CN110508392B - Magnetic-floating separation and comprehensive utilization method of high-sulfur magnetite concentrate - Google Patents

Magnetic-floating separation and comprehensive utilization method of high-sulfur magnetite concentrate Download PDF

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CN110508392B
CN110508392B CN201910839683.2A CN201910839683A CN110508392B CN 110508392 B CN110508392 B CN 110508392B CN 201910839683 A CN201910839683 A CN 201910839683A CN 110508392 B CN110508392 B CN 110508392B
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sulfur
dosage
concentrate
iron
flotation
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CN110508392A (en
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伍红强
刘军
王星
张永
赵艳
赵蒙生
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Sinosteel Maanshan General Institute of Mining Research Co Ltd
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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
    • B03B—SEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
    • B03B1/00—Conditioning for facilitating separation by altering physical properties of the matter to be treated
    • 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
    • B03B—SEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
    • B03B7/00—Combinations of wet processes or apparatus with other processes or apparatus, e.g. for dressing ores or garbage
    • 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
    • B03B—SEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
    • B03B9/00—General arrangement of separating plant, e.g. flow sheets
    • 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
    • B03C1/02—Magnetic separation acting directly on the substance being separated
    • 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
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00—Flotation
    • B03D1/001—Flotation agents
    • B03D1/002—Inorganic compounds
    • 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
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00—Flotation
    • B03D1/001—Flotation agents
    • B03D1/004—Organic compounds
    • B03D1/012—Organic compounds containing sulfur
    • 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
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00—Flotation
    • B03D1/001—Flotation agents
    • B03D1/018—Mixtures of inorganic and organic compounds
    • 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
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00—Flotation
    • B03D1/02—Froth-flotation processes
    • 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
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2201/00—Specified effects produced by the flotation agents
    • B03D2201/02—Collectors
    • 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
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2201/00—Specified effects produced by the flotation agents
    • B03D2201/04—Frothers
    • 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
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2203/00—Specified materials treated by the flotation agents; specified applications
    • B03D2203/02—Ores
    • B03D2203/04—Non-sulfide ores

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  • Inorganic Chemistry (AREA)
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Abstract

The invention discloses a magnetic-floating separation and comprehensive utilization method of high-sulfur magnetite concentrate, which comprises the steps of carrying out ore grinding-low intensity magnetic separation on the high-sulfur magnetite concentrate to obtain low intensity magnetic separation iron concentrate with TFe grade of more than or equal to 64.0 percent and TS of more than or equal to 10.0 percent, carrying out primary floating sulfur roughing, primary floating sulfur concentration and primary floating sulfur scavenging on the low intensity magnetic separation iron concentrate to obtain high iron-sulfur concentrate with TS grade of more than 24.0 percent and TFe grade of more than 60.0 percent, feeding the discharged primary scavenging sulfur tailings into a floating sulfur scavenging open circuit operation to respectively obtain heavy medium products for coal separation with iron grade of more than 63.0 percent and iron concentrate with iron grade of more than 67.0 percent and TS content of less than 1.1 percent, using the obtained high iron-sulfur concentrate with TS grade of more than 24.0 percent and TFe grade of more than 60.0 percent as raw materials for acid preparation in a sulfuric acid plant, and directly using sulfuric acid slag after acid preparation as qualified iron concentrate, thereby realizing sulfur reduction and realizing comprehensive utilization of iron resources and economic benefit, The social benefit and the environmental benefit are obvious.

