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WO1998008989A1 - Procede d'oxydation par micro-onde d'un minerai sulfure dans un lit fluidise, sans emission de dioxyde de soufre - Google Patents

Procede d'oxydation par micro-onde d'un minerai sulfure dans un lit fluidise, sans emission de dioxyde de soufre Download PDF

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Publication number
WO1998008989A1
WO1998008989A1 PCT/CA1997/000561 CA9700561W WO9808989A1 WO 1998008989 A1 WO1998008989 A1 WO 1998008989A1 CA 9700561 W CA9700561 W CA 9700561W WO 9808989 A1 WO9808989 A1 WO 9808989A1
Authority
WO
WIPO (PCT)
Prior art keywords
reaction
bed
reactor
temperature
fluidizing
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/CA1997/000561
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English (en)
Inventor
James M. Tranquilla
Paul R. Kruesi
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.)
EMR Microwave Technology Corp
Original Assignee
EMR Microwave Technology Corp
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 EMR Microwave Technology Corp filed Critical EMR Microwave Technology Corp
Priority to CA002263497A priority Critical patent/CA2263497A1/fr
Priority to EP97935397A priority patent/EP0950122A1/fr
Priority to AU38439/97A priority patent/AU721221B2/en
Publication of WO1998008989A1 publication Critical patent/WO1998008989A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • 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
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/02—Roasting 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
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/02—Roasting processes
    • C22B1/10—Roasting processes in fluidised form
    • 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
    • C22B15/00—Obtaining copper
    • C22B15/0002—Preliminary treatment
    • C22B15/001—Preliminary treatment with modification of the copper constituent
    • C22B15/0013—Preliminary treatment with modification of the copper constituent by roasting
    • C22B15/0015—Oxidizing roasting
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008—Controlling the process
    • B01J2208/00017—Controlling the temperature
    • B01J2208/00026—Controlling or regulating the heat exchange system
    • B01J2208/00035—Controlling or regulating the heat exchange system involving measured parameters
    • B01J2208/00044—Temperature measurement

