CN105866387A - Manganese ore phase analyzing method - Google Patents

Manganese ore phase analyzing method Download PDF

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CN105866387A
CN105866387A CN201610432502.0A CN201610432502A CN105866387A CN 105866387 A CN105866387 A CN 105866387A CN 201610432502 A CN201610432502 A CN 201610432502A CN 105866387 A CN105866387 A CN 105866387A
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acid
manganese ore
manganese
ore phase
water
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CN105866387B (en
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姜云
张文娟
郑建业
刘晶
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SHANDONG GEOLOGICAL SCIENCES INSTITUTE
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
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Abstract

The invention relates to an analysis determination method for specific compounds in ore, in particular to a manganese ore phase analyzing method. The manganese ore phase analyzing method is characterized in by comprising the following steps that firstly, manganese ore is weighed and smashed; secondly, an aluminum nitrate aqueous solution is added into the smashed manganese ore, extracting and filtering are carried out, filter residues are collected, and the manganese carbonate ore phase of filter liquor is determined; thirdly, a hydroxylamine sulphate and sulfuric acid solution is added into the filter residues collected in the second step, extracting and filtering are carried out, filter residues are collected, and the manganese oxide ore phase of filter liquor is determined; fourthly, the filter residues obtained the third step are ashed, mixed acid including nitric acid, hydrofluoric acid and perchloric acid is added for dissolving the ashed filter residues, and the manganese ore phase is determined. The manganese ore phase analyzing method is accurate and simple, the influence of phase shifting in the extraction processes is greatly relieved, the accuracy of an analyzing result is improved, and the problems that in a traditional manganese ore phase analyzing method, errors are large, phase shifting is serious, and efficiency is low are solved.

Description

A kind of manganese ore Phase Analysis
Technical field
The present invention relates to the analysis determining method of specific compound in a kind of Ore, be specifically related to a kind of manganese ore material phase analysis Method.
Background technology
In manganese ore, the material phase analysis of manganese is that research manganese difference composes the method for quantitatively determining depositing valence state or form and relevant reason Opinion.Manganese is the widest in distributed in nature, it is known that the mineral of manganese there are about kind more than 150, according to manganese existence form and industry in nature Purposes, generally only requires pyrolusite (MnO2), manganite (Mn2O3·H2O), braunite (Mn2O3), manganese spar (MnCO3) with And manganous silicate (MnSiO3) carry out material phase analysis.Under certain condition, the row that certain solvent is showed by the compound of these manganese For being different, so allow the manganese mineral of variform leach one by one, collect respectively, measure containing of every kind of component the most one by one Amount.Also can be selected for another other components of solvent dissolution, and make to be intended to record a certain component and stay in insoluble sludge, then measure residue In the content of this component.
Chemical phase analysis is research element existence in various carrier minerals and the method for content thereof, for geology Prospecting looks for ore deposit, ore-dressing technique research and mineral resource assessment to provide Back ground Information.China's manganese ore material phase analysis does not has skill at present Art specification, analysis method Main Basis " rock mineral analysis " (4 editions. Beijing: Geology Publishing House, 2011:856-861) provide Analysis process.But these methods are both for single mineral, a kind of method is not had to can be suitably used for most manganese ore.Example If it is for the leaching of manganese carbonate phase in manganese oxide ore as leached the leaching agent of manganese carbonate phase, the phenomenon of its string phase will compare Seriously, the accuracy of manganese carbonate phase result is influenced whether.And according to " ferrum, manganese, chrome ore geological exploration norm " (DZ/T 0200-2002) requirement, as long as manganese thing phase analyzes manganese carbonate, manganese oxide and manganous silicate, and does not has in existing analysis method To manganese carbonate, manganese oxide and the method for manganous silicate systematic analysis.
Summary of the invention
The invention aims to eliminate above-mentioned the deficiencies in the prior art and shortcoming, a kind of manganese ore material phase analysis is provided Method, solves in traditional manganese ore Phase Analysis error relatively big, goes here and there problem mutually serious, inefficient.
