CN103884691B - Molybdenum leaching and assay method in a kind of nickel-molybdenum ore - Google Patents
Molybdenum leaching and assay method in a kind of nickel-molybdenum ore Download PDFInfo
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- CN103884691B CN103884691B CN201410130840.XA CN201410130840A CN103884691B CN 103884691 B CN103884691 B CN 103884691B CN 201410130840 A CN201410130840 A CN 201410130840A CN 103884691 B CN103884691 B CN 103884691B
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Abstract
Adopt roasting-alkaline leaching to process nickel-molybdenum ore, and use L9(34) orthogonal design, carry out Three factors-levels test, extraction conditions to the molybdenum content in nickel-molybdenum ore is optimized, get leaching liquid centrifugal filtration under optimum condition, dilution constant volume, measure again the content of molybdenum with Atomic Emission Spectrometer AES, result shows: the main order that affects the recovery rate of the molybdenum content in nickel-molybdenum ore is naoh concentration > roasting time > sintering temperature, the optimum condition that leaches molybdenum with NaOH is roasting time 2.5h, 500 DEG C of sintering temperatures, naoh concentration 40%. Under same atomic emission spectrum optimal conditions, sample is carried out to recovery testu, element recovery rate that the method is surveyed all, within the scope of 97.2%-102.3%, proves that the method degree of accuracy is high. Relative standard deviation, between 0.92%-1.24%, proves that the method precision is good. Illustrate that the method can carry out reliable analysis to molybdenum content in nickel-molybdenum ore.
Description
Technical field
The present invention relates to nickel-molybdenum ore to process and measure the method for molybdenum content.
Background technology
Molybdenum is a kind of important rare metal, and its fusing point is high, and heat resistance is good, and molybdenum is mainly used in steel industry, the oxygen of molybdenumCompound and sulfide for catalyst, lubricant molybdate for corrosion-inhibiting material, simultaneously containing Mo coating, pigment industry,Photoelectric field has development prospect widely.
Nickel-molybdenum ore is a kind of many metal composite ore deposit, and comparison of ingredients complexity, includes various metals and nonmetalloid, mainForm with carbon sulphur molybdenum ore exists, but because its complicated component, grade are relatively low, thereby adopt traditional physics and chemistry choosingOre deposit technology is more difficult by effective useful constituent wherein enrichment.
Molybdenum is low because of the not good rate of recovery that causes of process conditions aborning, mainly: molybdenum trioxide vapour pressure is high, and Yi Shenghua,Molybdenum is easily with particle form volatilization loss. Molybdenum in China mine ore is but more and more tending towards dilution. Make the molybdenum concentrate grade of ore dressingBe affected with the rate of recovery. Therefore, the rational exploitation and utilization of molybdenum ore is become a key content of ore dressing field.
Summary of the invention
The object of this invention is to provide a kind of method of nickel-molybdenum ore being processed and measured molybdenum content.
Technical scheme of the present invention is: this process using roasting-alkaline leaching is processed nickel-molybdenum ore, and question response is completeAfter, its solution dilution constant volume is got in centrifugal filtration, then measures the content of molybdenum with Atomic Emission Spectrometer AES, comprises Atomic Emission Spectrometer AESCondition optimizing and testing result preci-sion and accuracy are analyzed. It is strong that this technical scheme is cleared up ability, sample complete decomposition, and reagent is usedAmount is few, and blank value is low.
Concrete steps are as follows:
(1) alkali leaching sample condition optimization
First adopt Muffle furnace to calcine nickel-molybdenum ore, then with Muffle furnace, nickel-molybdenum ore is calcined at 500 DEG C,Liquid-solid ratio is under 2 condition, then nickel-molybdenum ore and 40% NaOH after calcining are reacted to 2.5h at 90 DEG C, treats fullyAfter reaction, its solution dilution constant volume is got in centrifugal filtration, then uses inductively coupled plasma aes determination reactant liquorThe content of middle molybdenum.
(2) Atomic Emission Spectrometer AES device condition optimizing
Select the optimized analysis wavelength of Mo (202.031nm) as element to be measured, at atomic emission spectrum cooling gas flowFor 15L/min, atomization gas flow is 0.8L/min, and assisted gas flow is 0.2L/min, and radio-frequency power is 1300W, and sample size isUnder the best instrument condition of 1.5mL/min, digestion solution is detected.
(3) result preci-sion and accuracy is analyzed
Soak in sample solution and add molybdenum standard liquid at alkali, under same atomic emission spectrum optimal conditions, sample is carried outRecovery testu, element recovery rate that the method is surveyed all, within the scope of 97.2%-102.3%, proves that the method degree of accuracy is high.And detection elements in this mark-on sample solution is carried out to precision analysis, and every kind of element continuous detecting 6 times, relative standard deviation existsBetween 0.92%-1.24%, prove that the method precision is good.
The present invention adopts roasting-alkaline leaching to process nickel-molybdenum ore, and after question response is complete, it is rare that its solution is got in centrifugal filtrationRelease constant volume, then measure the content of molybdenum with Atomic Emission Spectrometer AES, stronger than general Wet ability, sample complete decomposition, molybdenum is carriedThe rate of getting is high. The task of nickel-molybdenum ore oxidizing roasting is mainly that the sulfide of molybdenum is oxidized to molybdenum trioxide, to refining molybdenum-iron and copper metallurgySpeech, it is low containing total sulfur for special requirement, and for producing molybdenum chemical products, it is difficult to require in ammonia spirit and other alkaline solutionMolten molybdenum compound will lack. The method provides a kind of better sample treatment and detection method for the extraction of molybdenum in nickel-molybdenum ore.
Detailed description of the invention
Further describe the present invention below in conjunction with embodiment. Be noted that the present invention is not limited to following embodiment.
