CN105866387B - A kind of manganese ore Phase Analysis - Google Patents
A kind of manganese ore Phase Analysis Download PDFInfo
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- CN105866387B CN105866387B CN201610432502.0A CN201610432502A CN105866387B CN 105866387 B CN105866387 B CN 105866387B CN 201610432502 A CN201610432502 A CN 201610432502A CN 105866387 B CN105866387 B CN 105866387B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/24—Earth materials
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
Abstract
The present invention relates to a kind of analysis determining methods of specific compound in ore, are specifically related to a kind of manganese ore Phase Analysis.Manganese ore Phase Analysis in the present invention, which is characterized in that using following steps：（1）Manganese ore is weighed, is crushed；（2）Aluminum nitrate aqueous solution is added in manganese ore after crushing, is leached, filter residue is collected in filtering, and filtrate measures manganese carbonate ore phase；（3）Step（2）Hydroxyl sulfate sulfuric acid solution is added in the filter residue of collection, is leached, filter residue is collected in filtering, and filtrate measures manganese oxide ore phase；（4）Step（3）After the filter residue ashing, the mixed-acid dissolution for including nitric hydrofluoric acid perchloric acid is added in, measures silicic acid manganese ore phase.The present invention provides a kind of accurate, succinct manganese ore Phase Analysis, the influence of string phase in leaching process is greatly reduced, precision of analysis is improved, it is larger to solve error in traditional manganese ore Phase Analysis, the problem of string is mutually serious, and efficiency is low.
Description
Technical field
The present invention relates to a kind of analysis determining methods of specific compound in ore, are specifically related to a kind of manganese ore object phase
Analysis method.
Background technology
The material phase analysis of manganese is the method for quantitatively determining for studying manganese difference preservation valence state or form and related reason in manganese ore
By.Manganese is very wide in distributed in nature, it is known that the mineral of manganese are there are about more than 150 kinds, existence form and industry in nature according to manganese
Purposes is usually only required to 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 the compound of these manganese shows certain solvent
To be different, the manganese mineral of variform is allowed to leach one by one in this way, is collected respectively, then measures containing for each component one by one
Amount.Also another solvent dissolution other components can be selected, and make to be intended to measure a certain component and stay in insoluble sludge, then measure residue
In the component content.
Chemical phase analysis is the method for studying existence and its content of the element in various carrier minerals, is geology
Prospecting looks for ore deposit, ore-dressing technique research and mineral resource assessment to provide basic information.Manganese ore material phase analysis in China's does not have skill at present
Art specification, analysis method Main Basiss《Rock mineral analysis》（4 editions Beijing：Geology Publishing House, 2011:856-861）It provides
Analysis process.But these methods, both for single mineral, none of these methods can be suitably used for most manganese ores.Example
The leaching agent for such as leaching manganese carbonate phase if it is for the leaching of manganese carbonate phase in manganese oxide ore, go here and there phase the phenomenon that will compare
Seriously, the accuracy of manganese carbonate phase result is influenced whether.And according to《Iron, manganese, chrome ore geological exploration norm》（DZ/T
0200-2002）It is required that as long as manganese object phase analysis manganese carbonate, manganese oxide and manganous silicate, and do not have in existing analysis method
To the method for manganese carbonate, manganese oxide and manganous silicate network analysis.
Invention content
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 the problem of error is larger, and string is mutually serious, efficiency is low.
To reach above-mentioned technique effect, the present invention adopts the following technical scheme that：
A kind of manganese ore Phase Analysis, using following steps：
（1）Manganese ore is weighed, is crushed；
（2）Step（1）Aluminum nitrate aqueous solution is added in manganese ore after crushing, is leached, filter residue is collected in filtering, and filtrate is surveyed
Determine manganese carbonate ore phase；
（3）Step（2）Hydroxyl sulfate-sulfuric acid solution is added in the filter residue of collection, is leached, filter residue is collected in filtering, and filtrate is surveyed
Determine manganese oxide ore phase；
（4）Step（3）After the filter residue ashing, the mixed-acid dissolution for including nitrate acid and hydrofluoric acid-perchloric acid is added in, is measured
Silicic acid manganese ore phase.
