EP0341580A2 - Procédé de purification par distillation de matériaux contenant du mercure ou bien de matériaux mixtes - Google Patents

Procédé de purification par distillation de matériaux contenant du mercure ou bien de matériaux mixtes Download PDF

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Publication number
EP0341580A2
EP0341580A2 EP89108089A EP89108089A EP0341580A2 EP 0341580 A2 EP0341580 A2 EP 0341580A2 EP 89108089 A EP89108089 A EP 89108089A EP 89108089 A EP89108089 A EP 89108089A EP 0341580 A2 EP0341580 A2 EP 0341580A2
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EP
European Patent Office
Prior art keywords
distillation apparatus
mercury
feed material
liquid
distillation
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.)
Granted
Application number
EP89108089A
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German (de)
English (en)
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EP0341580B1 (fr
EP0341580A3 (en
Inventor
Gerhard Dipl.-Ing. Bernecker
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Individual
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Publication of EP0341580B1 publication Critical patent/EP0341580B1/fr
Anticipated expiration legal-status Critical
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B43/00—Obtaining mercury

Definitions

  • the invention relates to a method for the purification by distillation of mercury-containing substances or mixtures of substances and / or for the production of mercury therefrom.
  • Processes for the production of mercury by dry distillation from mercury-containing substances are known from the smelting of ores or minerals containing mercury. It is also known to purify mercury-containing residues, for example from acetaldehyde electrolysis or activated carbon sludges from chloralkali electrolysis, by such dry distillation from mercury.
  • These prior art methods include that the feed is dried as much as possible before being introduced into the distillation apparatus so as not to have to additionally apply the heat of vaporization for the water in the distillation process, which must therefore be removed beforehand by drying. If, for example, the raw material was enriched by flotation in the case of mercury smelting, the aim is to use the material in the still lation or roasting ovens reduce the moisture content to approx. 8 to 10%.
  • residues containing mercury are also dewatered by mechanical separation processes before the mercury is removed by distillation by thermal treatment of the feed material; for example, mercury-containing sludges from chlor-alkali electrolysis are reduced to approx. 20 to 45% by weight in the moisture content by filter presses.
  • the known distillers for the production of mercury or the purification of mercury can be classified according to whether and how the feed material is moved during the distillation process.
  • the material is not moved. It rests in one or more layers either directly on the walls of the distillation apparatus or on sheets to which it was previously applied and which are then introduced into the distillation apparatus.
  • These apparatuses are preferably used when fine-grained or powdery material is treated in order to minimize the dust discharge with the vapors and gases which are derived from the distillation apparatus. This process is a batch operation with the Heating of inert masses.
  • the material is moved slightly during the distillation process, but migrates through the distillation apparatus during the process.
  • This principle is preferably used in the smelting of minerals containing mercury, e.g. in shaft furnaces with or without built-in.
  • a third variant involves moving the material during the distillation process in order to improve mass and heat transfer processes during the distillation process.
  • rotary kilns are known in the prior art. These work by rotating a rotary tube with its axis set up horizontally or slightly inclined against the horizontal around its axis. This means that the material always comes into contact with new parts of the wall or, in contrast to a dormant layer, is exposed to a different surface of the furnace atmosphere.
  • rotary kiln devices are usually loaded and emptied in batch mode. In the case of a slightly inclined arrangement, the material to be treated migrates in the direction of inclination of the axis through the rotary kiln, the residence time being the set speed is true. It is also known to install internals inside the rotary tubes which are intended to prevent the material from being reduced in size and to support movements of the goods.
  • the known methods for the distillation treatment of mercury-containing substances can also be differentiated according to whether the distillation - at atmospheric pressure or slight negative pressure, - Or is carried out in a vacuum.
  • the known apparatus for treating mercury-containing substances are operated at about atmospheric pressure.
  • a slight negative pressure is set, which has the purpose of preventing leaks from the furnace atmosphere to the outside, to prevent mercury losses to the environment, as well as for reasons of occupational health and safety and to increase the mercury yield.
  • the low pressure in the distillation apparatus is usually only a few millimeters of water, but not less than 0.9 bar absolute pressure.
  • the distillation furnaces are heated either directly, for example by flames or flue gases, or indirectly via one of the walls, for example by flames or electrically.
  • the processes that work at atmospheric pressure or slight negative pressure to reduce the leakage, and essentially all of those in which the material is moved during the distillation process, require high temperatures, above about 400 to 600 ° C. Otherwise the residual mercury content in the treated substances is too high.
  • the introduction of the required heat in indirect heat exchange by condensing steam from a heating medium or by releasing the heat of a heat transfer fluid is technically not possible under economic conditions.
  • distillation ovens in which the good during the distillation process is not moved, working in a vacuum is known.
