US3656888A - Liquid phase oxidation process - Google Patents
Liquid phase oxidation process Download PDFInfo
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- US3656888A US3656888A US863197A US3656888DA US3656888A US 3656888 A US3656888 A US 3656888A US 863197 A US863197 A US 863197A US 3656888D A US3656888D A US 3656888DA US 3656888 A US3656888 A US 3656888A
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- 238000007254 oxidation reaction Methods 0.000 title abstract description 24
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- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 60
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- 238000006243 chemical reaction Methods 0.000 abstract description 45
- 229910000476 molybdenum oxide Inorganic materials 0.000 abstract description 19
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- 229910052782 aluminium Inorganic materials 0.000 description 1
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- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/02—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Definitions
- LIQUID PHASE OXIDATION PROCESS [72] Inventors: Henry F. Barry; Calvin J. Hallada, both of Ann Arbor; Robert W. McConnell, South Lyon, all of Mich.
- ABSTRACT A process for effecting an aqueous liquid phase oxidation of molybdenum disulfide to molybdenum oxide by agitating, at elevated temperature, a slurry of molybdenum disulfide particles in water, under pressure, in the presence of oxygen for a period of time sufficient to effect the conversion of at least a portion of the molybdenum disulfide to molybdenum oxide,
- Such ore beneficiaation processes conventionally comprise a grinding operation by which the ore is reduced to a particle size usually less than about 200 mesh and wherein the particles are subjected to a flotation extraction operation using a hydrocarbon oil, such as pine oil or petroleum oil, in combination with wetting agents to effect a separation of the molybdenum disulfide constituent from the gangue.
- a hydrocarbon oil such as pine oil or petroleum oil
- molybdenum disulfide While some of the molybdenum disulfide, after further purification, is employed directly in the compounding of lubricants, the predominant portion is converted to the oxide form in which it is employed as an alloying constituent in various metal alloys or is further reduced from the oxide form to the pure metallic state for special uses.
- the present invention provides for an improved oxidation process for effecting a conversion of molybdenum disulfide to the corresponding oxide whereby the sulfur by-product constituent can be recovered as a sulfate and the molybdenum constituent is recovered as the trioxide.
- this improved process it is now economically feasible to effect a liquid phase oxidation of molybdenum disulfide to provide molybdenum trioxide of high purity and in commercially acceptable yields.
- aqueous slurry consisting of finely particulated particles containing molybdenum disulfide dispersed in water which is heated to a temperature preferably in excess of about 80 C. under an atmosphere containing free oxygen at an oxygen partial pressure of preferably at least about 50 psi.
- the slurry is subjected to agitation sufficient to maintain a substantially uniformdispersion of the particles through the aqueous medium and to further effect entrainment and dissolving of the free oxygen in the aqueous medium for reaction with the surfaces of the molybdenum disulfide particles.
- reaction progresses, sulfur oxides are formed, which in turn form sulfuric acid that effect a progressive reduction in the pH of the reaction medium as the reaction continues.
- the reaction is continued for a period of time, normally about one to six hours, depending on the specific temperature-pressureparticle size conditions employed, whereafter the molybdenum trioxide product can be separated from the acidic aqueous medium, such as by filtration.
- the extracted solids it is usually preferred to subject the extracted solids to a wash with ammonium hydroxide, effecting a conversion of the molybdenum oxide to ammonium molybdate and leaving a solid residue consisting of unreacted molybdenum disulfide and other insoluble impurities such as the gangue.
- the solid residue if desired, can be subjected to further liquid phase oxidation to effect conversion of the balance of the molybdenum disulfide to molybdenum oxide.
- the resultant ammonium molybdate solution can be concentrated, such as in an evaporator, and the crystals can thereafter be subjected to calcination, providing a relatively pure grade of molybdenum trioxide.
- the drawing comprises a diagrammatic flow sheet of the process for effecting a liquid phase oxidation of molybdenum disulfide to molybdenum oxide in accordance with the preferred embodiments of the present invention.
- the molybdenum disulfide starting material may comprise a concentrate as derived from flotation extraction operations in which molybdenum disulfide is usually present in amounts in excess of percent by weight and is in the form of finely divided particles of a size usually less than 200 mesh.
- Concentrates of the foregoing type derived directly from the ore beneficiaation process are in the form of wet oily masses which usually contain up to about 5 percent water and up to about 7 percent of the hydrocarbon flotation oils employed in the flotation extraction operation.
- Such concentrates ordinarily require no pretreatment prior to oxidation in accordance with the practice of the present invention, although in some situations, it has been found advantageous to remove the predominant portion of the flotation oils to provide for increased efiiciency in the oxidation reaction. This is particularly true when only a single-pass liquid phase oxidation reaction is employed.
