US20140056786A1 - Device and Method for the Thermal Treatment of Fluorine-Containing and Noble Metal-Containing Products - Google Patents

Device and Method for the Thermal Treatment of Fluorine-Containing and Noble Metal-Containing Products Download PDF

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Publication number
US20140056786A1
US20140056786A1 US13/969,009 US201313969009A US2014056786A1 US 20140056786 A1 US20140056786 A1 US 20140056786A1 US 201313969009 A US201313969009 A US 201313969009A US 2014056786 A1 US2014056786 A1 US 2014056786A1
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US
United States
Prior art keywords
exhaust gas
thermal treatment
scrubber
plant according
insulating lining
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.)
Abandoned
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US13/969,009
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English (en)
Inventor
Jose Manuel Romero
Horst Meyer
Steffen Voss
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.)
Heraeus Deutschland GmbH and Co KG
Original Assignee
Heraeus Precious Metals GmbH and Co KG
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 Heraeus Precious Metals GmbH and Co KG filed Critical Heraeus Precious Metals GmbH and Co KG
Assigned to HERAEUS PRECIOUS METALS GMBH & CO. KG. reassignment HERAEUS PRECIOUS METALS GMBH & CO. KG. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: Romero, Jose Manuel, VOSS, STEFFEN, MEYER, HORST, DR
Publication of US20140056786A1 publication Critical patent/US20140056786A1/en
Abandoned legal-status Critical Current

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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
    • C22B11/00—Obtaining noble metals
    • C22B11/02—Obtaining noble metals by dry processes
    • C22B11/021—Recovery of noble metals from waste materials
    • C22B11/026—Recovery of noble metals from waste materials from spent catalysts
    • 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
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/001—Dry processes
    • 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
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • 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
    • C22B11/00—Obtaining noble metals
    • C22B11/02—Obtaining noble metals by dry processes
    • 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
    • C22B11/00—Obtaining noble metals
    • C22B11/02—Obtaining noble metals by dry processes
    • C22B11/021—Recovery of noble metals from waste materials
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/008—Disposal or recycling of fuel cells
    • 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
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling
    • 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
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/84—Recycling of batteries or fuel cells