  • indirect heating with equipment such as water vapor or heat transfer oil is known. Such heating is desirable because it gives better heat transfer coefficients than heating with gaseous media. Overall, indirect heating is desirable, because with direct heating the amount of exhaust gas increases and the mercury losses increase due to the partial pressure of mercury. This is the main source of loss in mercury smelters. With direct heating, there is also a greater risk of dust being carried away due to higher flow velocities in the furnace. There is also a fire risk if mercury-containing activated carbon is to be freed from mercury.
  • Distillation ovens with essentially static goods have the disadvantage of poor heat and mass transfer. Layers can crust over, especially with fine-grained substances such as activated carbon in powder form. There is no adequate transport mechanism through the dormant material layer to create a sufficient partial pressure gradient for mercury. As a result, there are long treatment times in the ovens.
  • the usual reduction of the water content before on according to the state of the art The introduction into the distillation apparatus should also be considered with regard to the formation of dust in the distillation apparatus and the introduction of dust into the condensation stage. By reducing the water content in the feed, the amount of water evaporating in the still is to be reduced. In the case of directly heated stoves, the amount of flue gas can be kept lower.
  • the oven throughput time can be shortened for indirectly heated, especially those with stationary goods.
  • the heating and evaporation takes place, for example, via electrical heating elements which were arranged in the interior of the furnace. Heat transfer takes place - by radiation from the heating elements to the hood, - from the hood in turn to the hordes by radiation, - Of these by heat conduction and radiation to the feed.
  • ballast masses of steel must be warmed up and cooled for each batch. This is very energy intensive. In addition, due to the sluggish heat transfer only one oven load in 24 hours.
  • the furnace heating is switched off when the shift of the system operated in viewing mode ends.
  • the ovens are left with the trolleys and the feed material until the start of the shift the next morning for cooling by natural convection.
  • the emergency vehicles have to be changed at the beginning of the shift.
  • the flange connection for exhaust gas cleaning must be loosened on the emergency vehicle that has not yet cooled to ambient temperature.
  • the emergency vehicle which is pulled out of the oven by muscle power, is then left to cool down further.
  • the liquid mercury which had accumulated in the collecting pipe under the emergency vehicle, is drained by gravity in the open river into a collecting vessel, driven with the forklift to the collecting container of the mercury filling and drained there.
  • the hood is pulled.
  • the tray trays on the emergency vehicles are transported to the emptying site by forklift trucks.
  • the treated material is transferred to the landfill in transport packaging using a vacuum suction system.
  • mercury can be obtained from substances containing mercury. Furthermore, gases or vapors are led to the condensation stage, which contain little dust due to the washing effect of the suspension applied. Without this washing effect, the intended movement of the goods in the apparatus would not be possible, since too much dust would be discharged, especially when treating activated carbon, which is already in powder form, which would be ground, or which would have had the corresponding amounts of dust due to the abrasion of granular coal. Especially when it comes to the treatment of activated carbon, there are all the features that favor the formation of stupp according to the known state of the art: - carbon content, - fine grain, - Movement in the still.
  • mercury can be obtained from substances containing mercury. Furthermore, gases or vapors are led to the condensation stage, which contain little dust due to the washing effect of the suspension applied. Without this washing effect, the intended movement of the goods in the apparatus would not be possible, since too much dust would be discharged, in particular when treating activated carbon, which is already in powder form, and would be ground, or would have been given the appropriate proportion of dust by abrasion of granular coal. Especially when it comes to the treatment of activated carbon, there are all the features that favor the formation of stupp according to the known state of the art: Carbon content, Fine grain, Movement in the still.
  • the possibility of working in a vacuum in the method according to the invention enables indirect heating with steam and / or a heat transfer fluid to be implemented, because the vapor pressure of the mercury then enables a sufficiently low residual mercury content in the treated material at temperatures below 400 ° C.
  • the lower temperatures simplify the choice of material for the distillation apparatus, and the conditions are created for the mechanical implementation of the rotating internals for scraping the material off walls.
  • the disadvantage of the dormant layers of the material to be treated with poor heat and mass transfer ratios is avoided.
  • the batch operation typical of stills with still layers is avoided, in which, when heating up and cooling down, ever larger masses of the furnace construction have to be heated and cooled as ballast. Health hazards to the operating personnel when handling material containing mercury, which is mostly manual loading, are avoided.
  • the liquid of the sprayed-in suspension exerts a washing action on the vapors and gases passing in countercurrent in the upper part of the distillation apparatus and thus reduces the dust discharge to a tolerable residue.
  • the present invention is based on the object of providing a method for the distillative cleaning of mercury-containing substances or mixtures of substances which enables extensive cleaning of the feed material, is environmentally friendly and does not burden people, which can be operated continuously and is energy-efficient.
  • This object is achieved according to the invention in a method of the type mentioned at the outset by injecting the feed material into the distillation apparatus as a solid / liquid suspension or solution, or atomizing or spraying therein, preferably by means of a rotary atomizer.
