AU2018101150C4 - This patent application is a description of an extraction process which maximises resource utilisation by extracting valuable molybdenum oxides from overburden developed by oxidation processes above a metal deposit. The product of this process is then utilised as components of molybdenum trioxide - based fertiliser. - Google Patents
This patent application is a description of an extraction process which maximises resource utilisation by extracting valuable molybdenum oxides from overburden developed by oxidation processes above a metal deposit. The product of this process is then utilised as components of molybdenum trioxide - based fertiliser. Download PDFInfo
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Abstract
This patent application is a description of an extraction process which
maximises resource utilisation by extracting valuable molybdenum oxides
from overburden developed by oxidation processes above a metal deposit.
By use of physical extraction utilising gravity separation post-treatment of
crushing the raw rock material, refined molybdenum trioxide can be added
to composted material to increase the efficacy of the product for plant
uptake. Molybdenum Oxide has vast potential as a fertiliser product,
particularly due to its role in nitrogen metabolism, and the synthesis of
protein in plants. Molybdenum is one of the essential micronutrients that
acts as a catalyst required by plants and symbiotic bacteria in order to make
nitrogen plant-available.
Description
[001] This is a method of recovering / extracting molybdenum oxide ore from overburden developed by oxidation processes above a metal deposit comprising separation ofthe overburden through gravityseparation methods based on the differential density properties of the overburden.
[002] The method appended in Claim Iis applicable to molybdenum oxide-bearing granitic hosts for recovering molybdenum oxides using cyclones which classify as a dry mineral processing technique.
[003] The method appended in Claim 1 is applicable to molybdenum oxide-bearingcarbonaceous shalehost material for recovering molybdenum oxides using spirals which classify as a wet mineral processing technique.
Please refer to Figure 1Steps 9 to 20 and Figures 2 to 3 for a graphical explanation of these methods.
[004] The innovation revolves around theextraction of molybdenum oxidesfrom the oxidisedoverburden appended in Claim No. 1. This overburden contains ore. This material can be used to make a varietyof productssuch as fertiliser for legumes and molybdenum metal - based products such as battery anodes without the need for industrial chemical processing to make the source material, from which we extract molybdenum-based products
[005] Molybdenum forms chemical compounds in oxidation states from -II to +VI. Higher oxidation states are more relevant to its terrestrial occurrence and its biologicalroles,mid-level oxidation statesare often associated with metal clusters, and very low oxidation states are typically associated with organomolybdenum compounds. In chemistry a molybdate is a compound with molybdenum in its highest oxidation state of6. These various valenciesproduce a multiplicity of both natural source material (e.g., oxidised carbonaceous shale and iron ore), mineral separation techniques (e.g., gravity separation and magnetic separation) and end results products.
[006] In order to make commercial grade fertiliser material the production process will continuallyimprove thegrade or purity of the oxide source rock from 0.5%MoO3 in the run of mine ore to a significantly more refined grade of 90% Mo3. Molybdenum oxide can occur naturally (but rarely) as the yellow crystalline mineral molybdite (MoO3).
What
[007] Although it is toxic in anything other than small quantities,molybdenum is an essentialelementfor animalsand plants. There are about 50 different enzymes used by plants and animals that contain molybdenum. One of theseis nitrogenase, found in nitrogen-fixing bacteria that make nitrogen from theair available to plants. Leguminous plants have root nodules that contain these nitrogen-fixing bacteria.
[008] By use of physicalextraction utilising gravity separation post-treatment ofcrushing theraw rock material,refined molybdenum trioxide can be added to composted material to increase the efficacy of the product for plantuptake. This increases resource utilisation efficiencies and also improves soil nitrogen cycling viaecosystem functionsof nitrogen fixing bacteria. In addition it improves energy use cost due tonot having to producethe nitrogen via the Haber Bosch methodology. Note that this process is registered for use in organicfarming practices and will becompliant assuchto the National Standard fororganic and biodynamic products (Version 3.7) andthe Australian Standard AS 6000 which is a component of Standards Australia.