Preferably, step（1）A concentration of 40-80g/L of the aluminum nitrate solution；
Preferably, step（2）And step（3）The temperature of the leaching is 95-100 DEG C；
Preferably, step（4）The molar ratio of nitric acid, hydrofluoric acid and perchloric acid is 47 in the mixed acid：138：12.
Preferably, step（3）A concentration of 30-50g/L of the hydroxyl sulfate-sulfuric acid solution；Preparation method is weighs
30-50g hydroxyl sulfate is dissolved in the aqueous sulfuric acid that 1L volume fractions are 1-3%.
Preferably, step（4）The addition sequence of the mixed acid after heating 30min, adds height first to add in nitric acid
Chloric acid and hydrofluoric acid.
Step（4）The mixed acid further includes hydrochloric acid；Nitric acid, hydrofluoric acid, perchloric acid and hydrochloric acid molar ratio be 47:
138:12：（60-120）.
Preferably, step（2）And step（3）The filtering is filtered using chronic quantitative filter paper.
Preferably, step（1）The granularity of the crushing is 160-200 mesh.
A kind of manganese ore Phase Analysis, concrete operation method are：
（1）Manganese ore is weighed, is crushed to 160-200 mesh；
（2）Weigh step（1）Manganese ore 0.1-0.2g after crushing is placed in 100mL beakers, adds in a concentration of 40- of 50ml
80g/L aluminum nitrate solutions, cap upper surface ware are put into 95-100 DEG C of water-bath, intermittent stirring, and water-bath 40-60min is cooled to
Filter residue is collected in room temperature, filtering, and filtrate measures manganese carbonate ore phase；Preferably, intermittent stirring is primary every 10min stirrings；
（3）Step（2）A concentration of 30-50g/L hydroxyl sulfate-sulfuric acid solutions of 50mL are added in the filter residue of collection, cover table
Face ware, is put into 95-100 DEG C of water-bath, intermittent stirring, and water-bath 20-30min is cooled to room temperature, filtering, collects filter residue, filter
Liquid measures manganese carbonate ore phase；30-50g/L hydroxyl sulfate-sulfuric acid solution preparation method is dissolved in 1L to weigh 30-50g hydroxyl sulfate
Volume fraction is in the aqueous sulfuric acid of 1-3%；Preferably, intermittent stirring is primary every 10min stirrings；
（4）By step（3）The filter residue is put into porcelain crucible, is put into Muffle furnace, is risen to 700 DEG C of ashing 1h, is taken out, move
Enter in polytetrafluoroethylene (PTFE) crucible, add the hydrochloric acid 9mL, 15.7mol/LHNO of 12.0mol/L3 3mL heats 30min, adds
11.6mol/L HClO41mL, 27.6mol/L hydrofluoric acid 5mL are heated to white cigarette and emit the hydrochloric acid 2mL for the greatest extent, adding 12.0mol/L, uses
10-15ml deionized waters rinse sidewall of crucible, dissolve by heating, and measure silicic acid manganese ore phase.
The present invention establishes a kind of Phase Analysis for being suitable for most manganese ores, passes through 8 or more laboratories
The precision coordinated trials participated in jointly, it is determined that repeatability limit and the reproducibility limit of analysis method scientifically have evaluated foundation
Manganese ore Phase Analysis quality level, in laboratory and the quality control of laboratory monitoring chemical phase analysis provide
The foundation of science.The present invention for the first time evaluates manganese ore Phase Analysis accuracy, by rock-mineral determination and not
With the contrast test of method, system contrast verification is carried out to method of chemical phase analysis, to lack the analysis side of standard substance
Method accuracy estimating provides referential technical method and means.