- the removal of the flotation oils or a reduction in the quantity thereof can be achieved, for example, by retorting the concentrate, efiecting a volatilization and/or thermal degradation and decomposition of the oils, providing a resultant substantially dry concentrate usually containing less than about 0.5 percent oil and, more usually, less than about 0. 1 percent.
- the retorting operation is conventionally carried out at a temperature of about 1,200 F which also effects a corresponding reduction in the water content of the concentrate.
- the concentrate can be subjected to solvent washing for removing the flotation oils followed by filtration to recover the de-oiled molybdenite.
- molybdenite concentrates consist predominantly of molybdenum disulfide, about 5 percent to about 10 percent silica is also normally present.
- Other metals are also present in minimal quantities such as lead, copper, zinc, iron, aluminum, calcium, magnesium, etc.
- the presence of such contaminating metals, which are present in amounts of less than 1 percent, does not detract from the efficiency of the liquid phase oxidation process comprising the present invention.
- the concentrate can be subjected to further leaching so as to effect an extraction of one or more of such metals with any one of a variety of techniques well known in the art.
- the concentrate as derived from the mine, or as derived after further pretreatment is of an average particle size of less than about 200 mesh and can be employed directly in forming an aqueous dispersion without further comminution. While particle sizes of less than about 200 mesh are satisfactory for the practice of the process of the present invention, it is generally preferred that the concentrate have an average particle size of less than about 20 microns, and preferably less than about 5 microns, due to the increased surface area which further promotes the efiiciency of the oxidation reaction. Particles of such smaller size also facilitate the formation and maintenance of a substantially uniform aqueous dispersion and are usually preferred for this purpose.
- the molybdenum disulfide concentrate is discharged from a storage hopper 2 into a dispersion tank 4 provided with an agitator 6 for effecting the formation of an aqueous dispersion or slurry which is intermittently or continuously transferred by means of a pump 8 into the inlet side of an autoclave 10.
- a dispersion tank 4 provided with an agitator 6 for effecting the formation of an aqueous dispersion or slurry which is intermittently or continuously transferred by means of a pump 8 into the inlet side of an autoclave 10.
- slurries which contain up to about 40 percent by weight of molybdenum disulfide based on the total weight of the slurry can be formed.
- the liquid phase oxidation in the autoclave 10 can be carried out batchwise and also, preferably, in a continuous manner as shown.
- batch operations it is convenient to form the dispersion directly in the autoclave, while in continuous operation, it is preferred to form the dispersion exteriorly of the autoclave employing a dispersion tank 4, as shown in the drawing, from which the slurry is continuously added to the inlet side of the autoclave and passes in a serpentine manner, as provided by the baffles 12, to the outlet side thereof.
- the autoclave 10 is further provided with an agitator 14 of the mechanical mixing type for maintaining a substantially uniform dispersion of the particles in the aqueous medium.
- agitation devices can be satisfactorily employed in lieu of the mechanical propellertype agitator 14, illustrated in the drawing, including, for example, sparger-type agitators through which the free oxygencontaining gas is admitted under pressure into the autoclave in the form of a stream of bubbles, imparting turbulence to the aqueous medium, as well as effecting a contact of the free oxygen with the surfaces of the molybdenum disulfide particles.
- the provision of free oxygen in the autoclave 10 can be accomplished by introducing pure oxygen gas through a supply line 16 or, alternatively, can be provided by air or a mixture of the two. Additional free oxygen is continuously or intermittently supplied to the autoclave to replenish that consumed during the oxidation reaction. When air is employed as the source of free oxygen replenishment, it is preferred to provide a vent line 18 in the upper portion of the autoclave for continuously and/or intermittently withdrawing gas from the upper portion of the autoclave to avoid the formation of an atmosphere which is excessively rich in nitrogen.
- oxygen partial pressures at or about atmospheric pressure At oxygen pressures at or about atmospheric pressure, the oxidation reaction has been observed to be very slow and totally impractical from a commercial standpoint. It has been discovered that as the partial pressure of the free oxygen is increased to above about 50 p.s.i., a marked improvement in the rate of reaction and in the product yield takes place. Particularly satisfactory results are attained employing oxygen partial pressures of from about 300 p.s.i. up to about 600 p.s.i. or above. While oxygen partial pressures in excess of about 600 p.s.i. have been found to provide for further improvements in the reaction rate, the increases in reaction rate at these higher levels become progressively smaller and are not significantly greater than that attained at pressures at or about 600 p.s.i. Additionally, oxygen partial pressures in excess of about 600 p.s.i. require that the processing equipment employed be of substantially greater structural strength, and it is because of the foregoing considerations that the use of such higher pressures is not ordinarily economically justified.