For reaching above-mentioned technique effect, the present invention adopts the following technical scheme that:
A kind of manganese ore Phase Analysis, employing following steps:
(1) weigh manganese ore, pulverize;
(2) adding aluminum nitrate aqueous solution, leaching in the manganese ore after step (1) is pulverized, filter, collect filtering residue, filtrate measures carbon Acid manganese ore phase;
(3) adding oxammonium sulfate .-sulfuric acid solution, leaching in the filtering residue that step (2) is collected, filter, collect filtering residue, filtrate measures oxygen Change manganese ore phase;
(4), after the ashing of step (3) described filtering residue, add the mixed-acid dissolution comprising nitrate acid and hydrofluoric acid-perchloric acid, measure silicic acid Manganese ore phase.
Preferably, the concentration of the aluminum nitrate solution described in step (1) is 40-80g/L;
Preferably, the temperature of step (2) and step (3) described leaching is 95-100 DEG C;
Preferably, in step (4) described mixed acid, the mol ratio of nitric acid, Fluohydric acid. and perchloric acid is 47:138:12.
Preferably, the concentration of the oxammonium sulfate .-sulfuric acid solution described in step (3) is 30-50g/L;Compound method is for weighing 30-50g oxammonium sulfate. is dissolved in the aqueous sulfuric acid that 1L volume fraction is 1-3%.
Preferably, the addition sequence of the mixed acid described in step (4), for being initially charged nitric acid, after heating 30min, adds height Chloric acid and Fluohydric acid..
Mixed acid described in step (4) also includes hydrochloric acid;The mol ratio of nitric acid, Fluohydric acid., perchloric acid and hydrochloric acid is 47: 138:12:(60-120).
Preferably, step (2) and the filtration described in step (3) all use chronic quantitative filter paper to filter.
Preferably, the granularity of step (1) described pulverizing is 160-200 mesh.
A kind of manganese ore Phase Analysis, concrete operation method is:
(1) weigh manganese ore, be crushed to 160-200 mesh;
(2) weighing the manganese ore 0.1-0.2g after step (1) is pulverized to be placed in 100mL beaker, adding 50ml concentration is 40-80g/ L aluminum nitrate solution, cap upper surface ware, put in 95-100 DEG C of water-bath, intermittent stirring, water-bath 40-60min, it is cooled to room temperature, Filtering, collect filtering residue, filtrate measures manganese carbonate ore phase;Preferably, intermittent stirring is to stir once every 10min;
(3) adding 50mL concentration in the filtering residue that step (2) is collected is 30-50g/L oxammonium sulfate .-sulfuric acid solution, cap upper surface ware, Put in the water-bath of 95-100 DEG C, intermittent stirring, water-bath 20-30min, it is cooled to room temperature, filters, collect filtering residue, filtrate is surveyed Determine manganese carbonate ore phase;30-50g/L oxammonium sulfate .-sulfuric acid solution compound method is dissolved in 1L volume for weighing 30-50g oxammonium sulfate. Mark is in the aqueous sulfuric acid of 1-3%;Preferably, intermittent stirring is to stir once every 10min;
(4) filtering residue described in step (3) is put in porcelain crucible, put into Muffle furnace, rise to 700 DEG C of ashing 1h, take out, move into poly- In tetrafluoroethene crucible, add the hydrochloric acid 9mL, 15.7mol/LHNO of 12.0mol/L3 3mL, heats 30min, adds 11.6mol/ L HClO41mL, 27.6mol/L Fluohydric acid. 5mL, is heated to white cigarette and emits to the greatest extent, add the hydrochloric acid 2mL of 12.0mol/L, go with 10-15ml Ionized water rinses sidewall of crucible, heating for dissolving, measures silicic acid manganese ore phase.
The present invention establishes a kind of Phase Analysis being applicable to most manganese ore, by more than 8 laboratorys The common precision coordinated trials participated in, it is determined that analyze repeatability limit and the repeatability limit of method, scientifically have evaluated foundation The quality level of manganese ore Phase Analysis, for providing with the quality control of laboratory monitoring chemical phase analysis in laboratory The foundation of science.Manganese ore Phase Analysis accuracy is not evaluated by the present invention first, by rock-mineral determination and not With the contrast test of method, method of chemical phase analysis is carried out system contrast verification, for lacking the analysis side of standard substance Method accuracy estimating provides referential technical method and means.
