CN114609000A - Judgment method for reducing magnetic effectiveness of pyrrhotite and application - Google Patents
Judgment method for reducing magnetic effectiveness of pyrrhotite and application Download PDFInfo
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- CN114609000A CN114609000A CN202210506484.1A CN202210506484A CN114609000A CN 114609000 A CN114609000 A CN 114609000A CN 202210506484 A CN202210506484 A CN 202210506484A CN 114609000 A CN114609000 A CN 114609000A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C1/00—Magnetic separation
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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
- G01N21/84—Systems specially adapted for particular applications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
- G01N23/2251—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
Abstract
The invention provides a judgment method for reducing the magnetic effectiveness of pyrrhotite and application thereof, and particularly relates to the technical field of mineral measurement. The method comprises the following steps: step a: adding an oxidant into the mineral to react to obtain an oxidized mineral; step b: sampling the oxidized minerals to prepare epoxy resin polished sections; step c: when the magnetite in the oxidized mineral has no oxidation coating edge, observing the coating condition of the oxidation product of the pyrrhotite in the mineral, and judging whether the coating is effective or ineffective; step d: repeating the step b to enable the observed pyrrhotite particles to reach N particles and recording the area S; step e: calculating the effective rate through the area S and judging the effectiveness. The method is convenient to measure, is easy to identify the coating condition of the pyrrhotite oxide, is more accurate in the measurement result of the magnetic reduction of the pyrrhotite, and is closer to actual production.
Description
Technical Field
The invention relates to the technical field of mineral measurement, in particular to a judgment method for reducing the magnetic effectiveness of pyrrhotite and application thereof.
Background
In the oxidation process of the strong magnetic monoclinic pyrrhotite, products such as weak magnetic ferric oxide and the like can be formed, and the magnetism of the whole particles is reduced to a certain degree. This property can be exploited when separation of monoclinic pyrrhotite from other strongly magnetic minerals, such as magnetite ore, is required during mineral processing. By adding the oxidant, oxides are generated on the surfaces of the pyrrhotite particles, so that the magnetic property between the pyrrhotite and the magnetite is greatly different, and the magnetic separation is realized.
The condition control of the oxidation process has an important effect on the quality of the whole production index, the stability of the process and the like, and if the oxidation degree of the pyrrhotite is insufficient and the magnetic difference is insufficient, effective separation still cannot be realized. When the oxidation degree is excessive, other minerals in the material can be oxidized to a certain degree, the magnetism of other magnetic minerals is changed, and the pyrrhotite cannot be separated from other magnetic minerals.
The existing ubiquitous problem is that although a corresponding process flow method is provided, due to the lack of a proper representation technical means, how to specifically judge the magnetism reduction of the pyrrhotite reaches a proper degree, the method is suitable for magnetic separation, and the judgment of the magnetic separation time is always based on experience and experimental groping, so that specific quantitative standards are difficult to be provided.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
One of the purposes of the invention is to provide a method for judging the magnetic effectiveness of pyrrhotite, which solves the technical problem that the magnetic effectiveness of pyrrhotite is judged by lacking a proper representation technical means and a specific quantitative standard in the prior art.
The second purpose of the invention is to provide the application of the judgment method for reducing the magnetic effectiveness of pyrrhotite in magnetic separation, so as to provide more accurate basis for guiding the actual production.
In order to solve the technical problems, the invention adopts the following technical scheme:
the first aspect of the invention provides a judgment method for reducing the magnetic regulation effectiveness of pyrrhotite, which comprises the following steps:
step a: adding an oxidant into the mineral to react to obtain an oxidized mineral;
step b: sampling the oxidized minerals to prepare epoxy resin polished sections;
step c: when other ferromagnetic minerals in the oxidized minerals have no oxidized coating edges, observing the coating condition of oxidized products of pyrrhotite in the minerals, and judging whether the coating is effective or ineffective;
step d: repeating the step b to enable the observed pyrrhotite particles to reach N particles and recording the area S;
step e: calculating the effective rate through the area S and judging the effectiveness.
Optionally, in step e, the effective rate γ =
Wherein S isIs effectiveTo coat the effective total area of the particles, SIs effectiveIs the total area of all particles observed.
Optionally, in the step c, when the coating proportion is more than or equal to 75%, the coating is effective, and when the coating proportion is less than 75%, the coating is ineffective.
Optionally, in the step e, when the efficiency is more than or equal to 85%, the method for reducing the magnetism of the pyrrhotite is effective, and when the efficiency is less than 85%, the method for reducing the magnetism of the pyrrhotite is ineffective.
Optionally, in step d, N is greater than or equal to 200 and N is an integer.
Optionally, in step c, the observation is performed in an optical microscope or a scanning electron microscope.