Advantageous effect
（1）The present invention provides a kind of accurate, succinct manganese ore Phase Analysis, use aluminum nitrate solution, sulfuric acid
Azanol-sulfuric acid solution and mixed acid respectively mutually leach manganese carbonate phase, the manganese oxide phase in manganese ore with manganous silicate, significantly
The influence of string phase in leaching process is reduced, precision of analysis is improved, solves traditional manganese ore material phase analysis side
The problem of error is larger in method, and string is mutually serious, and efficiency is low.
（2）The present invention establishes a kind of Phase Analysis for being suitable for most manganese ores, and for the first time to manganese ore
Phase Analysis correctness is evaluated.
Specific embodiment
The present invention is further illustrated with comparative example in conjunction with the embodiments, it should explanation, the description below be only for
It explains the present invention, its content is not defined.
Embodiment 1
（1）The manganese spar 0.1g for weighing 160 mesh is placed in 100mL beakers, and wherein manganese content is 21.08%, is added in a concentration of
The aluminum nitrate solution 50mL of 40g/L, cap upper surface ware are put into the water-bath boiled, after water is waited to boil again, start timing,
It is primary every stirring in 8 minutes,（After noticing that the water in water-bath is reduced, boiling water should be added）, water-bath 40min, quantitative filter paper at a slow speed
Filtering（To prevent filter, to add filter paper pulp on filter paper）, filter residue is collected, filtrate measures manganese carbonate ore phase；
（2）Step（1）The filter residue is put into together with filter paper in former beaker, adds in -1% sulphur of 50mL 30g/L hydroxyl sulfate
Acid solution is put into the water-bath boiled, after water is waited to boil again, starts timing, primary every stirring in 10 minutes, water-bath
20min, at a slow speed quantitative filter paper filtering（To prevent filter, to add filter paper pulp on filter paper）, filter residue is collected, filtrate measures manganese oxide ore
Phase；- 1% sulfuric acid solution preparation method of 30g/L hydroxyl sulfate is to weigh 30g hydroxyl sulfate to be dissolved in the sulfuric acid that 1L volume fractions are 1%
In aqueous solution；
(3) by step（2）The filter residue is put into together with filter paper in porcelain crucible, is put into Muffle furnace, and low temperature rises to 700 DEG C of ashes
Change 1h, take out, move into polytetrafluoroethylene (PTFE) crucible, add the hydrochloric acid 9mL, 15.7mol/LHNO of 12.0mol/L3 3mL, heating
30min adds 11.6mol/L HClO41mL, 27.6mol/L hydrofluoric acid 5mL are heated to white cigarette and emit to the greatest extent, add
The hydrochloric acid 2mL of 12.0mol/L rinses sidewall of crucible with 10ml deionized waters, dissolves by heating, pour in 50mL colorimetric cylinders and measure silicic acid
Manganese ore phase.
Embodiment 2
（1）The manganese spar 0.2g for weighing 200 mesh is placed in 100mL beakers, and wherein manganese content is 19.77%, is added in a concentration of
The aluminum nitrate solution 50mL of 50g/L, cap upper surface ware are put into 95 DEG C of water-baths, etc. after water temperatures reach 95 DEG C again, start to count
When, it is primary every stirring in 10 minutes,（After noticing that the water in water-bath is reduced, 95 DEG C of hot water should be added）, water-bath 60min, at a slow speed
Quantitative filter paper filters（To prevent filter, to add filter paper pulp on filter paper）, filter residue is collected, filtrate measures manganese carbonate ore phase；
（2）Step（1）The filter residue is put into together with filter paper in former beaker, adds in -3% sulphur of 50mL 30g/L hydroxyl sulfate
Acid solution is put into 95 DEG C of water-baths, etc. after water temperatures reach 95 DEG C again, start timing, water-bath primary every stirring in 10 minutes
30min, at a slow speed quantitative filter paper filtering（To prevent filter, to add filter paper pulp on filter paper）, filter residue is collected, filtrate measures manganese oxide ore
Phase；- 3% sulfuric acid solution preparation method of 30g/L hydroxyl sulfate is to weigh 30g hydroxyl sulfate to be dissolved in the sulfuric acid that 1L volume fractions are 3%
In aqueous solution；
(3) by step（2）The filter residue is put into together with filter paper in porcelain crucible, is put into Muffle furnace, and low temperature rises to 650 DEG C of ashes
Change 1h, take out, move into polytetrafluoroethylene (PTFE) crucible, add the hydrochloric acid 8mL, 15.7mol/LHNO of 12.0mol/L3 3mL, heating
30min adds 11.6mol/L HClO41mL, 27.6mol/L hydrofluoric acid 5mL are heated to white cigarette and emit to the greatest extent, add
The hydrochloric acid 2mL of 12.0mol/L rinses sidewall of crucible with 15ml deionized waters, dissolves by heating, pour in 50mL colorimetric cylinders and measure silicic acid
Manganese ore phase.