Embodiment
(1) dissolving of sample
Molybdenum is all stable in air or water at normal temperatures. Experimental result shows: molybdenum ability dilute sulfuric acid, hydrochloric acid, hydrogen fluorineThe corrosion such as acid, phosphoric acid. But in the time that temperature reaches 400 DEG C, start to occur slight oxidation, when reach after 600 DEG C, occur violentBe oxidized and generation molybdenum trioxide. This experiment adopts orthogonal design method, taking NaOH as leaching agent, selects roasting time (A),Sintering temperature (B), three factors of naoh concentration (C), adopt L9(34) orthogonal design, carry out Three factors-levels test, rightThe extraction conditions of the molybdenum content in nickel-molybdenum ore is optimized, and factor and water-glass are in table 1.
Table 1L9(34) orthogonal design
From the range analysis of showing, the main order that affects the recovery rate of the molybdenum content in nickel-molybdenum ore is C > A > B,Naoh concentration > roasting time > sintering temperature, optimum combination is A1B2C2, therefore, by the best of NaOH leaching molybdenumCondition is roasting time 2.5h, 500 DEG C of sintering temperatures, naoh concentration 40%.
(2) configuration of molybdenum standard reserving solution
Get a certain amount of smart molybdenum powder, after dry 4 hours, accurately take 0.0100g essence molybdenum powder at 85 DEG C in 50ml beaker,Dissolve (low-grade fever) with 10ml chloroazotic acid, after dissolving, constant volume, in 100ml volumetric flask, makes the molybdenum storing solution of 100 μ g/ml.
(3) atomic emission spectrometry is surveyed linear equation and the coefficient correlation of molybdenum
The curvilinear equation of table 2 method and coefficient correlation
Molybdenum standard reserving solution is diluted with ultra-pure water, be formulated as respectively 0.25,1.00,2.00,4.00,8.00 μ g/ML standard liquid, drawing standard curve and coefficient correlation under best Atomic Emission Spectrometer AES device optimal conditions. By number in upper tableAccording to finding out, the coefficient correlation of molybdenum is 0.999011. Therefore, the linearity of this calibration curve is good.
(4) molybdenum assay
After solution after dilution constant volume is measured with Atomic Emission Spectrometer AES, calculate the content of molybdenum according to following formula:
The content Y (%) of molybdenum=Am2×10-6v1v2/m×100％
In formula, m represents the quality (g) of nickel-molybdenum ore; m2Represent the content (μ g/ml) of Molybdenum in Solution to be measured; v1Represent before dilutionLiquor capacity (ml); v2Represent the volume (ml) of solution to be measured; A represents by v1Dilution is v2Extension rate.
(5) rate of recovery and Precision Experiment
In table 3 sample, molybdenum recovery and Precision Experiment result (μ g/ml) are (n=6)
As can be seen from the above table, element recovery rate that the method is surveyed all, within the scope of 97.2%-102.3%, proves the partyThe method degree of accuracy is high. Relative standard deviation (RSD), between 0.92%-1.24%, proves that the method precision is good. The method is describedIn can nickel-molybdenum ore, molybdenum content carries out reliable analysis.
(6) sample determination
Table 4 sample determination result (mg/g) (n=6)
This process using roasting-alkaline leaching is processed nickel-molybdenum ore, and after question response is complete, it is rare that its solution is got in centrifugal filtrationRelease constant volume, then measure the content of molybdenum with Atomic Emission Spectrometer AES, by finding out in upper table: respectively to samples' representativeness sampleDetect, testing result shows that result is very approaching. This result of study provides new method to molybdenum assay in nickel-molybdenum ore.
Above embodiment has described the present invention sample roasting-alkaline leaching has been cleared up and Atomic Emission Spectrometer AES device optimum determiningCondition, principal character and advantage. The technical staff of the industry should understand, and the present invention is not restricted to the described embodiments, above-mentionedThat in embodiment and description, describes just illustrates condition determination of the present invention, principal character and advantage, is not departing from the present inventionScope under, the present invention also has various changes and modifications, these changes and improvements all fall in the scope of protection of the invention.
Claims (1)
1. molybdenum leaching and an assay method in nickel-molybdenum ore, the method adopts roasting-alkaline leaching to process nickel-molybdenum ore,After question response is complete, its solution dilution constant volume is got in centrifugal filtration, then measures the content of molybdenum with Atomic Emission Spectrometer AES, and its feature existsIn step be:
(1) this experiment adopts orthogonal design method, taking NaOH as leaching agent, selects roasting time (A), sintering temperature (B),Three factors of naoh concentration (C), adopt L9(34) orthogonal design, carry out Three factors-levels test, to the molybdenum in nickel-molybdenum oreThe extraction conditions of content is optimized, and adopting the optimum condition of roasting-alkaline leaching leaching molybdenum is roasting time 2.5h, sintering temperature500 DEG C, naoh concentration 40%;
(2) get a certain amount of smart molybdenum powder, after dry 4 hours, accurately take 0.0100g essence molybdenum powder at 85 DEG C in 50ml beaker,Dissolve with 10ml chloroazotic acid, low-grade fever, after dissolving, constant volume, in 100ml volumetric flask, makes the molybdenum storing solution of 100 μ g/ml;
(3) add the standard liquid of different molybdenums in solution in leaching, under same atomic emission spectrum optimal conditions to sampleCarry out recovery testu, element recovery rate that the method is surveyed all, within the scope of 97.2%-102.3%, proves that the method is accurateSpend high; Relative standard deviation, between 0.92%-1.24%, proves that the method precision is good, illustrates that the method can be to nickel molybdenumIn ore deposit, molybdenum content carries out reliable analysis.
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