- the liquid phase reaction medium preferably comprises an aqueous dispersion containing from about 10 percent up to about 30 percent by weight of molybdenum disulfide particles of an average particle size of less than about 200 mesh which is vigorously agitated at a temperature preferably ranging from about l50 C. to about 250 C. in contact with free oxygen present at a partial pressure of from about 300 p.s.i. to about 600 p.s.i.
- substantially complete reaction and conversion of the molybdenum disulfide to the corresponding oxide takes place within about one to about six hours.
- the acid aqueous slurry is withdrawn from the autoclave and is transferred, as shown in the drawing, to a filter 20 for effecting a separation of the molybdenum trioxide reaction product from the filtrate.
- the filter cake also contains unreacted molybdenum disulfide particles and any other solid contaminating material such as the gangue present in the original concentrate which is predominantly in the form of silica.
- the aqueous filtrate which is acidic due to the presence of the sulfuric acid formed during the oxidation reaction also contains some dissolved molybdenum in the form of molybdenyl sulfate.
- the acidity of the filtrate conventionally ranges from a pH of about 0 to a pH of about 2.0, depending upon the concentration of molybdenum disulfide in the original slurry charge and the extent to which the conversion reaction has taken place.
- the filtrate discharged from the filter 20 is preferably transferred, as shown in the drawing, to a neutralizer 22 in which an alkaline compound, such as caustic, is added and causes precipitation of the dissolved molybdenum trioxide.
- the precipitated molybdenum oxide can be recovered in a flter 24.
- the neutralized filtrate from the filter 24 can be suitably discharged to storage and subsequently utilized as a source of sulfate.
- a portion of the filtrate from the filter 20 can be recycled back to the autoclave or to the tank 4 used for preparing the slurry prior to charging the autoclave.
- the recycling of such acidic filtrate causes the initial slurry charge to be slightly on the acid side, resulting in an increased acidity of the reacted slurry as withdrawn at the output end of the autoclave. For this reason, while a recycling of a portion of the filtrate from the filter can be accomplished, generally the quantity recycled is small.
- all of the filtrate is directly transferred to the neutralizer 22.
- the filter cake derived from the filter 20 consists of a precipitated molybdenum trioxide product in combination with unreacted molybdenum disulfide and a small proportion of inert contaminants, such as silica, originally introduced with the molybdenum disulfide concentrate.
- An extraction of the molybdenum trioxide product from the filter cake is conveniently achieved by transferring the filter cake to a wash treatment 26, in which it is subject to an aqueous ammonium hydroxide wash solution prepared in a make-up tank 28.
- the aqueous ammonium hydroxide wash solution may range in concentration from about 1 to about 12 normal (N), and preferably, concentrations of about 10 to 12 N are used in order to minimize water dilution of the resultant molybdate solution.
- the quantity of wash solution employed is designed to provide a molar ratio of ammonia to molybdenum of preferably at least 2.3 up to about 3.0.
- the wash solution effects a dissolving of the molybdenum oxide by converting it to ammonium molybdate.
- the unreacted molybdenum disulfide and solid contaminants are thereafter removed in a filter and the filtrate containing the dissolved ammonium molybdate can be concentrated, such as by evaporation or in a crystalizer 32, as shown in the drawing.
- the solid ammonium molybdate derived from the crystalizer can be employed as a product in that form or, alternatively, can be transferred to a calciner 34 in which it is heated, effecting an evolution of ammonium gas which is recycled back to the ammonium hydroxide make-up tank 28.
- the resultant molybdenum trioxide product is of high purity.
- the filter cake derived from the filter 30 containing unreacted molybdenum disulfide in combination with inert contaminants is preferably accumulated and thereafter charged to a second autoclave 36 in which an aqueous slurry is formed and a further oxidation reaction is carried out in accordance with the reaction as previously described in connection with the autoclave It).
- the autoclave 36 similarly is provided with appropriate agitation and means for introducing oxygen under pressure to effect a conversion of the residual molybdenum disulfide to the corresponding oxide with a formation of sulfuric acid in accordance with the reaction equation as hereinbefore set forth.
- the reacted slurry is transferred from the autoclave 36 to a filter 38 in which the precipitated molybdenum trioxide particles are removed in combination with the contaminating inert particles along with any residual unreacted molybdenum disulfide.
- the filtrate from the filter 38 may conveniently be transferred to the neutralizer 22 at which it is treated with caustic in a manner as previously described.
- the resultant filter cake from the filter 38 similarly is washed with an aqueous ammonium hydroxide solution, effecting a dissolving of the molybdenum trioxide product in a treating tank 40, whereafter it is transferred to a filter 42 for removal of the undissolved solids which comprise essential inert contaminating materials originally present in the molybdenum disulfide concentrate.