Definitions

  • This invention relates to a microwave fluidized bed reactor which is used to oxidize pyritic ores by controlling microwave power density, oxygen concentration and fluidizing gas flow in such a way as to prevent oxidation of the sulphur into gaseous sulphur dioxide.
  • Pyrometallurgical recovery involves heating the ore mass and in the process decomposing the sulphide through oxidation resulting in the formation of sulphur dioxide gas.
  • Hydrometallurgical recovery on the other hand involves the dissolution of the ore constituents in a liquid medium in which one or more chemical reactions can be initiated which will cause the important metals to form a new, recoverable compound.
  • Pyrometallurgical recovery is unsatisfactory today because of the formation of sulphur dioxide gas in the so-called roaster oxidation reaction. Accordingly, this technique has largely been abandoned due to legislation restricting sulphur dioxide emissions.
  • Hydrometallurgical recovery is also an unsatisfactory process because metal recovery is hindered and, in many cases, rendered practically useless in the presence of sulphidic compounds.
  • reaction (I) pyrite (FeS 2 ) is decomposed into pyrrhotite (FeS) and elemental sulphur (S).
  • the associated reactions (II) and (III) include the oxidation of pyrrhotite to form hematite and sulphur dioxide, and of sulphur to form sulphur dioxide.
  • These reactions are highly exothermic, hence it is not possible in conventional roasting reactors to prevent the temperature from increasing to the point where SO 2 is produced. In fact, in conventional roaster operation, this exothermic energy is necessary to provide the reaction energy needed to cause (I) to occur.
  • This reaction when augmented by steam and oxygen, may be used as a means of producing high quality SO 2 as a desired product, as disclosed by Jukkola in United States Patent No. 3,632,312.
  • reaction (IV) in order for reaction (IV) to be favored and to avoid the entire roaster reaction (I-HI), the operating temperature must be maintained below approximately 1000°K (727°C). Further, in order to avoid the reaction (V) the temperature must be maintained below approximately 800°K (527°C)
  • the most strongly favored pyrite reaction is the one which produces hematite (Fe ⁇ ) and SO 2 shown as the lowermost curve in Figure 4 from data in Table 3.
  • oxygen must be restricted to allow the production of elemental sulphur (central curve in Figure 4). Accordingly, to limit SO 2 production, the preferred operating temperature is below 527°C where the reaction products of pyrite and oxygen are restricted to hematite and sulphur as described in reaction (IV).
  • the ability to maintain the otherwise highly exothermic oxidation reaction temperature below 527 °C requires separate control of: (1) the oxygen supplied to the reaction; (2) the power (energy) introduced into the material; and (3) the gas flow through the reaction environment (coolant). Control of the aforesaid factors can be achieved, in association with the present invention, using a fluidized bed reactor with power supplied by microwave energy, for treating pyritic mineral ore.
  • Fluidized bed reactors are presently widely used in many ore processing applications where strong interaction between a solid product and gas medium is required and the use of microwave energy to provide some or all of the required reaction energy has been disclosed in, for example, U.S. Patents Nos. 3,528,179; 4,126,945; 4,967,486; 4,511,362; 4,476,098; 5,382,412 and 5,051 ,456.
  • a fluidized bed reactor with a microwave source of power provides the ability to control the oxygen supply to the material undergoing treatment (which governs the rate of reaction and hence reaction temperature) independently of the microwave power (which supplies the energy to initiate the chemical reaction and compensates for other energy losses).
  • the use of microwave energy also provided the unique ability to selectively heat certain materials in the presence of less absorptive gangue materials as is the case with pyritic ores.
  • the exhaust stream from the reactor is depleted of oxygen as a consequence of the oxidation reaction with the fluidized bed and consists principally of nitrogen. It has been found that by diverting and preferably cooling the exhaust stream and reintroducing it into the reactor with the fluidizing stream that it is effective as a coolant and thus provides the final factor required to achieve the preferred chemical reaction to process pyrite minerals under temperature conditions that provide reaction products that are free of SO 2 emissions.
  • the invention comprises a method of oxidizing pyritic ores using a reaction vessel.
  • the method comprises the steps of: (a) fluidizing a bed of pyritic ore in said reactor using a fluidizing gas; (b) heating said bed of ore with microwave energy to initiate an exothermic oxidation reaction in the bed; and (c) cooling the temperature of the reaction in said bed to a temperature at which the preferred reaction products are hematite and elemental sulphur.
  • the invention also comprises a method of oxidizing pyritic ores using a fluidizing bed reactor.
  • the method comprises the steps of: (a) heating a bed of pyritic ore with microwave energy to initiate an exothermic oxidation reaction within the bed; (b) controlling the inflow of oxygen to the reaction in the reaction chamber; and (c) cooling the temperature of the reaction in said bed to a temperature at which the reaction products are hematite and elemental sulphur, while continuing to supply said bed with microwave energy to selectively heat the pyrite in the presence of magnetite and hematite.
  • the invention still further comprises a method for the oxidization of pyritic ores, without the production of SO 2 as a by product, using a fluidized bed reactor powered by microwave energy.
  • the method comprises the steps of: (a) isolating the vent gases from the reactor when in operation; (b) cooling the said vent gases; and (c) re-introducing the vent gases into the fluidization gases in the reactor to cool the internal reaction temperature.
  • FIGURE 1 is a cross sectional view of a fluidized bed reactor of the present invention
  • FIGURE 2 is a graph showing thermodynamic stability data of Table
  • FIGURE 3 is a graph showing thermodynamic stability data of Table
  • FIGURE 4 is a graph showing the Gibbs Free Energy for various pyrite reactions from data of Table 3.
  • a reactor vessel such as a fluidized bed reactor 10, comprises a tubular waveguide resonator reaction chamber or cavity 12, bed fluidizer screen 14, and a pressure chamber 16.
  • the reaction chamber 12 is connected to a microwave energy source via waveguide fittings 18 and 20 which may include a coupling iris (not shown) as well as a pressurized gas seal 22.
  • the reaction chamber 12 has a material inlet valve 24, material exit valve 26, gas inlet valve 28 and a gas exhaust port 30. Exhaust port 30 is connected to pipe 40 which is in turn connected to particulate separator 42 (which may be a cyclonic separator), and a first control valve 44.
  • Control valve 44 is connected by pipe 41 to heat exchanger 46 and second control valve 48, which is connected by pipe 43 to the gas inlet valve 28.
  • Pipe 40 has a gas exit port temperature monitor 50 and an SO 2 sensor 52.
  • Solid material to be processed is introduced through the inlet valve and is to be fluidized by gas 32 which is supplied from an external source through pipe 43 to control valve 48 and the gas inlet valve 28.
  • gas 32 which is supplied from an external source through pipe 43 to control valve 48 and the gas inlet valve 28.
  • the introduction of gas will cause the material which has been introduced through the inlet valve to form a fluidized bed 34 which is suspended through the adjustment of the gas pressure in the pressure chamber 16 and the bed fluidizer screen 14.
  • the fluidized bed is then ready for treatment with microwave energy which is introduced into the reaction chamber from the top via the waveguide fittings.
  • the bed is in a fluidized state, the solid material is heated by the dielectric and resistive effects caused by interaction between the electromagnetic field and the solid material constituents.
  • the fluidizing gas will be continuously pumped through valve 28 and exhausted through port 30 during the treatment process.
  • the exhaust stream will be passed through particulate separator 42 to clean the gas of particulate matter (either fines blown free from the fluidized bed or sulphur powder produced from the reaction).
  • the stream will then pass through control valve 44 by which some or all of the exhaust stream, which will be depleted of O 2 and consist primarily of N 2 , can be recirculated back to the chamber after being passed through heat exchanger 46 and second control valve 48.
  • Second control valve 48 allows the exhaust gas to be mixed with fresh air, or gases (if required), to provide the fluidizing stream and act as a coolant for the reaction chamber to achieve the preferred chemical reaction to process pyrite minerals under temperature conditions that provide reaction products that are free of SO 2 emissions.
  • the region 36 above the suspended fluidized bed 34 is generally essentially free of solid material and consists primarily of fluidized gas and gaseous reaction products.
  • the gas seal 22 permits the transmission of microwave energy into the reaction chamber 12 while isolating the atmosphere and contents of the chamber from the connecting waveguide attached via fittings 18 and 20.
  • the pyritic ore is loaded into the reaction chamber 12 through valve 24.
  • the ore is then fluidized into the bed 34 by pumping a fluidizing gas, which is generally just air, through valve 28.
  • microwave energy is applied, via the waveguide fitting.
  • the microwave energy raises the fluidized bed to the preferred operating temperature in the range of about 300 C C - 550 °C, where as can be seen from the data of Table 1 and shown in Figure 2, pyrite is preferred over pyrrhotite. Additionally, as can be seen in Table 2 and Figure 3, recombination of hematite and sulphur (reaction (IV)) is not favoured at temperatures below 550°C.
  • the sulphur-hematite reaction commences. If the temperature rises too quickly (i.e. the N 2 in the vent gasses is not yet sufficient to restrict the amount of O 2 and thus cool the reaction), N 2 can be introduced into the fluidizing stream via valve 48. The reaction can be monitored by checking the particulate separator 42, which will reveal the presence of sulphur, an indicator of the reaction, or by a temperature spike from temperature probe 50 since the initial pyrite reaction is exothermic.
  • the reaction can be cooled by reducing the input of microwave energy; although, as will be discussed below, it is preferable to maintain at least some input of microwave energy, in the range of 0.5kw.
  • the second control of the reaction temperature is through the manipulation of the recirculating gases which, due to the reaction in the chamber, has been reduced to primarily N 2 . If the reaction has not sufficiently reduced the O 2 from the circulating gases, additional inert gasses can be introduced into the stream to control the amount of O in the reactor. Additionally, the recirculating gases themselves can be cooled prior to reintroduction into the reaction chamber.
  • Pyrite can be selectively heated while in the presence of magnetite and hematite since it absorbs microwave energy more efficiently. Accordingly, it may be treated by the continued application of microwave energy during the exothermic reaction which is ongoing in the reaction chamber while at the same time the mass of the bed is being cooled by the recirculating gas stream.
  • reaction chamber 12 can be of any appropriate dimension or geometry as dictated by the microwave field distribution. Additionally, while being described as an iris coupled resonator, the reaction chamber may operate as a terminated waveguide (iris fully open) in which case the absorptive action of the load material gives the reactor the characteristics of a travelling-wave applicator.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Geology (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