Alternatively, when the method of reducing the magnetic properties of pyrrhotite is ineffective, steps b-d are repeated until the method of reducing the magnetic properties of pyrrhotite is effective.
Optionally, the oxidant comprises at least one of hydrogen peroxide, potassium permanganate and sodium peroxide.
The second aspect of the invention provides the application of the judgment method for reducing the magnetic effectiveness of pyrrhotite in magnetic separation.
Optionally, the magnetic separation comprises magnetic separation of pyrrhotite from magnetite.
Compared with the prior art, the invention has at least the following beneficial effects:
the judgment method for reducing the magnetic effectiveness of pyrrhotite provided by the invention solves the technical problem that no proper representation technical means and specific quantitative standards exist in the prior art for judging the magnetic effectiveness reduction of pyrrhotite. The method is convenient to measure, is easy to identify the coating condition of the pyrrhotite oxide, is more accurate in the measurement result of the magnetic reduction of the pyrrhotite, and is closer to actual production.
The judgment method for reducing the magnetic effectiveness of pyrrhotite, provided by the invention, is applied to magnetic separation, provides more accurate basis for guiding actual production, and is suitable for large-scale popularization and use.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a micrograph of an oxidized coated edge formed by oxidation of pyrrhotite;
FIG. 2 is a micrograph of magnetite which has been oxidized;
FIG. 3 is a schematic diagram of the effect of oxidizing pyrrhotite;
FIG. 4 is a micrograph of the oxidized coated side of pyrrhotite in the example;
FIG. 5 is a flow chart of a desulfurization process of high-sulfur magnetic concentrate provided by a verification example;
FIG. 6 is a micrograph of the oxidized coated side of pyrrhotite after the first oxidation in the experimental example;
fig. 7 is a micrograph of the coating of the oxidized coated edge of pyrrhotite after the second oxidation in the experimental example.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. The components of embodiments of the present invention may be arranged and designed in a wide variety of different configurations.
During the oxidation process of the strong-magnetic monoclinic pyrrhotite, products such as weak-magnetic ferric oxide and the like can be formed on the surface of the strong-magnetic monoclinic pyrrhotite, as shown in figure 1. If the oxidation degree is proper, a remarkable oxidation surface can be formed on the surface of the pyrrhotite, and the magnetism of pyrrhotite particles is reduced. This property can be used when the separation of monoclinic pyrrhotite from other strongly magnetic minerals, such as magnetite, is required for the separation of pyrrhotite for desulfurization in mineral separation: by adding the oxidant, oxidation products are generated on the surfaces of the pyrrhotite particles, and the magnetic strength between the pyrrhotite and the magnetite is greatly different, so that the magnetic separation is realized.
The oxidation degree of pyrrhotite is insufficient, the reduction magnetic degree is insufficient, and the difference between the pyrrhotite and magnetite is insufficient, so that effective separation still cannot be realized; if the oxidation process is too deep, magnetite is oxidized, and as shown in fig. 2, the magnetic property of magnetite is also changed, and magnetic separation cannot be performed because a magnetic difference cannot be formed. Therefore, the judgment on the effectiveness of the magnetic reduction of the estramustine iron ore plays an important role in finally realizing the effective separation of the oxidized pyramustine iron ore.
According to the first aspect of the invention, the judgment method for reducing the magnetic effectiveness of pyrrhotite comprises the following steps:
step a: adding an oxidant into the mineral to react to obtain an oxidized mineral;
step b: sampling the oxidized minerals to prepare epoxy resin polished sections;
step c: when other ferromagnetic minerals in the oxidized minerals have no oxidized coating edges, observing the coating condition of oxidized products of pyrrhotite in the minerals, and judging whether the coating is effective or ineffective;
step d: repeating the step b to enable the observed pyrrhotite particles to reach N particles and recording the area S;
step e: calculating the effective rate through the area S and judging the effectiveness.
The judgment method for reducing the magnetic effectiveness of pyrrhotite provided by the invention solves the technical problem that no proper representation technical means and specific quantitative standards exist in the prior art for judging the magnetic effectiveness reduction of pyrrhotite. The method is convenient to measure, is easy to identify the coating condition of the pyrrhotite oxide, is more accurate in the measurement result of the magnetic reduction of the pyrrhotite, and is closer to actual production.
In addition, the other ferromagnetic minerals in step c are minerals having a ferromagnetic property other than pyrrhotite.
In step c, when the magnetite in the oxidized mineral has no oxidation coating edge, the coating effectiveness of the oxidation product of the pyrrhotite is judged.
In some embodiments of the present invention, the magnetite particles have oxidation coating or erosion edges, indicating that the minerals have been over oxidized, and it is necessary to reduce the amount of oxidant added in step a, or reduce the reaction time, and also to reduce the temperature of the oxidation reaction to prevent over-oxidation of the magnetite.