Beneficial effect
(1) the invention provides a kind of accurate, succinct manganese ore Phase Analysis, use aluminum nitrate solution, oxammonium sulfate .- Manganese carbonate phase in manganese ore, manganese oxide phase are leached mutually by sulfuric acid solution and mixed acid respectively with manganous silicate, are substantially reduced Leaching process goes here and there the impact of phase, improves precision of analysis, solve in tradition manganese ore Phase Analysis Error is relatively big, and string is serious mutually, inefficient problem.
(2) present invention establishes a kind of Phase Analysis being applicable to most manganese ore, and first to manganese ore Phase Analysis correctness is evaluated.
Detailed description of the invention
The present invention is further illustrated with comparative example in conjunction with the embodiments, it should explanation, the description below be only for The explanation present invention, is not defined its content.
Embodiment 1
(1) the manganese spar 0.1g weighing 160 mesh is placed in 100mL beaker, and wherein Fe content is 21.08%, and addition concentration is 40g/ The aluminum nitrate solution 50mL of L, cap upper surface ware, put in the water-bath boiled, after waiting water again to seethe with excitement, start timing, every 8 Once, (after noticing that the water in water-bath reduces, should add boiling water), water-bath 40min, quantitative filter paper filters at a slow speed for minute stirring (for preventing from filtering, filter paper pulp to be added on filter paper), collects filtering residue, and filtrate measures manganese carbonate ore phase;
(2) filtering residue described in step (1) is put in former beaker together with filter paper, adds 50mL 30g/L oxammonium sulfate .-1% sulphuric acid molten Liquid, puts in the water-bath boiled, and after waiting water again to seethe with excitement, starts timing, every stirring in 10 minutes once, and water-bath 20min, slowly Speed quantitative filter paper filters (for preventing from filtering, filter paper pulp to be added on filter paper), collects filtering residue, and filtrate measures manganese oxide ore phase;30g/L Oxammonium sulfate .-1% sulfuric acid solution compound method is to weigh 30g oxammonium sulfate. to be dissolved in the aqueous sulfuric acid that 1L volume fraction is 1%;
(3) putting in porcelain crucible by the filtering residue described in step (2) together with filter paper, put into Muffle furnace, low temperature rises to 700 DEG C of ashing 1h, takes out, and moves in politef crucible, adds the hydrochloric acid 9mL, 15.7mol/LHNO of 12.0mol/L3 3mL, heats 30min, Add 11.6mol/L HClO41mL, 27.6mol/L Fluohydric acid. 5mL is heated to white cigarette and emits to the greatest extent, adds the salt of 12.0mol/L Acid 2mL, by 10ml deionized water rinsing sidewall of crucible, heating for dissolving, pours mensuration silicic acid manganese ore phase in 50mL color comparison tube.
Embodiment 2
(1) the manganese spar 0.2g weighing 200 mesh is placed in 100mL beaker, and wherein Fe content is 19.77%, and addition concentration is 50g/ The aluminum nitrate solution 50mL of L, cap upper surface ware, put in 95 DEG C of water-baths, after again reaching 95 DEG C etc. water temperature, start timing, Every stirring in 10 minutes once, (after noticing that the water in water-bath reduces, 95 DEG C of hot water should be added), water-bath 60min, the most quantitatively Filter paper filtering (for preventing from filtering, filter paper pulp to be added on filter paper), collects filtering residue, and filtrate measures manganese carbonate ore phase;
(2) filtering residue described in step (1) is put in former beaker together with filter paper, adds 50mL 30g/L oxammonium sulfate .-3% sulphuric acid molten Liquid, puts in 95 DEG C of water-baths, after again reaching 95 DEG C etc. water temperature, starts timing, every stirring in 10 minutes once, and water-bath 30min, quantitative filter paper filters (for preventing from filtering, filter paper pulp to be added on filter paper) at a slow speed, collects filtering residue, and filtrate measures manganese oxide ore Phase;30g/L oxammonium sulfate .-3% sulfuric acid solution compound method is to weigh 30g oxammonium sulfate. to be dissolved in the sulphuric acid that 1L volume fraction is 3% In aqueous solution;
(3) putting in porcelain crucible by the filtering residue described in step (2) together with filter paper, put into Muffle furnace, low temperature rises to 650 DEG C of ashing 1h, takes out, and moves in politef crucible, adds the hydrochloric acid 8mL, 15.7mol/LHNO of 12.0mol/L3 3mL, heats 30min, Add 11.6mol/L HClO41mL, 27.6mol/L Fluohydric acid. 5mL is heated to white cigarette and emits to the greatest extent, adds the salt of 12.0mol/L Acid 2mL, by 15ml deionized water rinsing sidewall of crucible, heating for dissolving, pours mensuration silicic acid manganese ore phase in 50mL color comparison tube.