- the filtrate from the filter 42 is conveniently transferred and is mixed with the filtrate from the filter 30 for further concentration in the crystalizer 32 in a manner as previously described.
- the efficiency of conversion can be further improved by employing a multiple-phase reaction as exemplified by the continuous autoclave 10 and wherein any residual unreacted molybdenum disulfide is subsequently substantially completely converted to the oxide form using an auxiliary autoclave 36.
- EXAMPLE 1 A regular grade molybdenum disulfide concentrate derived from an oil flotation extracted molybdenite ore from Climax, Colo., having an average particle size of less than 200 mesh was employed for the liquid phase oxidation reaction. The concentrate was washed 6 times with acetone to remove the residual oils and was thereafter dried for several hours at a temperature of C. The chemical analysis of the de-oiled concentrate revealed that it contained 52.44 percent molybdenum and 35.54 percent sulfur with a sulfur to molybdenum mole ratio of 2.03:1.
- a l-liter capacity autoclave equipped with a magnetically driven agitator was employed for the liquid phase oxidation reaction.
- a slurry was prepared by mixing 50 grams of the molybdenum disulfide concentrate with 450 grams of water and charging the resultant slurry into the autoclave.
- the autoclave was pressurized with oxygen and thereafter heated, during agitation, to the operating temperature. Heating was continued to provide a substantially constant operating temperature of about 177 C. (350 F.) with a total vapor pressure of 750 p.s.i. gauge of which the calculated oxygen partial pressure was about 615 p.s.i.
- the charge was cooled and filtered through a Buchner funnel and the filter cake was dried for several hours at 110 C.
- the filtrate, at the completion of the reaction, was at a pH of less than zero.
- Thirty grams of the dry filter cake thereafter was stirred with 250 milliliters of 5 N ammonium hydroxide for 30 minutes at room temperature, effecting a dissolving of the molybdenum oxide and the charge was thereafter filtered and the residue again dried at 1 10 C. and weighed.
- the yield of molybdenum oxide was calculated based on the original filter cake recovered and the weight loss of the ammonium hydroxide-washed filter cake which revealed a conversion of about 88.4 percent of the molybdenum disulfide to molybdenum trioxide.
- EXAMPLE II A second test was conducted employing the same concentrate and equipment as previously described in connection with Example I. The same procedure utilizing the same temperature and reaction conditions, but a total pressure of 350 p.s.i.g., was used, providing a calculated oxygen partial pressure of 215 p.s.i. The resultant filtrate had a pH of 0.12 and an analysis of the reaction residue revealed a conversion of molybdenum disulfide to molybdenum trioxide of about 81 percent based on the original charge.
- EXAMPLE Ill A third test was conducted employing the same concentrate and equipment as previously described in connection with Example The same procedure utilizing the same temperature and reaction conditions were used but a total pressure of 1,500 p.s.i.g. was employed so as to provide a calculated oxygen partial pressure of 1,365 p.s.i. The resultant filtrate obtained had a pH of less than zero and analysis of the reaction residue revealed that 89.8 percent of the molybdenum disulfide present in the original charge was converted to molybdenum trioxide.
- a process for converting molybdenum disulfide to molybdenum oxide which comprises the steps. of dispersing a particulated molybdenum disulfide-bearing material having an average particle size less than about 20 microns in water forming an aqueous slurry containing up to about 40 percent by weight of said material, heating said slurry to a temperature of at least about C. and agitating said slurry while in contact with an atmosphere containing free oxygen at an oxygen partial pressure of at least about 215 p.s.i.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Manufacture And Refinement Of Metals (AREA)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US86319769A | 1969-10-02 | 1969-10-02 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US3656888A true US3656888A (en) | 1972-04-18 |