How
[009] We assume that the reader has a working knowledge of chemical terms such as element, ion, compound, molecule, mineral, oxidation. Molybdenum (atomic weight 95.96) is a hard, silvery-grey, ductile, malleable first-row transition metal in the periodic table.
[010] The upper part of the Earth's crust has developed over millionsof years by interacting with water and atmospheric gases, all of which contain oxygen, and which reactwith reduced elements incompounds such asthe metal sulphides and common rock-forming silicate minerals. This is why we see brown coloured rocks at thesurfaceand grey coloured rock cores brought up from depth (30 metres below ground level) by drillingrigs. Whether this"redox" interface or boundary between the oxidised rock layer and unoxidised (fresh) rock is at 30 or 50 metres etc. depends on many factors such as climate history, soil development and type, geological history etc. The other important factor is that much groundwater movement occurs within this weathered or oxidised zone.
[011] Within the oxidised zone grey molybdenite (MoS 2 ) is converted to the yellow trioxide molybdite (MoO3) and other molybdenum oxide compounds.
[012] The current methodology for making oxides of molybdenum is based on deriving the oxide from the sulphide metal ore. This process has high externalities associated with it. This patent provides material such as these oxides that are in a form that provides an ecologically softer footprint when used in agricultural and industrial applications. All current molybdenum oxide production is a by-product of metal refining and no dedicated primary extraction of molybdenum oxide exists. The next paragraph details aspectsof the chemistry underlyingthe current paradigm.
[013] The anions (negatively charged ions) which are of importance as plant nutrients are molybdate MoO4(2-). However to meet industrial demand sodium and ammonium molybdate are traditionally made inChina and the USA by a complex energy and chemical demanding process. Sodium molybdate is made by roasting in a caustic (alkali) environment.
2MoS 2+70 2 -- 2Mo+4SO2T, Equation 01 MoO3+2NaOH+H 20--Na2MoO 4 2H2 0.
[014] Ammonium Molybdate is made by roasting then ammonia leaching,purification and reaction with nitric acid. After separation, drying and sieving one can obtain the finished product.
Who/Why
[015] Molybdenum oxide has vast potential as a fertiliser product, particularly due to its role in nitrogen metabolism, and the synthesis of protein in plants. One of the largest crop types in the world of agriculture are legumes or pulses, which provide a plant-derived form of protein that is not sourced from animals. Molybdenum oxideassistsin nitrogen uptake by legumes in particular, and in crops in general. Molybdenum oxide fertiliser can be added to the soil,or directly to the plant.
[016] Molybdenum is one of the essential micronutrients required by plants and symbiotic bacteria. Molybdenum is important in nitrogen metabolism. Of all theessential micronutrients, molybdenum is required in thesmallest amount by plants. Symbiotic bacteria however, require approximately ten times more molybdenum fornitrogen fixationthan the host plant. If there is not enough molybdenum present, petro-chemical based fertilisers are required to accommodate for this and provide the required amount of nitrogen.
[017] Molybdenum is the least abundant of the trace elements in soils, and only a smallamount is present in forms that are available to plants. Molybdenum fertiliser is therefore necessary to ensure plants have the essential micronutrients to convert destructive nitrates into protein. Our invention represents a cleaner alternative to the traditional method noted below. It is alsocompliant to be registered for use in organic farming systems.
[018] Compounds mimicking the enzyme nitrogenase represent promising alternative routes to the current Haber Bosch industrial synthesis of ammonia from molecular hydrogen and nitrogen (Leigh, 2003). Noting the reduction of embedded energy due to the fostering of ecosystem services provided bythe symbioticprocesses inthe rhizosphere of legume plants. Note also that 74,000 tonnes ofN 2 is"in the air" above every hectare of land. Molybdenum acts as a catalyst to enable ecosystem functions to make it plant-available, hence reducing the downsize externalityand embedded energy costs of the Haber-Bosch process inflicts on the environment and society.
[019] The following article extract in the next two paragraphs (022/023) is from Hoffman (2014). Individual citations at the end of each sentence in Hoffman's paper will not be repeated here.