Embodiment 3
(1) the manganite 0.1g weighing 150 mesh is placed in 100mL beaker, and wherein Fe content is 46.34%, and addition concentration is 30g/ The aluminum nitrate solution 50mL of L, cap upper surface ware, put in the water-bath boiled, after waiting water again to seethe with excitement, start timing, every Once, (after noticing that the water in water-bath reduces, should add boiling water), water-bath 70min, quantitative filter paper filters at a slow speed in stirring in 10 minutes (for preventing from filtering, filter paper pulp to be added on filter paper), collects filtering residue, and filtrate measures manganese carbonate ore phase;
(2) filtering residue described in step (1) is put in former beaker together with filter paper, adds 50mL 50g/L oxammonium sulfate .-3% sulphuric acid molten Liquid, puts in the water-bath boiled, and after waiting water again to seethe with excitement, starts timing, every stirring in 10 minutes once, and water-bath 30min, slowly Speed quantitative filter paper filters (for preventing from filtering, filter paper pulp to be added on filter paper), collects filtering residue, and filtrate measures manganese oxide ore phase;50g/L Oxammonium sulfate .-3% sulfuric acid solution compound method is to weigh 50g oxammonium sulfate. to be dissolved in the aqueous sulfuric acid that 1L volume fraction is 3%;
(3) putting in porcelain crucible by the filtering residue described in step (2) together with filter paper, put into Muffle furnace, low temperature rises to 700 DEG C of ashing 1h, takes out, and moves in politef crucible, adds the hydrochloric acid 9mL, 15.7mol/LHNO of 12.0mol/L3 2mL, heats 30min, Add 11.6mol/L HClO41mL, 27.6mol/L Fluohydric acid. 5mL is heated to white cigarette and emits to the greatest extent, adds the salt of 12.0mol/L Acid 2mL, by 15ml deionized water rinsing sidewall of crucible, heating for dissolving, pours mensuration silicic acid manganese ore phase in 50mL color comparison tube.
Embodiment 4
(1) braunite 0.1 gram weighing 210 mesh is placed in 100mL beaker, and wherein Fe content is 45.88%, adds concentration and is The aluminum nitrate solution 50mL of 90g/L, cap upper surface ware, put in 92 DEG C of water-baths, after again reaching 92 DEG C etc. water temperature, start meter Time, every stirring in 8 minutes once, (after noticing that the water in water-bath reduces, 92 DEG C of hot water should be added), water-bath 30min, fixed at a slow speed Amount filter paper filtering (for preventing from filtering, filter paper pulp to be added on filter paper), collects filtering residue, and filtrate measures manganese carbonate ore phase;
(2) filtering residue described in step (1) is put in former beaker together with filter paper, adds 50mL 70g/L oxammonium sulfate .-4% sulphuric acid molten Liquid, puts in 92 DEG C of water-baths, after again reaching 92 DEG C etc. water temperature, starts timing, every stirring in 10 minutes once, and water-bath 20min, quantitative filter paper filters (for preventing from filtering, filter paper pulp to be added on filter paper) at a slow speed, collects filtering residue, and filtrate measures manganese oxide ore Phase;
70g/L oxammonium sulfate .-4% sulfuric acid solution compound method is to weigh 70g oxammonium sulfate. to be dissolved in the sulphuric acid that 1L volume fraction is 4% In aqueous solution;
(3) putting in porcelain crucible by the filtering residue described in step (2) together with filter paper, put into Muffle furnace, low temperature rises to 680 DEG C of ashing 0.6h, takes out, and moves in politef crucible, adds the hydrochloric acid 7mL, 15.7mol/LHNO of 12.0mol/L3 3mL, heating 30min, adds 11.6mol/L HClO41mL, 27.6mol/L Fluohydric acid. 5mL is heated to white cigarette and emits to the greatest extent, adds The hydrochloric acid 2mL of 12.0mol/L, by 20ml deionized water rinsing sidewall of crucible, heating for dissolving, pours mensuration silicic acid in 50mL color comparison tube Manganese ore phase.