Embodiment 3
（1）The manganite 0.1g for weighing 150 mesh is placed in 100mL beakers, and wherein manganese content is 46.34%, is added in a concentration of
The aluminum nitrate solution 50mL of 30g/L, cap upper surface ware are put into the water-bath boiled, after water is waited to boil again, start timing,
It is primary every stirring in 10 minutes,（After noticing that the water in water-bath is reduced, boiling water should be added）, water-bath 70min, quantitative filter paper at a slow speed
Filtering（To prevent filter, to add filter paper pulp on filter paper）, filter residue is collected, filtrate measures manganese carbonate ore phase；
（2）Step（1）The filter residue is put into together with filter paper in former beaker, adds in -3% sulphur of 50mL 50g/L hydroxyl sulfate
Acid solution is put into the water-bath boiled, after water is waited to boil again, starts timing, primary every stirring in 10 minutes, water-bath
30min, at a slow speed quantitative filter paper filtering（To prevent filter, to add filter paper pulp on filter paper）, filter residue is collected, filtrate measures manganese oxide ore
Phase；- 3% sulfuric acid solution preparation method of 50g/L hydroxyl sulfate is to weigh 50g hydroxyl sulfate to be dissolved in the sulfuric acid that 1L volume fractions are 3%
In aqueous solution；
(3) by step（2）The filter residue is put into together with filter paper in porcelain crucible, is put into Muffle furnace, and low temperature rises to 700 DEG C of ashes
Change 1h, take out, move into polytetrafluoroethylene (PTFE) crucible, add the hydrochloric acid 9mL, 15.7mol/LHNO of 12.0mol/L3 2mL, heating
30min adds 11.6mol/L HClO41mL, 27.6mol/L hydrofluoric acid 5mL are heated to white cigarette and emit to the greatest extent, add
The hydrochloric acid 2mL of 12.0mol/L rinses sidewall of crucible with 15ml deionized waters, dissolves by heating, pour in 50mL colorimetric cylinders and measure silicic acid
Manganese ore phase.