  • Special embodiments are characterized in that work is carried out at a pressure lower than 1 bar, under vacuum compared to atmospheric pressure or in a vacuum, that the feed is moved that the liquid phase begins to boil at lower temperatures than mercury, that the feed has a dry matter content ⁇ (less than or equal to) 42% by weight, preferably 10 to 30% by weight, that the feed material has been warmed up to such an extent before it is introduced into the still that the temperature level is not lower than 10 K below the evaporation point of the earliest boiling liquid constituents of the suspension - calculated at the absolute pressure prevailing in the still, preferably at or above it Temperature, but not higher than it would correspond to a spontaneous evaporation of 10% of the liquid when relaxing to the pressure prevailing in the distillation apparatus that a gaseous medium is introduced into the distillation apparatus at the outlet end in order to improve the mass transport for mercury in the part of the distillation apparatus as an entraining gas, in which the suspension liquid has largely evaporated and that the suspension is wet-milled before it is used in the
  • the second stage is designed as a washing column, preferably with a packed bed, and the liquid phase is discharged via a separating vessel, that a substance is added to the washing liquid to selectively increase the absorption of mercury, that the direct condensation works at a temperature of the feed liquid at the top of the column which is ⁇ (less than or equal to) 6 ° C., and that the partial pressure of the mercury in the gases which are not condensed when leaving the column is greatly reduced
  • the direct condensation stage is carried out in two stages with - a lower stage, in which the circulating liquid is recooled by a cooling medium that has a flow temperature ⁇ (greater / equal) 6 ° C, and a second stage, in which the added liquid has a temperature ⁇ (less / equal) 6 ° C is given up, that it is used for the regeneration of activated carbon, that a washing effect is exerted on occurring and discharged gases or vapors
  • a device for carrying out the method according to the invention is also claimed, which is characterized in that that the distillation apparatus is designed as a cylindrical container so that the inside length is at least four times as large as the inside knife, and consists of a fixed jacket - and a rotating device inside the same . for moving / promoting the feed material,. and for scraping or scraping the latter off the inner wall of the distillation apparatus, for preventing the feed material from falling freely until the end of the apparatus after scraping with a vertical arrangement of the axis of rotation of the distillation apparatus,.
  • the walls of the distillation apparatus are largely designed as double jackets or are equipped with pipe coils welded onto the outside, that the outer wall of the distillation apparatus is equipped with at least two different operating rooms, that the lower temperature level is generated on the equipment side by condensing water vapor in the equipment room at a pressure of 2 to 25 bar, preferably 10 to 12 bar, and the higher by heating the equipment rooms with a heat transfer medium in the temperature range of 250 to 370 ° C, preferably 300 to 350 ° C, that the vacuum generating device, preferably a water ring pump, is arranged between the first and second condensation stages.
  • an Hg-containing activated carbon suspension is introduced into this distillation apparatus and the treatment is freed of mercury in the manner described and thus - regenerates for reuse in adsorption processes - Or can be sent for further disposal by incineration or landfill without this mercury content.
  • the designs of the walls of the distillation apparatus have the task of keeping the wall temperatures at nominal operation above the dew point of vapors, which are evaporated from the feed material, and to serve as operating room for vaporous or liquid heating media for the transfer of the heat of vaporization and the sensible heat in indirect Heat exchange through the wall of the still to the feed.
  • the division of the apparatus means that impurities from the distillation apparatus preferably precipitate out in the first stage and, as a result, the washing liquid is not loaded with them in the second stage and pure Hg is obtained.
  • the cleaned exhaust gas is released into the atmosphere via an exhaust gas chimney.
  • the liquids condensed out in the condensation stages - essentially water and mercury with impurities - are separated by decantation.
  • the water is fed to a process water collection container. From it, the amount of water required for the preparation station is used again. The rest are then cleaned and then stored in a container for clean process water to e.g. to be used again as washing water in the process or the barrel washing station. Excess quantities are discharged into the sewage system as waste water after cleaning.
  • the separated mercury is weighed in a weighing station so that the recovered mercury can be assigned to the processed customer batches. Then it is collected in a buffer container. From there, if it is necessary for the respective application, it is further cleaned and in the filling station in the Commercially available 36.5 kg steel containers filled ready for dispatch.
  • FIG. 1 shows a device for carrying out the method according to the invention.
  • distillation apparatus 1 It is a distillation apparatus 1 with a rotary atomizer 2.
  • the jacket 3 of the distillation apparatus contains a rotating device 4 in the distillation apparatus.
  • the distillation apparatus 1 has an operating medium space 5 for water vapor and operating medium spaces 6, 7 for hot oil as the heat transfer medium.
  • the device has a heat exchanger 8 for water heating. There is also an injection condenser 9, separator / decanter 10, washing column 11 and separator / decanter 12.
  • the system has a vacuum pump 13 as well as an attachment and preheating container 14.
  • the distillation apparatus 1 is connected to a cooling device 18, which in turn is connected to discharge containers 19 and 20 from vacuum.
  • the system also has circulation pumps 23 and 25 and coolers 24 and 26.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Treating Waste Gases (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
EP89108089A 1988-05-12 1989-05-05 Procédé de purification par distillation de matériaux contenant du mercure ou bien de matériaux mixtes Expired - Lifetime EP0341580B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE3816282A DE3816282C1 (fr) 1988-05-12 1988-05-12
DE3816282 1988-05-12