La présente invention concerne un procédé de traitement de minéraux de pyrite par l'utilisation d'un réacteur de fluidisation alimenté par énergie micro-onde, à des conditions de température qui permettent d'obtenir des produits de réaction relativement exempts d'émissions de SO2. Les conditions de température contrôlées auxquelles les produits de réaction deviennent hématite ou soufre élémentaire peuvent être obtenues par recyclage et refroidissement d'une partie du gaz de fluidisation sortant et par régulation de l'énergie micro-onde qui alimente le lit fluidisé.
PCT/CA1997/000561 1996-08-27 1997-08-08 Procede d'oxydation par micro-onde d'un minerai sulfure dans un lit fluidise, sans emission de dioxyde de soufre Ceased WO1998008989A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
CA002263497A CA2263497A1 (fr) 1996-08-27 1997-08-08 Procede d'oxydation par micro-onde d'un minerai sulfure dans un lit fluidise, sans emission de dioxyde de soufre
EP97935397A EP0950122A1 (fr) 1996-08-27 1997-08-08 Procede d'oxydation par micro-onde d'un minerai sulfure dans un lit fluidise, sans emission de dioxyde de soufre
AU38439/97A AU721221B2 (en) 1996-08-27 1997-08-08 Method for microwave induced oxidation of sulphidic ore material in fluidized bed without sulphur dioxide emissions