Embodiment 4
（1）0.1 gram of braunite for weighing 210 mesh is placed in 100mL beakers, and wherein manganese content is 45.88%, adds in concentration
For the aluminum nitrate solution 50mL of 90g/L, cap upper surface ware is put into 92 DEG C of water-baths, etc. after water temperatures reach 92 DEG C again, start
Timing, it is primary every stirring in 8 minutes,（After noticing that the water in water-bath is reduced, 92 DEG C of hot water should be added）, water-bath 30min, at a slow speed
Quantitative filter paper filters（To prevent filter, to add filter paper pulp on filter paper）, filter residue is collected, filtrate measures manganese carbonate ore phase；
（2）Step（1）The filter residue is put into together with filter paper in former beaker, adds in -4% sulphur of 50mL 70g/L hydroxyl sulfate
Acid solution is put into 92 DEG C of water-baths, etc. after water temperatures reach 92 DEG C again, start timing, water-bath primary every stirring in 10 minutes
20min, at a slow speed quantitative filter paper filtering（To prevent filter, to add filter paper pulp on filter paper）, filter residue is collected, filtrate measures manganese oxide ore
Phase；
- 4% sulfuric acid solution preparation method of 70g/L hydroxyl sulfate is that weigh 70g hydroxyl sulfate to be dissolved in 1L volume fractions be 4%
In aqueous sulfuric acid；
(3) by step（2）The filter residue is put into together with filter paper in porcelain crucible, is put into Muffle furnace, and low temperature rises to 680 DEG C of ashes
Change 0.6h, take out, move into polytetrafluoroethylene (PTFE) crucible, add the hydrochloric acid 7mL, 15.7mol/LHNO of 12.0mol/L3 3mL, heating
30min adds 11.6mol/L HClO41mL, 27.6mol/L hydrofluoric acid 5mL are heated to white cigarette and emit to the greatest extent, add
The hydrochloric acid 2mL of 12.0mol/L rinses sidewall of crucible with 20ml deionized waters, dissolves by heating, pour in 50mL colorimetric cylinders and measure silicic acid
Manganese ore phase.
Embodiment 5
（1）0.1 gram of pyrolusite for weighing 180 mesh is placed in 100mL beakers, and wherein manganese content is 54.68%, adds in concentration
For the aluminum nitrate solution 50mL of 60g/L, cap upper surface ware is put into the water-bath boiled, after water is waited to boil again, starts to count
When, it is primary every stirring in 10 minutes,（After noticing that the water in water-bath is reduced, boiling water should be added）, water-bath 60min, at a slow speed quantitatively
Filter paper filters（To prevent filter, to add filter paper pulp on filter paper）, filter residue is collected, filtrate measures manganese carbonate ore phase；
（2）Step（1）The filter residue is put into together with filter paper in former beaker, adds in -3% sulphur of 50mL 50g/L hydroxyl sulfate
Acid solution is put into the water-bath boiled, after water is waited to boil again, starts timing, primary every stirring in 10 minutes, water-bath
30min, at a slow speed quantitative filter paper filtering（To prevent filter, to add filter paper pulp on filter paper）, filter residue is collected, filtrate measures manganese oxide ore
Phase；
- 3% sulfuric acid solution preparation method of 50g/L hydroxyl sulfate is that weigh 50g hydroxyl sulfate to be dissolved in 1L volume fractions be 3%
In aqueous sulfuric acid；
(3) by step（2）The filter residue is put into together with filter paper in porcelain crucible, is put into Muffle furnace, and low temperature rises to 700 DEG C of ashes
Change 1h, take out, move into polytetrafluoroethylene (PTFE) crucible, add the hydrochloric acid 9mL, 15.7mol/LHNO of 12.0mol/L3 3mL, heating
30min adds 11.6mol/L HClO41mL, 27.6mol/L hydrofluoric acid 5mL are heated to white cigarette and emit to the greatest extent, add
The hydrochloric acid 2mL of 12.0mol/L rinses sidewall of crucible with 10ml deionized waters, dissolves by heating, pour in 50mL colorimetric cylinders and measure silicic acid
Manganese ore phase.