Publications (3)

Publication Number Publication Date
EP0341580A2 true EP0341580A2 (fr) 1989-11-15
EP0341580A3 EP0341580A3 (en) 1990-10-17
EP0341580B1 EP0341580B1 (fr) 1995-07-26

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ID=6354263

Family Applications (1)

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EP89108089A Expired - Lifetime EP0341580B1 (fr) 1988-05-12 1989-05-05 Procédé de purification par distillation de matériaux contenant du mercure ou bien de matériaux mixtes

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Country Link
EP (1) EP0341580B1 (fr)
AT (1) ATE125575T1 (fr)
DE (2) DE3816282C1 (fr)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4127506C1 (fr) * 1991-08-20 1992-10-15 Hak-Anlagenbau Gmbh, 2000 Hamburg, De
EP0663960A4 (fr) * 1992-09-18 1996-05-29 Pittsburgh Mineral Environment Procede de suppression de mercure de sols et de dechets industriels contamines et dispositif correspondant.
US20120240761A1 (en) * 2011-03-22 2012-09-27 Mitsubishi Heavy Industries, Ltd. Air pollution control system and air pollution control method, spray drying device of dewatering filtration fluid from desulfurization discharged water, and method thereof
CN109705171A (zh) * 2019-01-08 2019-05-03 天元军融(辽宁)化工研究所新材料孵化器股份有限公司 一种二茂铁快速提纯方法及装置
CN115896485A (zh) * 2022-11-21 2023-04-04 中国电子科技集团公司第十一研究所 一种汞蒸馏提纯设备及汞提纯方法