Family
ID=25340519
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US863197A Expired - Lifetime US3656888A (en) | 1969-10-02 | 1969-10-02 | Liquid phase oxidation process |
Country Status (8)
| Country | Link |
|---|---|
| US (1) | US3656888A (fr) |
| AT (1) | AT305211B (fr) |
| BE (1) | BE756944A (fr) |
| CA (1) | CA935623A (fr) |
| FR (1) | FR2064092B1 (fr) |
| LU (1) | LU61791A1 (fr) |
| NL (1) | NL141841B (fr) |
| SE (1) | SE352613B (fr) |
Cited By (31)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4165362A (en) * | 1977-04-08 | 1979-08-21 | Engelhard Minerals & Chemicals Corporation | Hydrometallurgical processing of molybdenite ore concentrates |
| US4342728A (en) * | 1981-01-19 | 1982-08-03 | Amax Inc. | Process for digesting tungsten ores containing organic matter |
| US4379127A (en) * | 1981-07-22 | 1983-04-05 | Gfe Gesellschaft Fur Elektrometallurgie Mbh | Method of recovering molybdenum oxide |
| US4414060A (en) * | 1980-12-16 | 1983-11-08 | Nalco Chemical | Method for sulfite pulping using water-soluble molybdenum containing compounds |
| US4432947A (en) * | 1981-07-31 | 1984-02-21 | Uranium Pechiney Ugine Kuhlmann | Process for obtaining molybdenum as a useful product from molybdeniferous solutions containing alkali metal carbonate, sulphate, hydroxide or hydrogen carbonate and possibly uranium |
| US4512958A (en) * | 1983-10-28 | 1985-04-23 | Gfe Gesellschaft Fur Elektrometallurgie Mbh | Method of recovering molybdenum oxide |
| US4523948A (en) * | 1984-02-14 | 1985-06-18 | Amax Inc. | Roasting of molybdenite concentrates containing flotation oils |
| DE3443806A1 (de) * | 1984-11-27 | 1986-06-05 | Eberhard Priv. Doz. Prof. Dr.-Ing. 1000 Berlin Gock | Verfahren zur herstellung von reinem moo(pfeil abwaerts)3(pfeil abwaerts) ueber die extraktion von molybdaen aus sulfatloesungen |
| US4657745A (en) * | 1986-03-31 | 1987-04-14 | Chemical & Metal Industries, Inc. | Value recovery from spent alumina-base catalyst |
| WO1996012675A1 (fr) * | 1994-10-24 | 1996-05-02 | Kennecott Corporation | Procede d'oxydation sous pression pour la production de trioxyde de molybdene a partir de molybdenite |
| US5804151A (en) * | 1997-09-16 | 1998-09-08 | Cyprus Amax Minerals Company | Process for autoclaving molybdenum disulfide |
| US5820844A (en) * | 1997-01-29 | 1998-10-13 | Cyprus Amax Minerals Company | Method for the production of a purified MoO3 composition |
| US5985236A (en) * | 1998-06-09 | 1999-11-16 | Cyprus Amax Minerals Company | Ammonium octamolybdate composition and method for producing the same |
| US6451088B1 (en) | 2001-07-25 | 2002-09-17 | Phelps Dodge Corporation | Method for improving metals recovery using high temperature leaching |
| US6451089B1 (en) | 2001-07-25 | 2002-09-17 | Phelps Dodge Corporation | Process for direct electrowinning of copper |
| WO2002090263A1 (fr) * | 2001-05-09 | 2002-11-14 | H. C. Starck Gmbh | Mecanismes de commande d'autoclave pour oxydation de molybdenite sous pression |
| US6497745B2 (en) | 2000-07-25 | 2002-12-24 | Phelps Dodge Corporation | Method for processing elemental sulfur-bearing materials using high temperature pressure leaching |
| US6676909B2 (en) | 2000-07-25 | 2004-01-13 | Phelphs Dodge Corporation | Method for recovery of metals from metal-containing materials using medium temperature pressure leaching |
| US6680034B2 (en) | 2000-07-25 | 2004-01-20 | Phelps Dodge Corporation | Method for recovering metal values from metal-containing materials using high temperature pressure leaching |
| US20050109163A1 (en) * | 2001-07-25 | 2005-05-26 | Phelps Dodge Corporation | Process for multiple stage direct electrowinning of copper |
| US20050126923A1 (en) * | 2001-07-25 | 2005-06-16 | Phelps Dodge Corporation | Process for recovery of copper from copper-bearing material using medium temperature pressure leaching, direct electrowinning and solvent/solution extraction |
| US20060144717A1 (en) * | 2004-10-29 | 2006-07-06 | Phelps Dodge Corporation | Process for recovery of copper from copper-bearing material using pressure leaching, direct electrowinning and solvent/solution extraction |