Embodiment 5
(1) pyrolusite 0.1 gram weighing 180 mesh is placed in 100mL beaker, and wherein Fe content is 54.68%, adds concentration and is The aluminum nitrate solution 50mL of 60g/L, cap upper surface ware, put in the water-bath boiled, after waiting water again to seethe with excitement, start timing, Every stirring in 10 minutes once, (after noticing that the water in water-bath reduces, boiling water should be added), water-bath 60min, at a slow speed quantitative filter paper Filtering (for preventing from filtering, filter paper pulp to be added on filter paper), collect filtering residue, filtrate measures manganese carbonate ore phase;
(2) filtering residue described in step (1) is put in former beaker together with filter paper, adds 50mL 50g/L oxammonium sulfate .-3% sulphuric acid molten Liquid, puts in the water-bath boiled, and after waiting water again to seethe with excitement, starts timing, every stirring in 10 minutes once, and water-bath 30min, slowly Speed quantitative filter paper filters (for preventing from filtering, filter paper pulp to be added on filter paper), collects filtering residue, and filtrate measures manganese oxide ore phase;
50g/L oxammonium sulfate .-3% sulfuric acid solution compound method is to weigh 50g oxammonium sulfate. to be dissolved in the sulphuric acid that 1L volume fraction is 3% In aqueous solution;
(3) putting in porcelain crucible by the filtering residue described in step (2) together with filter paper, put into Muffle furnace, low temperature rises to 700 DEG C of ashing 1h, takes out, and moves in politef crucible, adds the hydrochloric acid 9mL, 15.7mol/LHNO of 12.0mol/L3 3mL, heats 30min, Add 11.6mol/L HClO41mL, 27.6mol/L Fluohydric acid. 5mL is heated to white cigarette and emits to the greatest extent, adds the salt of 12.0mol/L Acid 2mL, by 10ml deionized water rinsing sidewall of crucible, heating for dissolving, pours mensuration silicic acid manganese ore phase in 50mL color comparison tube.
Embodiment 6
(1) weighing 160 mesh rhodonite 0.1 gram to be placed in 100mL beaker, wherein Fe content is 25.43%, adds concentration and is The aluminum nitrate solution 50mL of 50g/L, cap upper surface ware, put in the water-bath boiled, after waiting water again to seethe with excitement, start timing, Every stirring in 10 minutes once, (after noticing that the water in water-bath reduces, boiling water should be added), water-bath 60min, at a slow speed quantitative filter paper Filtering (for preventing from filtering, filter paper pulp to be added on filter paper), collect filtering residue, filtrate measures manganese carbonate ore phase;
(2) filtering residue described in step (1) is put in former beaker together with filter paper, adds 50mL 30g/L oxammonium sulfate .-1% sulphuric acid molten Liquid, puts in the water-bath boiled, and after waiting water again to seethe with excitement, starts timing, every stirring in 10 minutes once, and water-bath 30min, slowly Speed quantitative filter paper filters (for preventing from filtering, filter paper pulp to be added on filter paper), collects filtering residue, and filtrate measures manganese oxide ore phase;
30g/L oxammonium sulfate .-1% sulfuric acid solution compound method is to weigh 30g oxammonium sulfate. to be dissolved in the sulphuric acid that 1L volume fraction is 1% In aqueous solution;
(3) putting in porcelain crucible by the filtering residue described in step (2) together with filter paper, put into Muffle furnace, low temperature rises to 700 DEG C of ashing 1h, takes out, and moves in politef crucible, adds the hydrochloric acid 9mL, 15.7mol/LHNO of 12.0mol/L3 3mL, heats 30min, Add 11.6mol/L HClO41mL, 27.6mol/L Fluohydric acid. 5mL is heated to white cigarette and emits to the greatest extent, adds the salt of 12.0mol/L Acid 2mL, by 15ml deionized water rinsing sidewall of crucible, heating for dissolving, pours mensuration silicic acid manganese ore phase in 50mL color comparison tube.