Optionally, in step e, the effective rate γ =
Wherein S isIs effectiveTo coat the effective total area of the particles, SIs effectiveIs the total area of all particles observed.
Optionally, in the step c, when the coating proportion is greater than or equal to 75%, the coating is effective, and when the coating proportion is less than 75%, the coating is ineffective, and the schematic diagram of the judgment is shown in table 3.
The coating proportion refers to the proportion of the inner circumference of the oxidized coating edge to the outer circumference of the pyrrhotite particle in an optical microscopic image or a scanning electron microscope picture.
Optionally, in the step e, when the efficiency is more than or equal to 85%, the method for reducing the magnetism of the pyrrhotite is effective, and when the efficiency is less than 85%, the method for reducing the magnetism of the pyrrhotite is ineffective.
Optionally, in step d, N is greater than or equal to 200 and N is an integer.
The number of particles observed should be 200 or more, and the more efficient data obtained to determine whether the degree of oxidation is sufficient, the more likely it is to reflect the actual reality as the number of particles observed is larger.
Optionally, in step c, the observation is performed in an optical microscope or a scanning electron microscope.
Alternatively, when the method of reducing the magnetic properties of pyrrhotite is ineffective, steps b-d are repeated until the method of reducing the magnetic properties of pyrrhotite is effective.
In some embodiments of the present invention, when the method for reducing the magnetism of pyrrhotite is judged to be ineffective, it indicates that the coating proportion of the pyrrhotite surface is insufficient, the circumference of the oxidized coating edge is insufficient, and the oxidation needs to be continued, typically but not limited to, prolonging the oxidation reaction time, increasing the reaction temperature or adding an oxidizing agent.
Optionally, the oxidant comprises at least one of hydrogen peroxide, potassium permanganate and sodium peroxide.
The criteria for oxidant selection is that it does not undergo oxidation reactions with other minerals, or that it undergoes oxidation at a slower rate than pyrrhotite.
According to the second aspect of the invention, the application of the judgment method for reducing the magnetic effectiveness of pyrrhotite in magnetic separation is provided.
Optionally, the magnetic separation comprises magnetic separation of pyrrhotite from magnetite.
The judgment method for reducing the magnetic effectiveness of pyrrhotite, provided by the invention, is applied to magnetic separation, provides more accurate basis for guiding actual production, and is suitable for large-scale popularization and use.
The present invention will be described in further detail with reference to examples and comparative examples.
Examples
The embodiment judges the magnetic reduction effectiveness of pyrrhotite in a certain high-sulfur magnetic concentrate, wherein the main minerals in the high-sulfur magnetic concentrate are magnetite and pyrrhotite, and the method specifically comprises the following steps:
(1) the magnetite and pyrrhotite are used as the strongly magnetic minerals in the high-sulfur magnetic concentrate, and the magnetite is an oxide mineral and is relatively stable, so that the problem of oxidation by an oxidant does not exist, and a strong oxidant hydrogen peroxide is selected as the oxidant.
(2) Mixing the high-sulfur magnetic concentrate with an oxidant, wherein the concentration of the oxidant is 30%, stirring at room temperature (the temperature is 25 ℃) for 10 min.
(3) A small amount of sample is prepared into an epoxy resin polished section which can be observed by an optical microscope.
(4) The condition that the magnetite particles are coated by the oxidation products in the sample is observed through an optical microscope, the fact that the surfaces of the magnetite particles are not oxidized at all is found, and the coating effectiveness can be judged.
(5) The coating condition of the pyrrhotite particles in the sample by the oxidation product was observed by an optical microscope, and a microscopic image is shown in fig. 4.
(6) The areas S of each pyrrhotite particle were recorded as valid and invalid, and the information is recorded in Table 1 below.
TABLE 1 Pyrite granule Scale Table
(7) The proportion of the effective fraction is calculated with the area of the particles as a weight. Effective rate Y =
=
=71.98%。
(8) The effective rate is lower than 85 percent, the step (2) is repeated, hydrogen peroxide with the concentration of 30 percent is added, the stirring is carried out for 5min, and the temperature is increased to 60 ℃ during the stirring.
(9) And (4) repeating the step (4) to prepare a sample of the sample after reoxidation, and observing the condition that the magnetite particles are coated by the oxidation products in the sample under an optical microscope, wherein the surface of the magnetite particles is not oxidized, and judging the coating effectiveness.
(10) Repeating the steps (5) to (7), observing the condition that the pyrrhotite particles are coated by the oxidation products in the sample through an optical microscope, marking the condition as effective and ineffective, and recording the area S information of each pyrrhotite particle into the following table 2.