[020] "Nitrogen fixation has a profound agronomic, economic, and ecological impact owing to the fact thatthe availability of fixed nitrogen represents the factor that most frequently limits agricultural productionthroughoutthe world. Indeed, nearly half of the existing human population could not exist without application of the Haber-Bosch process for production of nitrogen fertilizers. Given that over half of the fixed nitrogen input that sustains Earth's population is supplied biologically, there has been intense interest in understanding how the nitrogenase enzyme accomplishes the difficult task of N 2 fixation at ambient temperature and pressure. An understanding of biological N 2 fixation may further serve as the foundation for achieving twohighlydesirable, although so farunmet, goals: genetically endowing higher plants with the capacity to fix their own nitrogen and developing improved syntheticcatalystsbased on the biological mechanism.
[021] It has been over 150 years since Jodin first suggested that microbes could "fix" N2 and more thana century since the first isolation of N2-fixing bacteria around 1900. In 1934,Burk coined theterm "nitrogenase" forthe enzyme that catalyzes the conversion of N2 to a bioaccessible form of nitrogen,and initiatedthe first meaningful studies of nitrogenase in living cells. Methods for extracting nitrogenase in an active form were developed in the early 1960s, opening the way for serious mechanistic investigations. The next 35 years witnessed intensiveeffortsby numerous investigators to reveal the structure and catalytic function of nitrogenase. These developments were summarized in the magisterial review by Burgess and Lowe in 1996. Key advancesin understanding nitrogenase structureand function during those intervening years included the following: (i) It was determined that nitrogenase is a two-component system composed of the MoFe protein (also called dinitrogenase or component I) andthe electron-transfer Fe protein (also called dinitrogenase reductase or component II). (ii) A reducing source and MgATP are required for catalysis (iii) Fe protein and MoFe protein associate and dissociate in a catalytic cycle involving single electron transfer and MgATP hydrolysis. (iv) It was discovered that the MoFe protein contains two metal clusters: the iron-Molybdenum cofactor (FeMo-co), which provides the active site for substrate binding and reduction, and P-cluster, involved in electron transfer from the Fe protein to FeMo-co. (v) Crystallographic structures were solved for both Fe and MoFe proteins. (vi) Also, the alternative V- and Fe-type nitrogenases, in which the Mo of FeMo-co is replaced by V or Fe,were discovered. Despite this accumulation of functional and structural information, the catalytic mechanism remained elusive".
[022] To assist in the understanding of the invention, preferred embodiments ofthe inventionwill be describedby way of example with reference to the accompanying drawings. The brief text below introduces thesteps whichare described in detail in paragraphs [053] to [064]. Figures 2-3 were sourced from Wikipedia.
[023] Figure Ishows a holistic sketch of the overall process from run of mine natural resource material through to final packaged fertiliser product or metal derivatives. Step 1 is "Run of Mine" (ROM) ore. Step2 is primary crushing. Step 3 is screening. Step 4 is a conveyor. Step 5 is a coarse ore stockpile. Step 6is a conveyor. Step 7 is a secondary crusher. Step 8 is a screen deck. Step 9 is a cyclone. Step 9M is optionally a cyclone/ magnetic separator. Step 10is the cyclone oversize. Step 11 is a pipe. Step 12 is a pipe. Step 13 is a stockpile. Step 14 is a screen. Step 15 isa stockpile. Step 16 is a stockpile. Step 17 is a pipe. Step 18 isa screen. Step 19 is a stockpile. Step 20 is a stockpile. Figure 2 shows a sketch of a typical cyclone. Step 1 clean air exitsthe collector. Step2 secondary airnozzles. Step3 nozzles generate a secondary vortex. Step 4 inner vortex generated by a spinner. Step 5 secondary air returned to outlet stream. Step 6 particulate will follow the walls of the collector. Step 7 hopper outlet. Step 8 primaryair inlet. Step 9 secondary air inlet. Step 10 outlet. Figure 3 shows a sketch of a typical spiral. Step 1 is afeeder chute. Step2 is a centre column. Step 3 is a spiral chute. Step4 is a discharge box. Step 5 is a product collectionfunnel. Step 6is a discharge box. Step 7 is a feed box.
[024] Embodiments of the present invention reside primarily inan extraction process which maximises naturalresource utilisation by extracting molybdenum trioxide from overburden above a metallic mineral deposit.