Embodiment 7
(1) weighing 180 mesh pyrolusite 0.1 gram to be placed in 100mL beaker, wherein Fe content is 33.72%, and addition concentration is 50g/L Aluminum nitrate solution 50mL, cap upper surface ware, put in the water-bath boiled, after waiting water again to seethe with excitement, start timing, every 10 Once, (after noticing that the water in water-bath reduces, should add boiling water), water-bath 60min, quantitative filter paper filters at a slow speed for minute stirring (for preventing from filtering, filter paper pulp to be added on filter paper), collects filtering residue, and filtrate measures manganese carbonate ore phase;
(2) filtering residue described in step (1) is put in former beaker together with filter paper, adds 50mL 40g/L oxammonium sulfate .-2% sulphuric acid molten Liquid, puts in the water-bath boiled, and after waiting water again to seethe with excitement, starts timing, every stirring in 10 minutes once, and water-bath 30min, slowly Speed quantitative filter paper filters (for preventing from filtering, filter paper pulp to be added on filter paper), collects filtering residue, and filtrate measures manganese oxide ore phase;
40g/L oxammonium sulfate .-2% sulfuric acid solution compound method is to weigh 40g oxammonium sulfate. to be dissolved in the sulphuric acid that 1L volume fraction is 2% In aqueous solution;
(3) putting in porcelain crucible by the filtering residue described in step (2) together with filter paper, put into Muffle furnace, low temperature rises to 700 DEG C of ashing 1h, takes out, and moves in politef crucible, adds the hydrochloric acid 9mL, 15.7mol/LHNO of 12.0mol/L3 3mL, heats 30min, Add 11.6mol/L HClO41mL, 27.6mol/L Fluohydric acid. 5mL is heated to white cigarette and emits to the greatest extent, adds the salt of 12.0mol/L Acid 2mL, by 15ml deionized water rinsing sidewall of crucible, heating for dissolving, pours mensuration silicic acid manganese ore phase in 50mL color comparison tube.
Comparative example 1
Weighing manganese ore to be placed in 100mL beaker, addition volume fraction is 1%HClO4 40mL, cap upper surface ware, put into and boil Water-bath in, after waiting water again to seethe with excitement, start timing, every stirring in 10 minutes once, (notice that the water in water-bath reduces After, boiling water should be added), water-bath 30min;Wherein manganese ore chooses manganese ore used in embodiment 1-7 successively, and remaining operation is with real Execute example 1.
Comparative example 2
Weighing manganese ore to be placed in 100mL beaker, addition PH is 2, concentration is the (NH of 130g/L4)2SO4Solution 50 mL, covers Surface plate, puts in 65 DEG C of water-baths, starts timing, every stirring in 10 minutes once, and water-bath 30min;Wherein manganese ore is successively Choosing manganese ore used in embodiment 1-7, remaining operation is with embodiment 1.
Comparative example 3
Weighing manganese ore to be placed in 100mL beaker, addition PH is 2, concentration is the (NH of 130g/L4)2SO4Solution 25mL, room temperature is stirred Mix 4h;Wherein manganese ore chooses manganese ore used in embodiment 1-7 successively, and remaining operation is with embodiment 1.
Manganese carbonate ore Within Monominerals leaching experiment analysis in above-described embodiment and comparative example is measured, use atomic absorption method or Ammonium persulfate. oxidation volumetric determination ferrous ammonium sulfate Fe content, it the results are shown in Table 1:
Table 1 Manganous Carbonate in Manganese Ores phase leaching experiment ω (Mn)/10-2
Aluminum nitrate solution is to other phase leaching rate≤1.2% in addition to manganese carbonate as can be seen from the above table, much lower string item Impact, be better than existing three kinds of methods.
