl crystallizes and thallium is thereby extracted from the mineral salt solution.
Description
Die Erfindung betrifft ein Verfahren zur Reduzierung der Thalliumkonzentration in Mineralsalzlösungen.The invention relates to a method for reducing the thallium concentration in mineral salt solutions.
Stand der TechnikState of the art
Wegen der hohen Toxizität des Thalliums ist man häufig bestrebt, dieses aus wässrigen Lösungen bis zu einer irrelevanten End-Konzentration zu entfernen. Dieses Bestreben gilt auch für wässrige Mineralsalzlösungen, insbesondere, wenn diese oder einer ihrer Inhaltsstoffe während ihres Lebenszyklus mit Menschen, Tieren, Pflanzen oder allgemein der Umwelt in Berührung kommen. Für diesen Fall ist es wichtig, das Thallium möglichst vollständig aus den Lösungen zu entfernen, um damit das Gefahrenpotenzial infolge der Toxizität des Thalliums weitgehend abzubauen. Bekannte Verfahren zur Reduzierung der Thalliumkonzentration sind Fällprozesse durch Einstellung eines geeigneten pH-Wertes oder unter Zuhilfenahme von allgemein bekannten Fällmitteln, wie Eisen- oder Aluminiumsalze. Nachteilig an diesen Verfahren ist, dass die Abreicherung von Thallium auf eine Konzentration unterhalb von 1 mg/l nicht oder nur mit erhöhtem technischen Aufwand möglich ist.Because of the high toxicity of thallium, one often strives to remove it from aqueous solutions to an irrelevant end concentration. This endeavor also applies to aqueous mineral salt solutions, especially when these or one of their ingredients come in contact with humans, animals, plants or the environment in general during their life cycle. In this case, it is important to remove the thallium as completely as possible from the solutions in order to largely reduce the potential danger due to the toxicity of thallium. Known methods for reducing the thallium concentration are precipitation processes by adjusting a suitable pH or with the aid of well-known precipitants, such as iron or aluminum salts. A disadvantage of this method is that the depletion of thallium to a concentration below 1 mg / l is not possible or only with increased technical complexity.
Eine weitere Methode besteht in der Anwendung von Ionenaustauscherharzen mit spezifisch wirkenden funktionellen Gruppen. Die Patentschrift
Ein weiteres Verfahren besteht in der Extraktion von Thallium aus wässrigen Lösungen mittels eines wenig wasserlöslichen organischen Reagenzes, das in organischen Lösungsmitteln gelöst wird und anschließend mit der wässrigen, thalliumhaltigen Lösung in Kontakt gebracht wird, wodurch insbesondere dreiwertige Thalliumionen in die organische Phase übergehen. Nachteilig an dieser Verfahrensweise ist, dass das Extraktionsmittel aufbereitet werden muss und stets Verluste des organischen Reagenzes in Kauf genommen werden müssen.Another method consists in the extraction of thallium from aqueous solutions by means of a little water-soluble organic reagent which is dissolved in organic solvents and then brought into contact with the aqueous solution containing thallium, whereby in particular trivalent thallium ions pass into the organic phase. A disadvantage of this procedure is that the extractant must be processed and always losses of the organic reagent must be taken into account.
Aus der
Aufgabe der ErfindungObject of the invention
Der Erfindung liegt daher die Aufgabe zugrunde, ein alternatives, kostengünstiges Verfahren zur Verringerung der Thalliumkonzentration in Mineralsalzlösungen bereitzustellen.The invention is therefore based on the object to provide an alternative, cost-effective method for reducing the Thalliumkonzentration in mineral salt solutions.
Beschreibung der ErfindungDescription of the invention
Überraschenderweise wurde gefunden, dass Thallium in einfacher und zugleich sehr effektiver Weise aus wässrigen Salzlösungen bis auf Thallium-Konzentrationen von 10–9 mol/l reduziert werden kann, wenn man Kaliumchlorid in dieser Lösung zur Kristallisation bringt. Dabei ist es unwesentlich, welche Mineralsalze neben dem Kaliumchlorid in der wässrigen Lösung enthalten sind. Voraussetzung für die Kristallisation ist das Bewirken einer Übersättigung von Kaliumchlorid. Die Art und Weise, mit der die Übersättigung an Kaliumchlorid erzielt wird, spielt eine untergeordnete Rolle im Bezug auf die Abreicherung des Thalliums in der wässrigen Lösung.It has surprisingly been found that thallium can be reduced in a simple and at the same time very effective manner from aqueous salt solutions to thallium concentrations of 10 -9 mol / l, if potassium chloride is crystallized in this solution. It is immaterial which mineral salts are included in the aqueous solution in addition to the potassium chloride. Prerequisite for the crystallization is the effect of supersaturation of potassium chloride. The manner in which the supersaturation of potassium chloride is achieved plays a minor role in terms of the depletion of thallium in the aqueous solution.