[025] Metals occur in all kinds of rocks butusually in concentrations thatare too low to be mined. Metallic ore deposits, however, are relatively rare concentrations of metal-bearing minerals (usually sulphides) that contain enough metal to be profitably mined. Molybdenum oxides in Australia however, do occur as deposits in their own right. Prime examples are the carbonaceous shales referenced in Claim 2.
[026] Stoichiometry is the field of quantitative science involved with chemical reactions. It is an important aspectof the patent. From a chemical engineering perspective, it is all about increasing the concentration ofthe saleable commodity in any volume of crushed rock to the point where it is'fit for purpose'. We measure this commonly asper cent concentration by volume volumee% orv/v%.
[027] In wet chemistry, the numerator in the abovefraction iscalled the soluteand the denominator iscalledthe total volume of solution. Similar principles apply to rocks and minerals.
[028] Our naturally occurring ore (molybdite) will have a concentration (grade of Mo) of about11% by volume.
[029] We need to increase this grade range of0.5%tol1.0 %significantly in order to make our fertiliser products.
[030] Our 'base' is molybdite (molybdenum trioxide) which has a natural stoichiometric concentration of molybdenum of 6 6 %.Other products such as sodium and ammonium molybdate are derived from the molybdite (molybdenum trioxide) base. This figure can be derived empirically by simply replacing the elements in the formula withtheir respective atomic weights and performing the v/v quotient calculation.
[031] In Table Ibelow we have done this v/v calculation for the common molybdenum fertiliser products. Some numbers are higher (richer products) than others and each product has its own role in agriculture. For example, molybdite is sometimes preferred for soil conditioning as opposed to sodium molybdate (a type of salt) which may be used as foliate.
TABLE 1
Types of Molybdenum Oxides
Source Formula %/Molybdenum Ammonium Molybdate (NH 4 )6 Mo7 0 2 4 .2H2 0 54 Molybdenum Trioxide MoO3 66
Sodium Molybdate Na2MoO 4.2H20 39
[032] Our market differentiators revolve around how we plan to make and extract our products (as referred to in Claims 1-3) as well as the uniqueness of the products themselves. Noting that molybdenum has many applications other than just fertilizer.
[033] The simplest way to increase our grade of molybdenum oxide in our products is to make use of the naturally high density of the metal (and even in the oxide form). Gravity separation techniquesare the obvious solution (refer to Claims 2 and 3). This is a mechanical technique involving no addition ofchemicals. This technique has been used in the mineral sands industry for decades.
[034] In terms of invention one of our unique outputs will be our initial product mix using our base molybdite compound. We plan to mix it with compost to make an organic fertiliser.
[035] It is also only within the shallow weathered zone that the molybdite fertiliser occurs,(this zone has traditionally been regarded as valueless hence the innovative nature of this patent application)thus creating a unique marketing opportunity for Kynoch Minerals in the future to take its molybdite fertiliser manufacturing method and apply itto what are currently millions of tons of useless overburden at various molybdenum depositsboth within Australia andaround the world (as referred to in Claim 1 and explained in Claims 2 and3).
[036] Australia accounts for just over 1.5%of the world's economic resources of Molybdenum metal.
[037] Molybdenum metal worldwide is only produced as a by-productof copper production.There are no Molybdenum Oxide specific mines anywhere in the world. Thus, the only current producers of molybdite forfertiliser are also producing copper - Molybdenum mines. In other words, there are no mines anywhere in the world that are dedicated to molybdite fertiliser production. Chemical engineers struggle to liberate anything economically from the upper parts of these deposits.
[038] Kynoch Minerals Pty Ltd (KM) has the potential to be a unique source for dedicated molybdite fertiliser production and also other industrial applications where warranted. Noting the innovative actiondescribed inClaim1
[039] In terms of molybdite fertiliser Climax Molybdenum Co. (Climax) isthe world's leading producer of Molybdenum chemical products such as molybdite. Jinduicheng Molybdenum Co Ltd (China) (Jinduicheng) as well asbeing Asia's largest molybdenum oxide metal miner is also a major producer of molybdite fertiliser chemicals.Thesetwo producers would be our international competitors for molybdite fertiliser production, but we would be uniquely different interms of environmentally-friendly production.