Comparative example 4
(1) weighing manganese ore to be placed in 100mL beaker, addition concentration is the aluminum nitrate solution 50mL of 50g/L, cap upper surface ware, Put in the water-bath boiled, after waiting water again to seethe with excitement, start timing, every stirring in 10 minutes once, (note in water-bath After water reduces, boiling water should be added), water-bath 60min, quantitative filter paper filters (for preventing from filtering, filter paper pulp to be added on filter paper) at a slow speed, Collecting filtering residue, filtrate measures manganese carbonate ore phase;
(2) filtering residue described in step (1) is put in beaker together with filter paper, and adding 30mL volume fraction is the H of 33%2SO3Room temperature is soaked Carrying 30min, quantitative filter paper filters at a slow speed, collects filtering residue, and filtrate measures manganese oxide ore phase;
Wherein manganese ore chooses manganese ore used in embodiment 3-7 successively, and remaining operation is with embodiment 1.
Comparative example 5
(1) weigh manganese ore to be placed in 100mL beaker, pulverize, add the aluminum nitrate solution 50mL that concentration is 50g/L, cover table Face ware, puts in the water-bath boiled, and after waiting water again to seethe with excitement, starts timing, every stirring in 10 minutes once, (notes water-bath After water in Guo reduces, boiling water should be added), water-bath 60min, quantitative filter paper filtration at a slow speed (for preventing from filtering, filter to be added on filter paper Paper pulp), collect filtering residue, filtrate measures manganese carbonate ore phase;
(2) filtering residue described in step (1) is put in beaker together with filter paper, adds 1mol/LH2SO430mL, 0.066gKF and 3mL Fluohydric acid., cap upper surface ware, put into leaching 60min in the water-bath that temperature is 95 DEG C, quantitative filter paper filters (for preventing at a slow speed Filter, filter paper pulp to be added on filter paper), collect filtering residue, filtrate measures manganese oxide ore phase;
Wherein manganese ore chooses manganese ore used in embodiment 3-7 successively, and remaining operation is with embodiment 1.
Measuring manganese oxide leaching experiment analysis in embodiment 3-7, comparative example 4 and comparative example 5, it the results are shown in Table 2
Manganese oxide phase leaching experiment ω (Mn)/10 in table 2 manganese ore-2
As can be seen from the above table, the 2 kinds of leaching agents provided for " rock mineral analysis " and the oxammonium sulfate .-sulfur of present invention research Acid solution carries out leaching experiment and compares, oxammonium sulfate .-sulphuric acid leaching rate >=99.5% monomineralic to manganese oxide, is far superior to existing The 2 kinds of methods having.

Claims (9)

1. a manganese ore Phase Analysis, it is characterised in that employing following steps:
(1) weigh manganese ore, pulverize;
(2) adding aluminum nitrate aqueous solution, leaching in the manganese ore after step (1) is pulverized, filter, collect filtering residue, filtrate measures carbon Acid manganese ore phase;
(3) adding oxammonium sulfate .-sulfuric acid solution, leaching in the filtering residue that step (2) is collected, filter, collect filtering residue, filtrate measures oxygen Change manganese ore phase;
(4), after the ashing of step (3) described filtering residue, add the mixed-acid dissolution comprising nitrate acid and hydrofluoric acid-perchloric acid, measure silicic acid Manganese ore phase.
A kind of manganese ore Phase Analysis the most according to claim 1, it is characterised in that the nitric acid described in step (2) The concentration of aluminum solutions is 40-80g/L;The temperature of step (2) and step (3) described leaching is 95-100 DEG C;Step (4) is described In mixed acid, the mol ratio of nitric acid, Fluohydric acid. and perchloric acid is 47:138:12.
A kind of manganese ore Phase Analysis the most according to claim 1, it is characterised in that the sulphuric acid described in step (3) The concentration of azanol-sulfuric acid solution is 30-50g/L;Compound method is 1-for weigh 30-50g oxammonium sulfate. being dissolved in 1L volume fraction In the aqueous sulfuric acid of 3%.
A kind of manganese ore Phase Analysis the most according to claim 1, it is characterised in that the mixing described in step (4) The addition sequence of acid, for being initially charged nitric acid, after heating 30min, adds perchloric acid and Fluohydric acid..