Description

Magnetic-floating separation and comprehensive utilization method of high-sulfur magnetite concentrate
Technical Field
The invention belongs to the technical field of iron ore dressing, and particularly relates to a method for sorting and comprehensively utilizing sulfur and iron of high-sulfur magnetite concentrate.
Background
With the development of economic and social environments, the quality requirements of China on iron ore concentrates are higher and higher, and especially the requirements on the sulfur content in the iron ore concentrates are stricter and stricter. The sulfur content in the iron ore concentrate has critical influence on iron making and steel making, is harmful to blast furnace production, and causes great pollution to the environment due to sulfur emission. Therefore, the desulfurization of the high-sulfur magnetite is an important task, and plays an important role in promoting the economic development and environmental protection of China, so that the content of the impurity sulfur in the iron ore concentrate entering the furnace is strictly controlled, and the TS is generally required to be less than 0.40%. However, for high-sulfur magnetite concentrate with a TS content of 8-15% (the sulfur occupancy of pyrrhotite is greater than 90%), because of the high desulfurization difficulty, the TS content is generally required to be reduced to below 2% and used as a burden for blast furnace smelting, and for example, the iron concentrate with a TS content of less than 2% in the main flow of the angqing copper mine can be used as qualified iron concentrate.
The sulfur-containing minerals in the magnetite mainly comprise pyrite and pyrrhotite, the pyrite is easy to separate from the magnetite in the magnetic separation process due to no magnetism, but the pyrrhotite is easy to enter magnetic separation concentrate in the magnetic separation process due to strong magnetism, and the pyrrhotite is difficult to separate from the magnetite through single magnetic separation. Therefore, the high-sulfur magnetite is difficult to desulfurize, and the pyrrhotite in the high-sulfur magnetite is mainly difficult to remove. The flotation separation of pyrrhotite and magnetite is one of the key technologies faced by high-sulfur magnetite all the time, and mineral processing workers such as mining enterprises, scientific research institutes and the like have made a great deal of research on similar mines and obtained some stage achievements.
The general process of the ore grinding-magnetic-floating combined process is adopted for the sulfur reduction of the magnetite concentrate, namely, the raw ore is ground to the proper ore grinding granularity, the low-intensity magnetic separation and tailing discarding are firstly carried out, the magnetite concentrate with qualified iron grade is obtained, and then the flotation and the desulfurization are carried out on the magnetite concentrate. The process has good desulfurization effect on the iron ore concentrate when the sulfur in the iron ore concentrate mainly exists in the form of pyrite; however, sulfur in iron ore concentrate mainly exists in the form of pyrrhotite, and when the sulfur content is as high as 8-15%, the desulfurization effect is not ideal, and the total sulfur content in the iron ore concentrate is difficult to be reduced to below 2%. In addition, the yield of the foam products removed by flotation is high, but the sulfur grade is not high, the iron grade is not high, and the foam products are reduced to chicken ribs, so that the waste of resources is caused.
The present situation of flotation desulfurization process and mechanism research of high-sulfur magnetite, published in "mineral protection and utilization" 5 th 2013 of Chinese journal, is considered as follows: the desulfurization of high-sulfur magnetite is a great technical problem faced by the steel industry for a long time, the separation of magnetite and pyrrhotite by using a magnetic separation method is almost impossible, and the flotation is one of the most effective ways for reducing sulfur in iron ore concentrate. However, in the several flotation desulfurization methods described in the article, the sulfur content in the magnetite concentrate with the sulfur content of about 1.0% can be reduced to about 0.45% by desulfurization flotation, and the sulfur reduction effect in the high-sulfur iron concentrate is not very obvious, for example, the sulfur content in the high-sulfur iron concentrate can be reduced to below 5% from about 20% of the original sulfur content. In addition, in the flotation and desulfurization of the high-sulfur magnetite concentrate in the prior art, the final product is only iron concentrate, and sulfur white in the high-sulfur magnetite concentrate is lost in tailings, so that not only is the resource waste caused, but also the environment is polluted. Moreover, the iron grade of the iron concentrate product obtained by the flotation and desulfurization of the high-sulfur magnetite concentrate in the prior art is low, generally less than 64.5 percent, and the iron concentrate product is difficult to adapt to the market demand.
Disclosure of Invention
The invention aims to provide a magnetic-floating separation and comprehensive utilization method of high-sulfur magnetite concentrate, which has high iron concentrate grade and good desulfurization effect and can obtain three products, aiming at the technical problems of high iron and sulfur separation difficulty, large tailing production amount and large resource waste in the prior art.
In order to realize the purpose, the magnetic-floating separation and comprehensive utilization method of the high-sulfur magnetite concentrate adopts the technical scheme that:
the invention relates to a magnetic-floating separation and comprehensive utilization method of high-sulfur magnetite concentrate, which adopts the following processes:
(1) high-sulfur magnetite concentrate ore grinding-low intensity magnetic separation
Sorting high-sulfur magnetite concentrate with the TFe grade of 55-60%, the TS content of 8-10% and the sulfur occupation rate of pyrrhotite of more than 90% of the total sulfur, carrying out ore grinding-low intensity magnetic separation on the high-sulfur magnetite concentrate to obtain low intensity magnetic separation iron concentrate with the TFe grade of more than or equal to 64.0% and the TS of more than or equal to 10.0%, and discharging low intensity magnetic separation tailings;