| RU2302997C2 (ru) * | 2001-05-09 | 2007-07-20 | Х.К. Штарк Гмбх | Способ получения высокочистого димолибдата аммония (его варианты) |
| US20080023342A1 (en) * | 2004-10-29 | 2008-01-31 | Phelps Dodge Corporation | Process for recovery of copper from copper-bearing material using pressure leaching, direct electrowinning and solution extraction |
| US20080124269A1 (en) * | 2006-11-16 | 2008-05-29 | Albemarle Netherlands B.V. | Purified molybdenum technical oxide from molybdenite |
| US20080166280A1 (en) * | 2006-11-16 | 2008-07-10 | Albemarle Netherlands B.V. | Purification Of Molybdenum Technical Oxide |
| US20090071839A1 (en) * | 2004-10-29 | 2009-03-19 | Phelps Dodge Corporation | Process for multiple stage direct electrowinning of copper |
| RU2398902C1 (ru) * | 2009-03-30 | 2010-09-10 | Российская Федерация, от имени которой выступает государственный заказчик-Государственная корпорация по атомной энергии "Росатом" | Способ гидрометаллургической переработки ренийсодержащего молибденитового концентрата |
| WO2011024164A1 (fr) * | 2009-08-24 | 2011-03-03 | Metal Tech Ltd. | Procédé pour la séparation de multiples métaux issus de matières premières et système de mise en uvre du procédé |
| US8753591B2 (en) | 2012-03-23 | 2014-06-17 | Kennecott Utah Copper Llc | Process for the conversion of molybdenite to molydenum oxide |
| CN106745262A (zh) * | 2016-12-12 | 2017-05-31 | 郑州大学 | 一种利用氧化少层硫化钼制备非晶氧化钼纳米片的方法 |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2354726C1 (ru) * | 2007-07-11 | 2009-05-10 | Государственное Учреждение Институт металлургии Уральского отделения Российской Академии Наук (ГУ ИМЕТ УрО РАН) | Способ получения диоксида молибдена |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1118150A (en) * | 1913-11-14 | 1914-11-24 | Michael J O Brien | Process for recovering molybdenum from its ores and concentrates. |
| GB457552A (en) * | 1935-02-25 | 1936-11-25 | Ig Farbenindustrie Ag | Method of carrying out chemical reactions and extraction processes |
| US3353908A (en) * | 1961-10-24 | 1967-11-21 | Knapsack Ag | Process for the manufacture of dicalcium phosphate |
-
0
- BE BE756944D patent/BE756944A/fr not_active IP Right Cessation
-
1969
- 1969-10-02 US US863197A patent/US3656888A/en not_active Expired - Lifetime
-
1970
- 1970-08-10 CA CA090360A patent/CA935623A/en not_active Expired
- 1970-09-11 FR FR7033076A patent/FR2064092B1/fr not_active Expired
- 1970-09-21 SE SE12822/70A patent/SE352613B/xx unknown
- 1970-09-30 AT AT882770A patent/AT305211B/de not_active IP Right Cessation
- 1970-09-30 LU LU61791D patent/LU61791A1/xx unknown
- 1970-10-02 NL NL707014530A patent/NL141841B/xx not_active IP Right Cessation
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1118150A (en) * | 1913-11-14 | 1914-11-24 | Michael J O Brien | Process for recovering molybdenum from its ores and concentrates. |
| GB457552A (en) * | 1935-02-25 | 1936-11-25 | Ig Farbenindustrie Ag | Method of carrying out chemical reactions and extraction processes |
| US3353908A (en) * | 1961-10-24 | 1967-11-21 | Knapsack Ag | Process for the manufacture of dicalcium phosphate |
Non-Patent Citations (2)
| Title |
|---|
| Dresher et al., Journal of Metals, June 1956, pp. 794 800. * |
| Usataya, Chemical Abstracts, Vol. 47, 1953, p. 5,313. * |
Cited By (55)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4165362A (en) * | 1977-04-08 | 1979-08-21 | Engelhard Minerals & Chemicals Corporation | Hydrometallurgical processing of molybdenite ore concentrates |
| US4414060A (en) * | 1980-12-16 | 1983-11-08 | Nalco Chemical | Method for sulfite pulping using water-soluble molybdenum containing compounds |
| US4342728A (en) * | 1981-01-19 | 1982-08-03 | Amax Inc. | Process for digesting tungsten ores containing organic matter |
| WO1982002540A1 (fr) * | 1981-01-19 | 1982-08-05 | Inc Amax | Oxydation par voie humide de matieres organiques |
| US4379127A (en) * | 1981-07-22 | 1983-04-05 | Gfe Gesellschaft Fur Elektrometallurgie Mbh | Method of recovering molybdenum oxide |
| US4432947A (en) * | 1981-07-31 | 1984-02-21 | Uranium Pechiney Ugine Kuhlmann | Process for obtaining molybdenum as a useful product from molybdeniferous solutions containing alkali metal carbonate, sulphate, hydroxide or hydrogen carbonate and possibly uranium |