A kind of manganese ore Phase Analysis the most according to claim 1, it is characterised in that the mixing described in step (4) Acid also includes hydrochloric acid;The mol ratio of nitric acid, Fluohydric acid., perchloric acid and hydrochloric acid is 47:138:12:(60-120).
A kind of manganese ore Phase Analysis the most according to claim 1, it is characterised in that step (2) and step (3) institute The filtration stated all uses chronic quantitative filter paper to filter.
A kind of manganese ore Phase Analysis the most according to claim 1, it is characterised in that step (1) described pulverizing Granularity is 160-200 mesh.
8. according to a kind of manganese ore Phase Analysis described in any one of claim 1-7, it is characterised in that concrete operations side Method is:
(1) weigh manganese ore, be crushed to 160-200 mesh;
(2) weighing the manganese ore 0.1-0.2g after step (1) is pulverized to be placed in 100mL beaker, adding 50ml concentration is 40-80g/ L aluminum nitrate solution, cap upper surface ware, put in 95-100 DEG C of water-bath, intermittent stirring, water-bath 40-60min, it is cooled to room temperature, Filtering, collect filtering residue, filtrate measures manganese carbonate ore phase;
(3) adding 50mL concentration in the filtering residue that step (2) is collected is 30-50g/L oxammonium sulfate .-sulfuric acid solution, cap upper surface ware, Put in the water-bath of 95-100 DEG C, intermittent stirring, water-bath 20-30min, it is cooled to room temperature, filters, collect filtering residue, filtrate is surveyed Determine manganese carbonate ore phase;30-50g/L oxammonium sulfate .-sulfuric acid solution compound method is dissolved in 1L volume for weighing 30-50g oxammonium sulfate. Mark is in the aqueous sulfuric acid of 1-3%;
(4) filtering residue described in step (3) is put in porcelain crucible, put into Muffle furnace, rise to 700 DEG C of ashing 1h, take out, move into poly- In tetrafluoroethene crucible, add the hydrochloric acid 9mL, 15.7mol/LHNO of 12.0mol/L3 3mL, heats 30min, adds 11.6mol/ L HClO41mL, 27.6mol/L Fluohydric acid. 5mL, is heated to white cigarette and emits to the greatest extent, add the hydrochloric acid 2mL of 12.0mol/L, go with 10-15ml Ionized water rinses sidewall of crucible, heating for dissolving, measures silicic acid manganese ore phase.
A kind of manganese ore Phase Analysis the most according to claim 8, it is characterised in that step (2) and step (3) institute The intermittent stirring stated is for stirring once every 10min.
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CN110286154A (en) * 2019-07-23 2019-09-27 长安大学 A kind of method of complete resolution manganese ore sample
CN111551509A (en) * 2020-05-15 2020-08-18 广东省资源综合利用研究所 Chemical quantitative analysis method for occurrence state of silver in iron-manganese oxidized ore

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Publication number Priority date Publication date Assignee Title
CN106370510A (en) * 2016-10-21 2017-02-01 天津大学 Method for microwave digestion of glass body
CN108020857A (en) * 2016-11-03 2018-05-11 中国辐射防护研究院 A kind of method that polonium leaches in aerosol
WO2019167841A1 (en) * 2018-03-01 2019-09-06 Jfeスチール株式会社 Method for manufacturing manganese raw material and method for smelting manganese-containing steel
KR20200112947A (en) * 2018-03-01 2020-10-05 제이에프이 스틸 가부시키가이샤 Manufacturing method of manganese raw material and solvent method of manganese-containing steel
KR102449547B1 (en) 2018-03-01 2022-09-29 제이에프이 스틸 가부시키가이샤 Manufacturing method of manganese raw material and melting method of manganese-containing steel
CN110286154A (en) * 2019-07-23 2019-09-27 长安大学 A kind of method of complete resolution manganese ore sample
CN110286154B (en) * 2019-07-23 2021-08-17 长安大学 Method for completely digesting manganese ore sample for element analysis
CN111551509A (en) * 2020-05-15 2020-08-18 广东省资源综合利用研究所 Chemical quantitative analysis method for occurrence state of silver in iron-manganese oxidized ore

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