[040] Strategically KM would however become the only molybdite fertiliser producer in theSouthern Hemisphere and could preclude Australian farmers and fertiliser manufacturers having to import this product.
[041] From an 'organic, clean and green' perspective because our molybdite fertiliser does not come out ofa metal refinery as do the chemicals at Climax and Jinduicheng, it may well find aunique market,evenin places like Chinaand India which increasingly look to Australia as part oftheir food securitystrategy.
[042] KM's molybdite will be produced by physical extraction methods which arecompliant to organic farming standards both in domestic and international markets.
[043] The final products are either multi-coloured powders or crystalline substancebased on valencies.
[044] While the quantity of molybdite for use on individual farms measured in kilograms per hectare issmall(e.g. 2kg/ha), the hectares of land under cultivation for legumes is enormous and growing rapidly.
[045] India has the largestshare of pulse production in the world at 2 5%. A quarter of thecountry isused for pulse production to feed the country's people.
[046] Pulses are important source of protein, high in fibre content and provide ample quantityof vitaminsand minerals. Keeping in view large benefits of pulses for human health, the United Nations proclaimed in 2016 asthe International Year of Pulses. Thus, due attention is required to enhance the production of pulses not only to meet the dietary requirement of protein but also to raise the awareness about pulses for achieving nutritional, food security and environmental sustainability.
[047] Pulses crops don't just feed people, they are good for the soil fertility via their action as a symbiont, which drives the ecosystem function that transforms Nitrogen toa plant available form.
[048] In India, the acreage for pulses ranged from 20.35 (2000-01) to 23.99 million ha (2012-13) and production varied from 11.08 (2000-01) to 18.45 million tons (2012-13). The productivity hasincreasedfrom 544kg/ha(2000 01) to 750 kg/ha (2012-13). The major pulses producing states are Madhya Pradesh (2 50/o),Utter Pradesh(13%), Maharashtra(12%), Rajasthan (11%), Andhra Pradesh (9%)and other states together (3 0%)during 2012-13.
[049] Some simple math highlights the potential for a'legume booster' market. If we assume just one annual application of molybdite for each hectare of farm under legume production:
million hectares (ha) * 1kg/ha * $40 / kg Equation 02
= $ 0.1 Billion (USD)
[050] This is just one annual treatment for one county. The Asian market alone could be worth many billionsof dollars for molybdite fertiliser.
[051] The following discussion related to the drawings.
[052] The elements of the apparatus have been illustrated in concise schematic form in the drawings, showing only those specific details that are necessary for understanding the embodiments of the present invention, but so asnot to obscure the disclosure with excessive detail that will be readily apparent to those ofordinary skill in the art having the benefit of the present description.
[053] In this specification, adjectives such as first and second, left and right, and the like may be used solelyto distinguish one element or action from another element or action without necessarily requiring or implyingany actual such relationship or order. Words such as "comprises" or "includes" are intended to define a non-exclusive inclusion, such that a process, method, article, or apparatusthat comprises a list of elements does not include onlythose elements but may include other elements not expressly listed, including elements that are inherent to such a process, method, article, or apparatus.
[054] Referring to Figure 1 there is shown a holistic sketch ofthe mining steps (1-7) and processingsteps (8-27) which detail this application.
[055] Steps Ito 7 are common to any mining operation. What is mining? Mining may be defined as the act, process or work of extracting earth materials from where theyoccurand then transporting them for processingor immediate use. A mine is, therefore, an excavation in the earth.
[056] Most of the remaining steps in Figurelrelate to mineral processing . The goals of mineral processing are to a) separate mineral particles from waste or gangue (rock minerals) b) subject minerals to processes in order to concentrate them or to extract metals from them. Mineral Processing comprisestwo steps; comminution and classification.
[057] Comminution is the process of breaking rock material into smaller pieces. Comminution aims to liberate mineral grains in preparation for separation. Itis common to consider comminution to be divisible intotwo subsets; crushing and grinding. The distinction is made on the basis of mechanical criteria, i.e. the machine types that are used to accomplish the rock breakage.