Definitions

  • the present invention relates to a device and a method for thermal treatment of noble metal-containing products which also contain fluorine aside from noble metals.
  • noble metal-containing products such as, for example, catalysts or fuel cells.
  • the noble metal-containing layer of catalysts is dissolved off the ceramic support by means of strong acids or bases. Subsequently, the noble metals are separated from the solution, for example through precipitation reaction.
  • the separation of noble metals proceeds through melting the noble metal-containing products in a metallurgical process.
  • the ceramic fraction is transferred in a slag phase and tapped, the noble metals are alloyed into a collector metal, which is then also tapped and processed further.
  • thermal reprocessing plants in particular ashing plants, comprise a thermal treatment chamber and an exhaust gas purification system.
  • the thermal treatment chamber is a component of a furnace and is provided with an insulating lining made, for example, of fireclay bricks or a ramming mass. These differ in composition.
  • all insulating linings comprise, inter alia, silicon dioxide SiO 2 (glass) and calcium oxide CaO. These components are attacked even by small amounts of the hydrofluoric acid and hydrogen fluoride that are generated and thus are dissolved out of the insulating lining which reduces the service life of the furnace and thus of the plant.
  • EP 1 478 042 A1 A method, in which the generation of HF is to be prevented, is disclosed in EP 1 478 042 A1.
  • components of fuel elements and catalysts are mixed with inorganic additives.
  • the hydrogen fluorides and other fluorine compounds are absorbed and chemically bound by the additive.
  • an up to 100-fold excess of the additive is added to the hydrogen fluoride gas that is being generated.
  • the absorption at the additive is insufficient or too slow in the case of materials releasing hydrogen fluoride already at low temperatures allowing some hydrogen fluoride gas to escape.
  • the additive occupies a fraction of the volume of the incineration space such that the quantity of material that can be processed is reduced.
  • the plant according to the invention shall allow all fluorine-containing products to be reprocessed, regardless of the volatility of the materials contained therein.
  • Another object of the present invention is to provide a method for enriching noble metals from fluorine-containing materials.
  • the exhaust gas cleaning system comprises at least one or more acid scrubber(s) ( 3 , 4 ) and at least one alkaline scrubber ( 5 ).
  • Another subject matter of the present invention is an ashing plant for enriching noble metals from fluorine-containing materials, comprising a thermal treatment chamber ( 1 ) having a refractory insulating lining on the inside of the thermal treatment chamber ( 1 ) and an exhaust gas cleaning system,
  • the exhaust gas cleaning system according to the invention preferably comprises at least one or more thermal after-incineration chambers ( 2 ).
  • the exhaust gas cleaning system comprises one after-incineration chamber ( 2 ).
  • FIG. 1 shows a schematic view of an ashing plant according to the invention.
  • the FIGURE shows a preferred embodiment that comprises two acid scrubbers ( 3 , 4 ).
  • the temperature on the inside of the thermal treatment chamber ( 1 ) usually is approx. 800° C.
  • the refractory insulating lining is designed to be stable at this continuous temperature. Moreover, it is also resistant to temperature peaks of up to approx. 2,000° C. It is feasible according to the invention to heat the thermal treatment chamber ( 1 ) directly or indirectly. All means of heating known according to the prior art are feasible, for example gas and oil heating or electrical heating.
  • Heating fluorine-containing materials in the thermal treatment chamber ( 1 ) in the ashing plant according to the invention produces exhaust gases that contain hydrogen fluoride gas. Since the thermal treatment chamber ( 1 ) is lined with the hydrofluoric acid-resistant insulating lining, the chamber is not attacked by the exhaust gases.
  • the exhaust gas cleaning system according to the invention the exhaust gas is initially subjected to thermal reprocessing in a thermal after-treatment chamber ( 2 ) and then all hydrogen fluoride gas or hydrofluoric acid already formed is removed in the acidic and alkaline scrubbing stages ( 3 , 4 , 5 ) such that the exhaust gases are then harmless and can be guided to the outside, for example by means of a chimney.
  • the ashing plant according to the invention can provide further cleaning stages or cleaning agents for exhaust gas cleaning in order to remove, for example, soot, chlorine or nitrous gases from the exhaust gases.
  • Pertinent cleaning agents or cleaning stages are described in the prior art.
  • the refractory insulating lining of the present invention can be a ramming mass.
  • Said ramming mass preferably has an aluminium oxide (Al 2 O 3 ) content of 85% by weight or more, in particular of 88% by weight or more.
  • Said insulating lining is stable at a working temperature and at a continuous temperature of approx. 800° C. However, it also withstands peak temperatures of up to approx. 2,000° C.
  • the thermal treatment chamber ( 1 ), the after-incineration chamber ( 2 ) and/or the exhaust gas conduit ( 6 ) further comprise an external lining.
  • the external lining can be provided using materials that are known according to the prior art.
  • the external lining is a mineral fibre.
  • the external insulation is surrounded by a steel plate. The steel plate fixes the external insulation in place and serves for stabilisation and shaping of the components of the ashing plant.
  • the effect of having the external insulation is that the temperature at the steel shell, i.e. at the external steel wall of the plant components, does not drop below 120° C.
  • the thickness of the external insulation is a function of the temperature profile on the inside of the corresponding component of the ashing plant. Condensation of hydrofluoric acid does not take place at a temperature of 120° C. Accordingly, if hydrogen fluoride gas were to diffuse through the refractory insulating lining towards the outside, no corrosion damage to load-bearing steel constructs is to be expected.
  • thermal treatment chamber ( 1 ), exhaust gas conduit ( 6 ), and after-incineration chamber ( 2 ) can differ.
  • thermal treatment chamber ( 1 ), exhaust gas conduit ( 6 ), and after-incineration chamber ( 2 ) can, for example, comprise an external insulation made of a mineral fibre at a thickness of approx. 10 cm.
  • the coolant for example water, flows between the external graphite wall and the external shell. This leads to indirect dissipation of heat from the exhaust gas via the scrubbing medium and the graphite walls.
  • the thickness of the graphite walls preferably is in the range of 3 cm to 4 cm. It has been evident that this thickness is sufficient to maintain sufficient temperature and acid stability.
  • the ashing plant of the present invention further comprises an alkaline scrubber ( 5 ).
  • the exhaust gases are guided from the at least one acid scrubber ( 3 , 4 ) into said alkaline scrubber after most or all of the hydrogen fluoride has been removed.
  • the alkaline scrubber ( 5 ) can comprise a coating on its inside that is resistant to alkaline scrubbing water and any traces of hydrogen fluoride gas that may still be present in the exhaust gas. Specifically, the coating is stable when exposed to bases having a pH of at least 10 or more, in particular of at least 11 or more.
  • the alkaline scrubber ( 5 ) comprises on its inside a coating made of a plastic material, in particular made of polypropylene.
  • the external shell of the alkaline scrubber can consist of steel.
  • the exhaust gas guided into the alkaline scrubber ( 5 ) is largely free of hydrogen fluoride gas. However, it cannot be excluded that some traces of hydrogen fluoride gas may still be present. If the alkaline scrubber ( 5 ) were lined with the otherwise common glass fibre-reinforced plastic materials (GFR), these residual amounts of hydrogen fluoride gas would be sufficient to attack and quickly etch away the glass fibres in the plastic material. The internal lining would have to be replaced after just a short time under these conditions.
  • the ashing plant according to the invention can further comprise a control unit.
  • the control unit controls the temperature profiles needed during the thermal treatment depending on the specific material and also controls the exhaust air line as a function of negative pressure, temperature, and oxygen content of the exhaust gas.
  • both continuous and discontinuous operation are feasible.
  • a discontinuous operation is preferred.
  • the present invention comprises a method for enriching noble metals from fluorine-containing materials, comprising a thermal treatment of the materials in a thermal treatment chamber ( 1 ) having a hydrofluoric acid-resistant refractory insulating lining and cleaning of the exhaust gases generated during the thermal treatment, whereby the cleaning comprises the following steps in the following order:
  • a noble metal-containing ash is generated during the thermal treatment of the noble metal-containing and fluorine-containing materials. Said ash is then reprocessed according to wet chemical methods known according to the prior art in order to recover the noble metals it contains.
  • noble metals are gold, silver, and the metals of the platinum group.
  • the exhaust gases generated during the thermal treatment are first subjected to thermal after-incineration in an after-incineration chamber ( 2 ), if applicable. Subsequently, the exhaust gases are washed with water or an acid in an acid scrubber. According to the invention, water is used as the scrubbing agent. Water washes hydrogen fluoride gas out of the exhaust gas. This produces an acid, which washes out more hydrogen fluoride gas such that, in the course of the entire scrubbing process, both water and an acid wash the exhaust gases.
  • the scrubbing water can have room temperature in this context. However, it is feasible just as well that the scrubbing water has a temperature that is slightly higher than room temperature. In this context, the temperature should not be more than 10 to 20° C. above ambient temperature.
  • scrubbing of the exhaust gases with water and/or an acid comprises two steps, namely
  • Hydrogen fluoride gas is removed from the exhaust gas by introducing water into the inside of the double-walled scrubber ( 3 ).
  • the exhaust gas is washed twice with water and/or an acid in a preferred embodiment and, for this purpose, is guided from the first double-walled graphite scrubber ( 3 ) into a second single-walled graphite scrubber ( 4 ).
  • the exhaust gas is washed with water and/or an acid in both scrubbers ( 3 , 4 ).
  • the initial scrubbing agent is water.
  • the water becomes acidified by the hydrogen fluoride gas washed out of the exhaust gas such that, overall, both water and an acid wash the exhaust gas at the respective stages. If the hydrogen fluoride gas is already removed completely from the exhaust gas in the first stage, the second stage entails a cleaning with water only.
  • step c the exhaust gas is neutralised and acidic components originating from step b) are removed.
  • a base with a pH of at least 10 or more, in particular of at least 11 or more, can be used as base in this context. It is preferred to use sodium hydroxide solution for scrubbing the exhaust gases in step c). Sodium hydroxide solution does not undergo any undesired reaction with the exhaust gas components. Moreover, it is inexpensive and easy to handle.
  • the method according to the invention is suitable preferably for the processing of materials that have a fluorine content of up to 5% by weight. It is preferred to use fluoro-organic materials, PTFE films, fuel cells, catalysts and/or pastes as materials to be subjected to the thermal treatment. As a matter of principle, the method is suitable for all materials having a fluorine content of up to 5% by weight that decompose at a temperature of approx. 800° C., in particular of approx. 600° C.
  • ashing plant of the type described above.
  • the ashing plant according to the invention is suitable for the use and implementation of the method according to the invention.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Sustainable Development (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Sustainable Energy (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Treating Waste Gases (AREA)
  • Gas Separation By Absorption (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Processing Of Solid Wastes (AREA)
US13/969,009 2012-08-21 2013-08-16 Device and Method for the Thermal Treatment of Fluorine-Containing and Noble Metal-Containing Products Abandoned US20140056786A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102012016420.3 2012-08-21
DE201210016420 DE102012016420A1 (de) 2012-08-21 2012-08-21 Vorrichtung und Verfahren zur thermischen Behandlung Fluor-und Edelmetallhaltiger Produkte