Eine Variante, mit der das kristallisierte und mit Thallium verunreinigte Kaliumchlorid weitgehend in den Prozess zurückgeführt werden kann, besteht darin, dass man das Kaliumchlorid-Thallium-Gemisch einer weiteren zu reinigenden Lösung zuführt, wodurch sich neben der Kaliumkonzentration auch die Thalliumkonzentration erhöht. Dabei ist zu beachten, dass die Löslichkeitsgrenze des Kaliumchlorids in der Lösung nicht überschritten wird. Dieses kann beispielsweise durch die Einstellung einer ausreichend hohen Temperatur bewirkt werden. Die nun mit Thallium weiter angereicherte Lösung kann mit anderen bekannten Verfahren, zum Beispiel Fällung, in ihrer Thalliumkonzentration verringert werden. Um Thallium quasi vollständig aus der Lösung zu entfernen, wird nach der Abtrennung des Präzipitates die Löslichkeitsgrenze des Kaliumchlorids beispielsweise durch Absenken der Temperatur überschritten, wodurch Kaliumchlorid kristallisiert und dabei das noch in der Lösung vorhandene Thallium mit aus der Lösung entfernt. Das Kaliumchlorid-Thallium-Gemisch kann anschließend wieder einer weiteren zu reinigenden Lösung zugeführt werden, und die Prozedur beginnt von neuem.A variant with which the crystallized and contaminated with thallium potassium chloride can be largely returned to the process, is that the potassium chloride-thallium mixture to another solution to be purified, whereby in addition to the potassium concentration and the thallium concentration increases. It should be noted that the solubility limit of the potassium chloride in the solution is not exceeded. This can be effected, for example, by setting a sufficiently high temperature. The now further enriched with thallium solution can be reduced by other known methods, such as precipitation, in their Thalliumkonzentration. To virtually completely remove thallium from the solution, after the separation of the precipitate, the solubility limit of the potassium chloride is exceeded, for example, by lowering the temperature, whereby potassium chloride crystallized, thereby removing the thallium still present in the solution with out of the solution. The potassium chloride-thallium mixture can then be returned to another solution to be purified, and the procedure begins again.
Es ist möglich, die Thalliumkonzentration in der Mineralsalzlösung auf einen Konzentrationsbereich von 10–10 bis 10–6 mol/l abzusenken.It is possible to lower the thallium concentration in the mineral salt solution to a concentration range of 10 -10 to 10 -6 mol / l.
Ausführungsbeispieleembodiments
Beispiel 1example 1
Eine Lösung mit 350 g/l KCl und 2,3 mg/l Thallium wird von 80°C auf 20°C abgekühlt, wodurch die KCl Konzentration auf 320 g/l und die Thalliumkonzentration auf 0,03 mg/l reduziert wurde. Das Kristallisat enthält 75 mg/kg Thallium.A solution containing 350 g / l KCl and 2.3 mg / l thallium is cooled from 80 ° C to 20 ° C, reducing the KCl concentration to 320 g / l and the thallium concentration to 0.03 mg / l. The crystals contain 75 mg / kg thallium.
Beispiel 2Example 2
Eine Lösung mit 330 g/l KCl, 15 g/l NaCl und 10 g/l Na2SO4 sowie mit 0,6 mg/l Thallium wird von 90°C auf 30°C abgekühlt. Nach der Abkühlung besitzt die Lösung folgende Zusammensetzung 315 g/l KCl, 14 g/l NaCl, 10 g/l Na2SO4 sowie 0,040 mg/l Thallium.A solution with 330 g / l KCl, 15 g / l NaCl and 10 g / l Na 2 SO 4 and with 0.6 mg / l thallium is cooled from 90 ° C to 30 ° C. After cooling, the solution has the following composition 315 g / l KCl, 14 g / l NaCl, 10 g / l Na 2 SO 4 and 0.040 mg / l thallium.
Beispiel 3Example 3
Eine Lösung mit 330 g/l KCl, 75 g/l NaCl und 5 g/l Na2SO4 sowie mit 1,6 mg/l Thallium wird von 90°C auf 10°C abgekühlt. Nach der Abkühlung besitzt die Lösung folgende Zusammensetzung: 310 g/l KCl, 76 g/l NaCl, 5 g/l Na2SO4 sowie 0,010 mg/l Thallium.A solution with 330 g / l KCl, 75 g / l NaCl and 5 g / l Na 2 SO 4 and with 1.6 mg / l thallium is cooled from 90 ° C to 10 ° C. After cooling, the solution has the following composition: 310 g / l KCl, 76 g / l NaCl, 5 g / l Na 2 SO 4 and 0.010 mg / l thallium.