| US4512958A (en) * | 1983-10-28 | 1985-04-23 | Gfe Gesellschaft Fur Elektrometallurgie Mbh | Method of recovering molybdenum oxide |
| US4523948A (en) * | 1984-02-14 | 1985-06-18 | Amax Inc. | Roasting of molybdenite concentrates containing flotation oils |
| DE3443806A1 (de) * | 1984-11-27 | 1986-06-05 | Eberhard Priv. Doz. Prof. Dr.-Ing. 1000 Berlin Gock | Verfahren zur herstellung von reinem moo(pfeil abwaerts)3(pfeil abwaerts) ueber die extraktion von molybdaen aus sulfatloesungen |
| US4657745A (en) * | 1986-03-31 | 1987-04-14 | Chemical & Metal Industries, Inc. | Value recovery from spent alumina-base catalyst |
| EP0241149A3 (en) * | 1986-03-31 | 1989-07-12 | Chemical & Metal Industries, Inc. | Value recovery from spent alumina-base catalysts |
| WO1996012675A1 (fr) * | 1994-10-24 | 1996-05-02 | Kennecott Corporation | Procede d'oxydation sous pression pour la production de trioxyde de molybdene a partir de molybdenite |
| US6149883A (en) * | 1994-10-24 | 2000-11-21 | Kennecott Utah Copper Corporation | Pressure oxidation process for the production of molybdenum trioxide from molybdenite |
| US5820844A (en) * | 1997-01-29 | 1998-10-13 | Cyprus Amax Minerals Company | Method for the production of a purified MoO3 composition |
| US5804151A (en) * | 1997-09-16 | 1998-09-08 | Cyprus Amax Minerals Company | Process for autoclaving molybdenum disulfide |
| US5985236A (en) * | 1998-06-09 | 1999-11-16 | Cyprus Amax Minerals Company | Ammonium octamolybdate composition and method for producing the same |
| WO1999064349A1 (fr) * | 1998-06-09 | 1999-12-16 | Cyprus Amax Minerals Company | Nouvelle composition d'octamolybdate d'ammonium et procede de production de ladite composition |
| US6235261B1 (en) | 1998-06-09 | 2001-05-22 | Cyprus Amax Minerals Co. | Method for producing ammonium octamolybdate composition |
| US20040146438A1 (en) * | 2000-07-25 | 2004-07-29 | Marsden John O | Method for recovery of metals from metal-containing materials using medium temperature pressure leaching |
| US7473413B2 (en) | 2000-07-25 | 2009-01-06 | Phelps Dodge Corporation | Method for recovering metal values from metal-containing materials using high temperature pressure leaching |
| US6497745B2 (en) | 2000-07-25 | 2002-12-24 | Phelps Dodge Corporation | Method for processing elemental sulfur-bearing materials using high temperature pressure leaching |
| US6676909B2 (en) | 2000-07-25 | 2004-01-13 | Phelphs Dodge Corporation | Method for recovery of metals from metal-containing materials using medium temperature pressure leaching |
| US6680034B2 (en) | 2000-07-25 | 2004-01-20 | Phelps Dodge Corporation | Method for recovering metal values from metal-containing materials using high temperature pressure leaching |
| US7341700B2 (en) | 2000-07-25 | 2008-03-11 | Phelps Dodge Corporation | Method for recovery of metals from metal-containing materials using medium temperature pressure leaching |
| US20040146439A1 (en) * | 2000-07-25 | 2004-07-29 | Marsden John O. | Method for recovering metal values from metal-containing materials using high temperature pressure leaching |
| WO2002090263A1 (fr) * | 2001-05-09 | 2002-11-14 | H. C. Starck Gmbh | Mecanismes de commande d'autoclave pour oxydation de molybdenite sous pression |
| RU2302997C2 (ru) * | 2001-05-09 | 2007-07-20 | Х.К. Штарк Гмбх | Способ получения высокочистого димолибдата аммония (его варианты) |
| US6818191B2 (en) * | 2001-05-09 | 2004-11-16 | H. C. Starck, Inc. | Autoclave control mechanisms for pressure oxidation of molybdenite |
| CN1300003C (zh) * | 2001-05-09 | 2007-02-14 | H·C·施塔克有限公司 | 高压氧化辉钼矿的高压釜控制方法 |
| US20050109163A1 (en) * | 2001-07-25 | 2005-05-26 | Phelps Dodge Corporation | Process for multiple stage direct electrowinning of copper |
| US20050126923A1 (en) * | 2001-07-25 | 2005-06-16 | Phelps Dodge Corporation | Process for recovery of copper from copper-bearing material using medium temperature pressure leaching, direct electrowinning and solvent/solution extraction |
| US20050155458A1 (en) * | 2001-07-25 | 2005-07-21 | Phelps Dodge Corporation | Method for Improving Metals Recovery Using High Temperature Pressure Leaching |