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US20140056786A1 true US20140056786A1 (en) 2014-02-27

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US (1) US20140056786A1 (zh)
EP (1) EP2700726B1 (zh)
JP (1) JP5714069B2 (zh)
KR (1) KR101548315B1 (zh)
CN (1) CN103695645A (zh)
AU (1) AU2013216667B2 (zh)
CA (1) CA2824003A1 (zh)
DE (1) DE102012016420A1 (zh)
TW (1) TW201408784A (zh)

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CN105675674B (zh) * 2016-01-13 2018-01-09 衢州学院 利用高温催化测定水体中有机氟浓度的方法
US20210362133A1 (en) * 2018-06-21 2021-11-25 Heraeus Deutschland GmbH & Co. KG Precious metal catalyst briquettes, process for the manufacture and for the inceneration thereof
CN113432432B (zh) * 2021-07-28 2023-08-25 周大福珠宝文化产业园(武汉)有限公司 一种电陶炉及其使用方法
EP4353372A1 (de) 2022-10-12 2024-04-17 Heraeus Precious Metals GmbH & Co. KG Verfahren zur veraschung fluor- und edelmetallhaltigen abfalls

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Also Published As

Publication number Publication date
JP2014040662A (ja) 2014-03-06
CA2824003A1 (en) 2014-02-21
KR20140024821A (ko) 2014-03-03
JP5714069B2 (ja) 2015-05-07
DE102012016420A1 (de) 2014-02-27
CN103695645A (zh) 2014-04-02
TW201408784A (zh) 2014-03-01
EP2700726A1 (de) 2014-02-26
AU2013216667B2 (en) 2015-04-30
EP2700726B1 (de) 2015-08-19
KR101548315B1 (ko) 2015-08-31
AU2013216667A1 (en) 2014-03-13

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