Beispiel 4Example 4
Eine an KCl gesättigte Lösung mit 5,3 mg/l Thallium wird durch Verdampfung von Wasser in ihrem Volumen halbiert. Nach Abtrennung des dadurch erhaltenen Kristallisates ist die Lösung weiterhin an KCl gesättigt, jedoch kann kein Thallium mehr nachgewiesen werden. Die Lösung wird zur Gewinnung von KCl weiter eingedampft. Das Kristallisat mit 30 mg/kg Thallium wird einer an KCl untersättigten Lösung mit 15 mg/l Thallium zugeführt. Nach Zufuhr von Eisen(III)-chlorid wird bei pH = 7 ein thalliumhaltiger Eisenhydroxidschlamm ausgefällt. Nach dessen Abtrennung beträgt die Thalliumkonzentration in der Lösung 4,7 mg/l. Die Lösung wird eingedampft, wobei bei einer Thalliumkonzentration von 5,3 mg/l auch die KCl-Kristallisation beginnt und das kristallisierte, thalliumhaltige KCl zur Verringerung der Thalliumkonzentration weiterer thalliumhaltiger Mineralsalzlösungen verwendet werden kann.A KCl-saturated solution containing 5.3 mg / l thallium is halved in volume by evaporation of water. After separation of the crystallizate thus obtained, the solution is further saturated with KCl, but no more thallium can be detected. The solution is further evaporated to recover KCl. The crystallizate containing 30 mg / kg thallium is fed to a KCl undersaturated solution containing 15 mg / l thallium. After addition of iron (III) chloride, a thallium-containing iron hydroxide sludge is precipitated at pH = 7. After its separation, the thallium concentration in the solution is 4.7 mg / l. The solution is evaporated, at a Thalliumkonzentration of 5.3 mg / l, the KCl crystallization begins and the crystallized, thallium-containing KCl can be used to reduce the thallium concentration of other thalliumhaltiger mineral salt solutions.
Claims (5)
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE102009018959.9A DE102009018959B4 (en) | 2009-04-25 | 2009-04-25 | Process for reducing thallium concentration in mineral salt solutions |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE102009018959.9A DE102009018959B4 (en) | 2009-04-25 | 2009-04-25 | Process for reducing thallium concentration in mineral salt solutions |
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| Publication Number | Publication Date |
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| DE102009018959A1 DE102009018959A1 (en) | 2010-10-28 |
| DE102009018959B4 true DE102009018959B4 (en) | 2016-09-29 |
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| DE102009018959.9A Expired - Fee Related DE102009018959B4 (en) | 2009-04-25 | 2009-04-25 | Process for reducing thallium concentration in mineral salt solutions |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012143394A1 (en) | 2011-04-20 | 2012-10-26 | Solvay Sa | Method for recovery of thallium from an aqueous solution |
| CN106082502B (en) * | 2016-08-16 | 2019-06-18 | 华南理工大学 | A kind of method of thallium in removal waste water |
| CN110655228A (en) * | 2019-08-31 | 2020-01-07 | 广东韶钢松山股份有限公司 | Wastewater treatment process and system |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1996019413A1 (en) * | 1994-12-20 | 1996-06-27 | M.I.M. Hüttenwerke Duisburg Gesellschaft Mit Beschränkter Haftung | Process for treating waste water containing metals |
| DE19963988A1 (en) * | 1999-12-31 | 2001-07-05 | Stefan Weisgraeber | Treatment of waste fluids containing arsenic involves treatment with ammonium iron sulfate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| FR2657863B1 (en) | 1990-02-05 | 1992-08-28 | Metaleurop Sa | THALLIUM EXTRACTION PROCESS. |
| DE4312038A1 (en) | 1993-04-13 | 1994-10-20 | Bayer Ag | Multiple regenerable ion exchange resins with low alkyl SH group occupancy |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1996019413A1 (en) * | 1994-12-20 | 1996-06-27 | M.I.M. Hüttenwerke Duisburg Gesellschaft Mit Beschränkter Haftung | Process for treating waste water containing metals |
| DE19963988A1 (en) * | 1999-12-31 | 2001-07-05 | Stefan Weisgraeber | Treatment of waste fluids containing arsenic involves treatment with ammonium iron sulfate |
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