Embodiment 6
（1）It weighs 0.1 gram of 160 mesh rhodonite to be placed in 100mL beakers, wherein manganese content is 25.43%, adds in concentration
For the aluminum nitrate solution 50mL of 50g/L, cap upper surface ware is put into the water-bath boiled, after water is waited to boil again, starts to count
When, it is primary every stirring in 10 minutes,（After noticing that the water in water-bath is reduced, boiling water should be added）, water-bath 60min, at a slow speed quantitatively
Filter paper filters（To prevent filter, to add filter paper pulp on filter paper）, filter residue is collected, filtrate measures manganese carbonate ore phase；
（2）Step（1）The filter residue is put into together with filter paper in former beaker, adds in -1% sulphur of 50mL 30g/L hydroxyl sulfate
Acid solution is put into the water-bath boiled, after water is waited to boil again, starts timing, primary every stirring in 10 minutes, water-bath
30min, at a slow speed quantitative filter paper filtering（To prevent filter, to add filter paper pulp on filter paper）, filter residue is collected, filtrate measures manganese oxide ore
Phase；
- 1% sulfuric acid solution preparation method of 30g/L hydroxyl sulfate is that weigh 30g hydroxyl sulfate to be dissolved in 1L volume fractions be 1%
In aqueous sulfuric acid；
(3) by step（2）The filter residue is put into together with filter paper in porcelain crucible, is put into Muffle furnace, and low temperature rises to 700 DEG C of ashes
Change 1h, take out, move into polytetrafluoroethylene (PTFE) crucible, add the hydrochloric acid 9mL, 15.7mol/LHNO of 12.0mol/L3 3mL, heating
30min adds 11.6mol/L HClO41mL, 27.6mol/L hydrofluoric acid 5mL are heated to white cigarette and emit to the greatest extent, add
The hydrochloric acid 2mL of 12.0mol/L rinses sidewall of crucible with 15ml deionized waters, dissolves by heating, pour in 50mL colorimetric cylinders and measure silicic acid
Manganese ore phase.
Embodiment 7
（1）It weighs 0.1 gram of 180 mesh pyrolusite to be placed in 100mL beakers, wherein manganese content is 33.72%, is added in a concentration of
The aluminum nitrate solution 50mL of 50g/L, cap upper surface ware are put into the water-bath boiled, after water is waited to boil again, start timing,
It is primary every stirring in 10 minutes,（After noticing that the water in water-bath is reduced, boiling water should be added）, water-bath 60min, quantitative filter paper at a slow speed
Filtering（To prevent filter, to add filter paper pulp on filter paper）, filter residue is collected, filtrate measures manganese carbonate ore phase；
（2）Step（1）The filter residue is put into together with filter paper in former beaker, adds in -2% sulphur of 50mL 40g/L hydroxyl sulfate
Acid solution is put into the water-bath boiled, after water is waited to boil again, starts timing, primary every stirring in 10 minutes, water-bath
30min, at a slow speed quantitative filter paper filtering（To prevent filter, to add filter paper pulp on filter paper）, filter residue is collected, filtrate measures manganese oxide ore
Phase；
- 2% sulfuric acid solution preparation method of 40g/L hydroxyl sulfate is that weigh 40g hydroxyl sulfate to be dissolved in 1L volume fractions be 2%
In aqueous sulfuric acid；
(3) by step（2）The filter residue is put into together with filter paper in porcelain crucible, is put into Muffle furnace, and low temperature rises to 700 DEG C of ashes
Change 1h, take out, move into polytetrafluoroethylene (PTFE) crucible, add the hydrochloric acid 9mL, 15.7mol/LHNO of 12.0mol/L3 3mL, heating
30min adds 11.6mol/L HClO41mL, 27.6mol/L hydrofluoric acid 5mL are heated to white cigarette and emit to the greatest extent, add
The hydrochloric acid 2mL of 12.0mol/L rinses sidewall of crucible with 15ml deionized waters, dissolves by heating, pour in 50mL colorimetric cylinders and measure silicic acid
Manganese ore phase.
Comparative example 1
It weighs manganese ore to be placed in 100mL beakers, addition volume fraction is 1%HClO4 40mL, cap upper surface ware, is put into
In the water-bath of boiling, after water is waited to boil again, start timing, it is primary every stirring in 10 minutes,（Notice that the water in water-bath is reduced
Afterwards, boiling water should be added）, water-bath 30min；Wherein manganese ore chooses manganese ore used in embodiment 1-7 successively, remaining operation is the same as real
Apply example 1.