[058] The crushing stages and the typical size ranges associated with the stages are threefold; primary - mined blocks are reduced to 8-15 cm diameter, secondary - 1cm to 0.5 cm output, tertiary - 0.5 cm output orless.
[059] Classification is the term given to the separation of mineral particles based on particle size. Classification behaviour is influenced by the size, shape and density of the individual particles. Two commontypes of classifiersare screens and hydrocyclones (spirals). With screens, separation takes placeby lettingfine particlesfallthrough openings in the screen deck. With cyclones, large particles settle faster than small particlesofthe same mineral. Dense particles settle faster than light particles of the same sizeand shape and this allows us to separate individual particles. Centrifugal force speeds up the settling. A cyclone usesa rotational motion to create the centrifugal force.
[060] Step 1 represents "Run of Mine" (ROM) ore which is produced by long-standing mining industry processesof scraping (if the ground is soft enough) or drilling and blasting. Step 2 represents primary crushing whichis designed to make small rocks from large rocks delivered bythe previous drill and blast process. Crushed rocks are typically screened in Step 3 to filter off the smaller material which is conveyed in Step 4 to a coarse ore stockpile(Step 5) from where it is conveyed in Step 6 to a secondarycrusher (Step 7) where the rock is crushed to even smaller particle size.
[061] Again, the products from the crushing are screened (Step 8) in order to filter the finer material in preparation for gravity separation by cyclones in Step 9. Spirals have been used in Mining Engineering for many decades to gravity separate commodities such as mineral sands in order to exploit the differential density contrast of commercial commodities (e.g. Titanium rich spinel) from barren gangue minerals such as sand. By the completion of Step 7our ROM will be of a similar sand size or smaller.
[062] A screen in Step 10 will filter off the molybdenum oxide coming out of the Cyclone Gravitycircuit(Step 9). Oversize material (Step 10) can be recycled through the gravitycircuit asStep 11 as required. The molybdenum oxide emanating from the spirals is piped in Step 12 to a molybdenum oxide stockpile(Step 13) prior to conveying (Step 17) to a packaging unit (Step 18) in the warehouse (Step 19) ready for distributionto market.
BIBLIOGRAPHY (Non-Patent Literature)
Amax Inc . (1975). Patent: Direct reduction of molybdenum oxide to substantially metallic molybdenum. N/A. Retrieved from https://patents.google.com/patent/US4045216
Hoffman, B. (2014). Mechanism of Nitrogen Fixation by Nitrogenase: The Next Stage. Chemical Reviews,114(8), 4041-4062. Retrieved from htts://www.ncbi.nlm.nih.qov/pmc/articles/PMC4012840/
Leigh, G. (2004). Haber-Bosch and Other Industrial Processes. In: Smith B.E., Richards R.L., Newton W.E. (eds) Catalysts for Nitrogen Fixation. Nitrogen Fixation: Origins, Applications, and Research Progress, vol1. Dordrecht: Springer
Mujumdar, D.K. (2011). Pulse Crop Production - Principles and Technologies. New Delhi: PHI Learning Private Limited.
Claims (3)
1. This is a method of recovering / extracting molybdenum oxide-ore (molybdate) from overburden developed by oxidation processes above a metal deposit processing the overburden through gravity methods based on the differential density of the overburden.
2. The method appended in Claim 1 , applicable to molybdate bearing granitic hosts for recovering molybdenum oxide-ore using cyclone machinery which classifies as dry mineral processing.
3. The method appended in Claim 1 , applicable to molybdate bearing carbonaceus shale for recovering molybdenum oxide-ore using spiral machinery which classifies as wet mineral processing.
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| Wang, L. et al: "Geochemical modeling for predicting potential solid phases controlling the dissolved molybdenum in coal overburden, Powder River Basin, WY, U.S.A." Applied Geochemistry (1994), 9(1), pp. 37-43 * |
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| Publication number | Publication date |
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| AU2018101150A4 (en) | 2018-09-13 |
| AU2018101150B4 (en) | 2019-01-17 |
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