| US7476308B2 (en) | 2001-07-25 | 2009-01-13 | Phelps Dodge Corporation | Process for multiple stage direct electrowinning of copper |
| US20060196313A1 (en) * | 2001-07-25 | 2006-09-07 | Phelps Dodge Corporation | Method for recovering copper from copper-containing materials using direct electrowinning |
| US7125436B2 (en) | 2001-07-25 | 2006-10-24 | Phelps Dodge Corporation | Method for improving metals recovery using high temperature pressure leaching |
| US6893482B2 (en) | 2001-07-25 | 2005-05-17 | Phelps Dodge Corporation | Method for improving metals recovery using high temperature pressure leaching |
| US6451088B1 (en) | 2001-07-25 | 2002-09-17 | Phelps Dodge Corporation | Method for improving metals recovery using high temperature leaching |
| US6451089B1 (en) | 2001-07-25 | 2002-09-17 | Phelps Dodge Corporation | Process for direct electrowinning of copper |
| US20040045406A1 (en) * | 2001-07-25 | 2004-03-11 | Marsden John O. | Method for improving metals recovery using high temperature pressure leaching |
| US20080023342A1 (en) * | 2004-10-29 | 2008-01-31 | Phelps Dodge Corporation | Process for recovery of copper from copper-bearing material using pressure leaching, direct electrowinning and solution extraction |
| US7722756B2 (en) | 2004-10-29 | 2010-05-25 | Freeport-Mcmoran Corporation | Process for multiple stage direct electrowinning of copper |
| US7736488B2 (en) | 2004-10-29 | 2010-06-15 | Freeport-Mcmoran Corporation | Process for recovery of copper from copper-bearing material using pressure leaching, direct electrowinning and solvent/solution extraction |
| US20060144717A1 (en) * | 2004-10-29 | 2006-07-06 | Phelps Dodge Corporation | Process for recovery of copper from copper-bearing material using pressure leaching, direct electrowinning and solvent/solution extraction |
| US7485216B2 (en) | 2004-10-29 | 2009-02-03 | Phelps Dodge Corporation | Process for recovery of copper from copper-bearing material using pressure leaching, direct electrowinning and solvent/solution extraction |
| US20090071839A1 (en) * | 2004-10-29 | 2009-03-19 | Phelps Dodge Corporation | Process for multiple stage direct electrowinning of copper |
| US20090101518A1 (en) * | 2004-10-29 | 2009-04-23 | Phelps Dodge Corporation | Process for recovery of copper from copper-bearing material using pressure leaching, direct electrowinning and solvent/solution extraction |
| US7736487B2 (en) | 2004-10-29 | 2010-06-15 | Freeport-Mcmoran Corporation | Process for recovery of copper from copper-bearing material using pressure leaching, direct electrowinning and solution extraction |
| US20080166280A1 (en) * | 2006-11-16 | 2008-07-10 | Albemarle Netherlands B.V. | Purification Of Molybdenum Technical Oxide |
| US20080124269A1 (en) * | 2006-11-16 | 2008-05-29 | Albemarle Netherlands B.V. | Purified molybdenum technical oxide from molybdenite |
| RU2398902C1 (ru) * | 2009-03-30 | 2010-09-10 | Российская Федерация, от имени которой выступает государственный заказчик-Государственная корпорация по атомной энергии "Росатом" | Способ гидрометаллургической переработки ренийсодержащего молибденитового концентрата |
| WO2011024164A1 (fr) * | 2009-08-24 | 2011-03-03 | Metal Tech Ltd. | Procédé pour la séparation de multiples métaux issus de matières premières et système de mise en uvre du procédé |
| US20120148461A1 (en) * | 2009-08-24 | 2012-06-14 | Metal Tech Ltd. | Process for multi metal separation from raw materials and system for use |
| US8753591B2 (en) | 2012-03-23 | 2014-06-17 | Kennecott Utah Copper Llc | Process for the conversion of molybdenite to molydenum oxide |
| CN106745262A (zh) * | 2016-12-12 | 2017-05-31 | 郑州大学 | 一种利用氧化少层硫化钼制备非晶氧化钼纳米片的方法 |
| CN106745262B (zh) * | 2016-12-12 | 2017-12-29 | 郑州大学 | 一种利用氧化少层硫化钼制备非晶氧化钼纳米片的方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| FR2064092B1 (fr) | 1973-12-21 |
| AT305211B (de) | 1973-02-12 |
| NL7014530A (fr) | 1971-04-06 |
| CA935623A (en) | 1973-10-23 |
| DE2043874A1 (fr) | 1971-04-15 |
| FR2064092A1 (fr) | 1971-07-16 |
| NL141841B (nl) | 1974-04-16 |
| DE2043874B2 (de) | 1972-08-31 |
| LU61791A1 (fr) | 1971-06-18 |
| BE756944A (fr) | 1971-03-16 |
| SE352613B (fr) | 1973-01-08 |
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