Comparative example 2
It weighs manganese ore to be placed in 100mL beakers, it is 2, a concentration of 130g/L's to add in PH（NH4）2SO450 mL of solution,
Cap upper surface ware is put into 65 DEG C of water-baths, starts timing, primary every stirring in 10 minutes, water-bath 30min；Wherein manganese ore
Manganese ore used in embodiment 1-7 is chosen successively, remaining operation is the same as embodiment 1.
Comparative example 3
It weighs manganese ore to be placed in 100mL beakers, it is 2, a concentration of 130g/L's to add in PH（NH4）2SO4Solution 25mL, room
Temperature stirring 4h；Wherein manganese ore chooses manganese ore used in embodiment 1-7 successively, remaining operation is the same as embodiment 1.
Manganese carbonate ore Within Monominerals leaching experiment analysis in above-described embodiment and comparative example is measured, using atomic absorption method or
Ammonium persulfate aoxidizes volumetric determination ferrous ammonium sulfate manganese content, and the result is shown in tables 1：
1 Manganous Carbonate in Manganese Ores phase leaching experiment ω of table（Mn）/10-2
Aluminum nitrate solution is to other phase leaching rate≤1.2% in addition to manganese carbonate, much lower as can be seen from the above table
The influence of string item, better than existing three kinds of methods.
Comparative example 4
（1）It weighs manganese ore to be placed in 100mL beakers, adds in the aluminum nitrate solution 50mL of a concentration of 50g/L, cap upper surface
Ware is put into the water-bath boiled, after water is waited to boil again, starts timing, primary every stirring in 10 minutes,（Pay attention to water-bath
In water reduce after, boiling water should be added）, water-bath 60min, quantitative filter paper filtering at a slow speed（To prevent filter, to add filter paper on filter paper
Slurry）, filter residue is collected, filtrate measures manganese carbonate ore phase；
（2）Step（1）The filter residue is put into together with filter paper in beaker, adds in the H that 30mL volume fractions are 33%2SO3Room
Filter residue is collected in temperature extraction 30min, at a slow speed quantitative filter paper filtering, and filtrate measures manganese oxide ore phase；
Wherein manganese ore chooses manganese ore used in embodiment 3-7 successively, remaining operation is the same as embodiment 1.
Comparative example 5
（1）It weighs manganese ore to be placed in 100mL beakers, crush, add in the aluminum nitrate solution 50mL of a concentration of 50g/L, lid
Upper surface ware is put into the water-bath boiled, after water is waited to boil again, starts timing, primary every stirring in 10 minutes,（Pay attention to
After water in water-bath is reduced, boiling water should be added）, water-bath 60min, quantitative filter paper filtering at a slow speed（It, will on filter paper to prevent filter
Add filter paper pulp）, filter residue is collected, filtrate measures manganese carbonate ore phase；
（2）Step（1）The filter residue is put into together with filter paper in beaker, adds in 1mol/LH2SO430mL, 0.066gKF and
3mL hydrofluoric acid, cap upper surface ware are put into the water-bath that temperature is 95 DEG C and leach 60min, and quantitative filter paper filters at a slow speed（To prevent
Filter will add filter paper pulp on filter paper）, filter residue is collected, filtrate measures manganese oxide ore phase；
Wherein manganese ore chooses manganese ore used in embodiment 3-7 successively, remaining operation is the same as embodiment 1.
Manganese oxide leaching experiment analysis in embodiment 3-7, comparative example 4 and comparative example 5 is measured, the result is shown in tables 2
Manganese oxide phase leaching experiment ω in 2 manganese ore of table（Mn）/10-2
As can be seen from the above table, for《Rock mineral analysis》The sulfuric acid hydroxyl that the 2 kinds of leaching agents provided are studied with the present invention
Amine-sulfuric acid solution carries out leaching experiment comparison, and hydroxyl sulfate-sulfuric acid monomineralic leaching rate >=99.5% to manganese oxide is much excellent
In existing 2 kinds of methods.