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
NL9101802A (nl) * 1991-10-28 1993-05-17 Recycling Nederland B V Werkwijze en inrichting voor het verwijderen van een of meer verontreinigingen uit een bulkmateriaal.
DE4429869C1 (de) * 1994-08-23 1996-01-18 Degussa Verfahren zur Aufarbeitung zinkhaltiger Amalgame
DE19547151C2 (de) * 1995-12-16 1999-06-17 Ald Vacuum Techn Gmbh Verfahren und Vorrichtung zum Aufarbeiten von Stoffgemischen mit mindestens zwei Phasen mit unterschiedlichen Siedetemperaturen

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE361439C (de) * 1921-02-17 1922-10-14 Alexander Wacker Dr Verfahren zur Regenerierung von Quecksilberschlamm
DE688563C (de) * 1938-08-17 1940-02-24 Georg Plueschke Vorrichtung zum Gewinnen von Quecksilber
GB1373771A (en) * 1971-03-05 1974-11-13 Bp Chem Int Ltd Mercury recovery process
SE361181B (fr) * 1971-07-02 1973-10-22 Graenges Eng Ab
IT1037842B (it) * 1975-05-05 1979-11-20 Anic Spa Processo per la rimozione di mercurio da fanghi che lo contengono
DD230270A3 (de) * 1982-09-07 1985-11-27 Bitterfeld Chemie Verfahren und vorrichtung zur aufarbeitung von quecksilberhaltigen materialien
JPH10222979A (ja) * 1997-01-31 1998-08-21 Mitsubishi Electric Corp 情報処理装置

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4127506C1 (fr) * 1991-08-20 1992-10-15 Hak-Anlagenbau Gmbh, 2000 Hamburg, De
EP0663960A4 (fr) * 1992-09-18 1996-05-29 Pittsburgh Mineral Environment Procede de suppression de mercure de sols et de dechets industriels contamines et dispositif correspondant.
US20120240761A1 (en) * 2011-03-22 2012-09-27 Mitsubishi Heavy Industries, Ltd. Air pollution control system and air pollution control method, spray drying device of dewatering filtration fluid from desulfurization discharged water, and method thereof
US8715402B2 (en) * 2011-03-22 2014-05-06 Mitsubishi Heavy Industries, Ltd. Air pollution control system and air pollution control method, spray drying device of dewatering filtration fluid from desulfurization discharged water, and method thereof
US20140202362A1 (en) * 2011-03-22 2014-07-24 Mitsubishi Heavy Industries, Ltd. Air pollution control system, air pollution control method, spray drying device of dewatering filtration fluid from desulfurization discharged water, and method thereof
US8883107B2 (en) 2011-03-22 2014-11-11 Mitsubishi Heavy Industries, Ltd. Air pollution control system, air pollution control method, spray drying device of dewatering filtration fluid from desulfurization discharged water, and method thereof
US9409117B2 (en) 2011-03-22 2016-08-09 Mitsubishi Hitachi Power Systems, Ltd. Air pollution control system, air pollution control method, spray drying device of dewatering filtration fluid from desulfurization discharged water, and method thereof
CN109705171A (zh) * 2019-01-08 2019-05-03 天元军融(辽宁)化工研究所新材料孵化器股份有限公司 一种二茂铁快速提纯方法及装置
CN115896485A (zh) * 2022-11-21 2023-04-04 中国电子科技集团公司第十一研究所 一种汞蒸馏提纯设备及汞提纯方法

Also Published As

Publication number Publication date
EP0341580B1 (fr) 1995-07-26
ATE125575T1 (de) 1995-08-15
EP0341580A3 (en) 1990-10-17
DE3816282C1 (fr) 1989-10-05
DE58909362D1 (de) 1995-08-31

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