TABLE 2 particle division table for pyrrhotite
(7) The proportion of the effective fraction is calculated with the area of the particles as the weight. Effective rate Y =
=
= 97.27%. The sample at this time is considered to have achieved effective magnetic reduction, and the pyrrhotite can be separated from the magnetite by magnetic separation.
Verification example
The same high-sulfur magnetic concentrate in the example was subjected to oxidation control magnetism of pyrrhotite, and the controlled magnetic concentrate was used to perform a desulfurization process (i.e., separation of magnetite from pyrrhotite), with the process flow diagram shown in fig. 5.
The sulfur content in the raw ore was 2.85% and the iron content was 69.47%.
After the first oxidation, the grade of iron and sulfur of the obtained magnetic concentrate is analyzed, and the result is shown in the following table 3:
TABLE 3 comparison of the iron and sulfur grades of the magnetite concentrate obtained after the first oxidation with the original high-sulfur magnetite concentrate composition
As can be seen from Table 3, the sulfur content in the magnetite concentrate was still high and the desulfurization effect was not achieved. The magnetic concentrate is examined under a microscope to find that the magnetic pyrite in the magnetic concentrate is mostly particles without generating oxidation coating edges, as shown in figure 6, thereby illustrating that the desulfurization effect of the magnetic concentrate is insufficient because the oxidation degree of the magnetic pyrite is still insufficient.
The indices of the obtained magnetic concentrate after the second oxidation are shown in table 4 below.
TABLE 4 magnetic separation desulfurization results after oxidation control of high-sulfur magnetite concentrate
It can be seen from table 4 that the sulfur content in the obtained magnetic concentrate is significantly reduced, i.e. the pyrrhotite is oxidized and does not enter the magnetic concentrate any more, so as to achieve the purpose of desulfurization of the magnetic concentrate. Microscopic examination of the pyrrhotite particles in the tailings revealed that the pyrrhotite particles formed distinct oxide coated edges at this time, as shown in fig. 7.
As can be seen from the embodiment and the verification example, the judgment method provided by the invention provides more accurate judgment for the effectiveness of the magnetic property reduction of the pyrrhotite, so that the effectiveness of the magnetic property reduction of the pyrrhotite is consistent with the production result, the actual production can be better guided, and the method is suitable for large-scale popularization and application.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A judgment method for reducing the magnetic effectiveness of pyrrhotite is characterized by comprising the following steps:
step a: adding an oxidant into the mineral to react to obtain an oxidized mineral;
step b: sampling the oxidized minerals to prepare epoxy resin polished sections;
step c: when other ferromagnetic minerals in the oxidized minerals have no oxidized coating edges, observing the coating condition of oxidized products of pyrrhotite in the minerals, and judging whether the coating is effective or ineffective;
step d: repeating the step b to enable the observed pyrrhotite particles to reach N particles and recording the area S;
step e: calculating the effective rate through the area S and judging the effectiveness.
2. The method for determining the magnetic effectiveness of pyrrhotite according to claim 1, wherein in step e, the effective rate γ = is
Wherein S isIs effectiveTo coat the effective total area of the particles, SIs effectiveIs the total area of all particles observed.
3. The method for judging the magnetic effectiveness of pyrrhotite according to claim 1, wherein in step c, when the coating ratio is greater than or equal to 75%, the coating is effective, and when the coating ratio is less than 75%, the coating is ineffective.
4. The method for judging the magnetic effectiveness of pyrrhotite according to claim 1, wherein in the step e, when the efficiency is more than or equal to 85%, the method for reducing the magnetic property of pyrrhotite is effective, and when the efficiency is less than 85%, the method for reducing the magnetic property of pyrrhotite is ineffective.
5. The method for judging the magnetic effectiveness of pyrrhotite according to claim 1, wherein in step d, N is not less than 200 and is an integer.
6. The method for judging the magnetic effectiveness of pyrrhotite according to any one of claims 1 to 5, characterized in that in step c, the observation is carried out in an optical microscope or a scanning electron microscope.
7. The method for judging the magnetic effectiveness of pyrrhotite according to claim 4, wherein when the method for reducing the magnetic property of pyrrhotite is ineffective, the steps b to d are repeated until the method for reducing the magnetic property of pyrrhotite is effective.
8. The method for judging the magnetic effectiveness of pyrrhotite according to claim 1, wherein the oxidant comprises at least one of hydrogen peroxide, potassium permanganate and sodium peroxide.
9. The use of the method for determining the effectiveness of the magnetism of pyrrhotite according to any one of claims 1 to 8 in magnetic separation.
10. Use according to claim 9, characterized in that the magnetic separation comprises magnetic separation of pyrrhotite from magnetite.
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