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US70370396A 1996-08-27 1996-08-27
US08/703,703 1996-08-27
US89710397A 1997-07-18 1997-07-18
US08/897,103 1997-07-18

Publications (1)

Publication Number Publication Date
WO1998008989A1 true WO1998008989A1 (fr) 1998-03-05

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PCT/CA1997/000561 Ceased WO1998008989A1 (fr) 1996-08-27 1997-08-08 Procede d'oxydation par micro-onde d'un minerai sulfure dans un lit fluidise, sans emission de dioxyde de soufre

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EP (1) EP0950122A1 (fr)
AU (1) AU721221B2 (fr)
CA (1) CA2263497A1 (fr)
WO (1) WO1998008989A1 (fr)

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1999036582A1 (fr) * 1998-01-16 1999-07-22 Emr Microwave Technology Corporation Procede d'oxydation par micro-ondes de minerais sulfures et de concentres de minerais sans production d'anhydride sulfureux
AT408992B (de) * 2000-06-28 2002-04-25 Voest Alpine Ind Anlagen Verfahren zur direktreduktion von feinerz sowie anlage zur durchführung des verfahrens
RU2224805C1 (ru) * 2002-06-20 2004-02-27 Швецов Владимир Алексеевич Способ предварительного обжига сульфидных руд и продуктов их переработки, содержащих золото и серебро, в пробирном анализе
WO2004056471A1 (fr) * 2002-12-23 2004-07-08 Outokumpu Technology Oy Procede et equipement pour le traitement thermique de solides granulaires dans un lit fluidise
WO2004056472A1 (fr) * 2002-12-23 2004-07-08 Outokumpu Technology Oy Procede et plante pour le traitement thermique de solides granulaires
US7625422B2 (en) 2002-12-23 2009-12-01 Outotec Oyj Method and plant for the heat treatment of solids containing iron oxide using a fluidized bed reactor
US7632334B2 (en) 2002-12-23 2009-12-15 Outotec Oyj Method and plant for the heat treatment of solids containing iron oxide
WO2011151294A1 (fr) * 2010-06-01 2011-12-08 Outotec Oyj Procédé et installation pour la réduction de la teneur en carbone résiduel de cendres
FR3136541A1 (fr) * 2022-06-14 2023-12-15 Innovation & Development Company four de calcination par micro-ondes et à lit fluidisé