Claims (6)
1. a kind of manganese ore Phase Analysis, which is characterized in that using following steps：
（1）Manganese ore is weighed, is crushed；
（2）Step（1）Aluminum nitrate aqueous solution is added in manganese ore after crushing, is leached, filter residue is collected in filtering, and filtrate measures carbon
Sour manganese ore phase；
（3）Step（2）Hydroxyl sulfate-sulfuric acid solution is added in the filter residue of collection, is leached, filter residue is collected in filtering, and filtrate measures oxygen
Change manganese ore phase；
（4）Step（3）After the filter residue ashing, the mixed-acid dissolution for including nitrate acid and hydrofluoric acid-perchloric acid is added in, measures silicic acid
Manganese ore phase；
Wherein, step（2）A concentration of 40-80g/L of the aluminum nitrate solution；Step（2）And step（3）The temperature of the leaching
Degree is 95-100 DEG C；Step（4）The molar ratio of nitric acid, hydrofluoric acid and perchloric acid is 47 in the mixed acid：138：12；
Wherein, step（4）The addition sequence of the mixed acid is first adds in nitric acid, after heating 30min, add perchloric acid and
Hydrofluoric acid；
Wherein, step（1）The granularity of the crushing is 160-200 mesh.
A kind of 2. manganese ore Phase Analysis according to claim 1, which is characterized in that step（3）The sulfuric acid
A concentration of 30-50g/L of azanol-sulfuric acid solution；Preparation method is 1- to weigh 30-50g hydroxyl sulfate to be dissolved in 1L volume fractions
In 3% aqueous sulfuric acid.
A kind of 3. manganese ore Phase Analysis according to claim 1, which is characterized in that step（4）The mixing
Acid further includes hydrochloric acid；Nitric acid, hydrofluoric acid, perchloric acid and hydrochloric acid molar ratio be 47:138:12：（60-120）.
A kind of 4. manganese ore Phase Analysis according to claim 1, which is characterized in that step（2）And step（3）Institute
The filtering stated is filtered using chronic quantitative filter paper.
5. according to a kind of manganese ore Phase Analysis of claim 1-4 any one of them, which is characterized in that concrete operations side
Method is：
（1）Manganese ore is weighed, is crushed to 160-200 mesh；
（2）Weigh step（1）Manganese ore 0.1-0.2g after crushing is placed in 100mL beakers, adds in a concentration of 40-80g/ of 50ml
L aluminum nitrate solutions, cap upper surface ware are put into 95-100 DEG C of water-bath, intermittent stirring, and water-bath 40-60min is cooled to room temperature,
Filtering, collects filter residue, and filtrate measures manganese carbonate ore phase；
（3）Step（2）Addition a concentration of 30-50g/L hydroxyl sulfate-sulfuric acid solutions of 50mL in the filter residue of collection, cap upper surface ware,
It is put into 95-100 DEG C of water-bath, intermittent stirring, water-bath 20-30min is cooled to room temperature, filtering, collects filter residue, and filtrate is surveyed
Determine manganese oxide ore phase；30-50g/L hydroxyl sulfate-sulfuric acid solution preparation method is dissolved in 1L volumes to weigh 30-50g hydroxyl sulfate
Score is in the aqueous sulfuric acid of 1-3%；
（4）By step（3）The filter residue is put into porcelain crucible, is put into Muffle furnace, is risen to 700 DEG C of ashing 1h, is taken out, moves 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 hydrofluoric acid 5mL are heated to white cigarette and emit the hydrochloric acid 2mL for the greatest extent, adding 12.0mol/L, uses
10-15ml deionized waters rinse sidewall of crucible, dissolve by heating, and measure silicic acid manganese ore phase.
A kind of 6. manganese ore Phase Analysis according to claim 5, which is characterized in that step（2）And step（3）Institute
The intermittent stirring stated is primary every 10min stirrings.
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