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4324582A (en) * 1980-06-11 1982-04-13 Kruesi Paul R Process for the recovery of copper from its ores
US4678478A (en) * 1986-04-14 1987-07-07 Massachusetts Institute Of Technology Method for desulfurization of coal
JPS63289496A (ja) * 1987-05-21 1988-11-25 Power Reactor & Nuclear Fuel Dev Corp 流動床システム
US5123956A (en) * 1991-04-12 1992-06-23 Newmont Mining Corporation Process for treating ore having recoverable gold values and including arsenic-, carbon- and sulfur-containing components by roasting in an oxygen-enriched gaseous atmosphere
JPH067132A (ja) * 1992-06-23 1994-01-18 Osaka Gas Eng Kk 粒状処理物の焙煎方法とその装置
DE4329417C1 (de) * 1993-09-01 1994-08-18 Metallgesellschaft Ag Verfahren zum Rösten refraktärer Golderze

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2209331A (en) * 1936-11-12 1940-07-30 Haglund Ture Robert Roasting process

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4324582A (en) * 1980-06-11 1982-04-13 Kruesi Paul R Process for the recovery of copper from its ores
US4678478A (en) * 1986-04-14 1987-07-07 Massachusetts Institute Of Technology Method for desulfurization of coal
JPS63289496A (ja) * 1987-05-21 1988-11-25 Power Reactor & Nuclear Fuel Dev Corp 流動床システム
US5123956A (en) * 1991-04-12 1992-06-23 Newmont Mining Corporation Process for treating ore having recoverable gold values and including arsenic-, carbon- and sulfur-containing components by roasting in an oxygen-enriched gaseous atmosphere
JPH067132A (ja) * 1992-06-23 1994-01-18 Osaka Gas Eng Kk 粒状処理物の焙煎方法とその装置
DE4329417C1 (de) * 1993-09-01 1994-08-18 Metallgesellschaft Ag Verfahren zum Rösten refraktärer Golderze

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
PATENT ABSTRACTS OF JAPAN vol. 013, no. 112 (P - 844) 17 March 1989 (1989-03-17) *
PATENT ABSTRACTS OF JAPAN vol. 018, no. 204 (C - 1189) 11 April 1994 (1994-04-11) *

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1999036582A1 (fr) * 1998-01-16 1999-07-22 Emr Microwave Technology Corporation Procede d'oxydation par micro-ondes de minerais sulfures et de concentres de minerais sans production d'anhydride sulfureux
AT408992B (de) * 2000-06-28 2002-04-25 Voest Alpine Ind Anlagen Verfahren zur direktreduktion von feinerz sowie anlage zur durchführung des verfahrens
RU2224805C1 (ru) * 2002-06-20 2004-02-27 Швецов Владимир Алексеевич Способ предварительного обжига сульфидных руд и продуктов их переработки, содержащих золото и серебро, в пробирном анализе
WO2004056471A1 (fr) * 2002-12-23 2004-07-08 Outokumpu Technology Oy Procede et equipement pour le traitement thermique de solides granulaires dans un lit fluidise
WO2004056472A1 (fr) * 2002-12-23 2004-07-08 Outokumpu Technology Oy Procede et plante pour le traitement thermique de solides granulaires
US7625422B2 (en) 2002-12-23 2009-12-01 Outotec Oyj Method and plant for the heat treatment of solids containing iron oxide using a fluidized bed reactor
US7632334B2 (en) 2002-12-23 2009-12-15 Outotec Oyj Method and plant for the heat treatment of solids containing iron oxide
US8021600B2 (en) 2002-12-23 2011-09-20 Outotec Oyj Method and plant for the heat treatment of solids containing iron oxide
WO2011151294A1 (fr) * 2010-06-01 2011-12-08 Outotec Oyj Procédé et installation pour la réduction de la teneur en carbone résiduel de cendres
AU2011260345B2 (en) * 2010-06-01 2014-03-13 Outotec Oyj Process and plant for lowering the residual carbon content of ash
US8876969B2 (en) 2010-06-01 2014-11-04 Outotec Oyj Process and plant for lowering the residual carbon content of ash
EA025146B1 (ru) * 2010-06-01 2016-11-30 Ототек Оюй Способ и установка для снижения остаточного содержания углерода в золе
FR3136541A1 (fr) * 2022-06-14 2023-12-15 Innovation & Development Company four de calcination par micro-ondes et à lit fluidisé

Also Published As

Publication number Publication date
AU3843997A (en) 1998-03-19
CA2263497A1 (fr) 1998-03-05
AU721221B2 (en) 2000-06-29
EP0950122A1 (fr) 1999-10-20

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