the weak magnetic separation is preferably performed by adopting one-time weak magnetic rough separation and one-time weak magnetic fine separation; a tower type grinding machine is adopted for grinding ore, and the grinding granularity is controlled to be between 78 and 83 percent of minus 0.043 mm; the low-intensity magnetic separation adopts a countercurrent permanent magnet drum magnetic separator, the magnetic induction intensity of primary roughing is controlled within the range of 135-150 kA/m, and the magnetic induction intensity of primary fine separation is controlled within the range of 120-135 kA/m.
(2) Low-intensity magnetic separation iron ore concentrate rough-fine-sweeping closed-circuit sulfur floating operation
Carrying out primary sulfur flotation roughing, primary sulfur flotation fine selection and primary sulfur flotation scavenging on the low-intensity magnetic iron ore concentrate obtained in the step (1) to obtain high-iron sulfur ore concentrate with the TS grade of more than 24.0% and the TFe grade of more than 60.0%, and discharging primary scavenging sulfur flotation tailings; and combining the tailings subjected to the primary sulfur flotation concentration and the concentrate subjected to the primary sulfur flotation scavenging and returning to the primary sulfur flotation roughing.
In the sulfur floating operation, oxalic acid is used as a complexing agent, copper sulfate is used as an activating agent, butyl xanthate is used as a collecting agent, and 2# oil is used as a foaming agent, and the dosage of the agent is as follows according to the dry ore amount of flotation feeding: the using amount of the first sulfur-floating roughing oxalic acid is 1200-2000 g/t, the using amount of copper sulfate is 400-1200 g/t, the using amount of butyl xanthate is 200-300 g/t, and the using amount of foaming agent No. 2 oil is 40-50 g/t; the dosage of the first flotation sulfur scavenging oxalic acid is 400-1200 g/t, the dosage of the copper sulfate is 300-500 g/t, the dosage of the butyl xanthate is 200-300 g/t, and the dosage of the foaming agent No. 2 oil is 20-30 g/t; the dosage of the xanthate for one-time sulfur floating selection is 100-150 g/t, and the dosage of the foaming agent No. 2 oil is 5-15 g/t.
According to the dry ore amount of flotation feeding, the preferable medicament dosage is as follows: the dosage of the first sulfur-floating roughing oxalic acid is 1600-1800 g/t, the dosage of the copper sulfate is 600-800 g/t, the dosage of the butyl xanthate is 200-300 g/t, and the dosage of the foaming agent No. 2 oil is 40-50 g/t; the dosage of the first flotation sulfur scavenging oxalic acid is 400-1200 g/t, the dosage of the copper sulfate is 300-500 g/t, the dosage of the butyl xanthate is 200-300 g/t, and the dosage of the foaming agent No. 2 oil is 20-30 g/t; the dosage of the xanthate for one-time sulfur floating selection is 100-150 g/t, and the dosage of the foaming agent No. 2 oil is 5-15 g/t.
(3) Open-circuit flotation of once scavenging sulfur tailings
And (3) feeding the primary scavenging sulfur flotation tailings discharged in the step (2) into a sulfur flotation scavenging open circuit operation to respectively obtain a heavy medium product for coal dressing with iron grade of more than 63.0% and iron ore concentrate with iron grade of more than 67.0% and TS content of less than 1.1%.
In open-circuit flotation operation, oxalic acid is used as a complexing agent, copper sulfate is used as an activating agent, a mixed medicine of butyl xanthate and butyl ammonium blackant is used as a collecting agent, and No. 2 oil is used as a foaming agent; according to the dry ore amount of flotation feeding, the dosage of the medicament is as follows: the dosage of oxalic acid is 400-1000 g/t, the dosage of copper sulfate is 300-500 g/t, the dosage of butyl xanthate and butyl ammonium nigride is 100-200 g/t, and the dosage of foaming agent No. 2 oil is 20-30 g/t.
According to the dry ore amount of flotation feeding, the optimized medicament dosage is as follows: the dosage of oxalic acid is 700-900 g/t, the dosage of copper sulfate is 400-450 g/t, the dosage of butyl xanthate and butyl ammonium nigride is 100-200 g/t, and the dosage of foaming agent No. 2 oil is 20-30 g/t.
In the mixed medicine of the butyl xanthate and the butyl ammonium nigride, the ratio of the butyl xanthate to the butyl ammonium nigride is 1: (0.8-1.2), wherein the ratio of 1: (0.9-1.1), and the synergistic effect of the butyl xanthate and the butyl ammonium nigride is the most ideal under the condition of the mixture ratio.
(4) Preparation of sulfuric acid from high-iron sulfur concentrate
And (3) taking the high-iron sulfur concentrate with the TS grade of more than 24.0% and the TFe grade of more than 60.0% obtained in the step (2) as a raw material for preparing acid in a sulfuric acid plant, and directly taking sulfuric acid residue after acid preparation as qualified iron concentrate to realize the sulfur-iron dual-resource utilization of the high-iron sulfur concentrate.
The specific values of the parameters such as the ore grinding granularity, the flotation times, the medicament dosage, the magnetic induction intensity and the like can be determined through laboratory test results according to the properties of ores.
Compared with the prior art, the magnetic-floating separation and comprehensive utilization method of the high-sulfur magnetite concentrate has the following advantages:
(1) the flotation process adopts a semi-closed-semi-open process, realizes the gradient recycling of the high-sulfur magnetite concentrate, and obtains three products of iron concentrate, high-iron-sulfur concentrate and dense medium products. Laboratory research results show that the comprehensive recovery rate of iron and sulfur in the three products is up to more than 96.0%, and the benefits and the resources are maximized;
(2) oxalic acid is used as a complexing agent, so that the influence of metal ions such as calcium ions in ore pulp on sulfur flotation is eliminated, and the consumption of sulfuric acid is reduced;
(3) the sulfuric acid residue after the acid preparation from the high-iron sulfur concentrate can be directly used as iron concentrate, so that the sulfur-iron dual-resource utilization is realized;
(4) the process flow is simple, the mineral separation cost is low, all the used reagents are easily purchased in the market, the obtained iron ore concentrate, the high-iron sulfur ore concentrate and the dense medium all have market sales, and unexpected technical effects and economic effects are obtained.
Drawings
Fig. 1 is a principle process flow chart of the magnetic-floating separation and comprehensive utilization method of the high-sulfur magnetite concentrate.
Detailed Description
For describing the present invention, the magnetic-floating separation and comprehensive utilization method of high-sulfur magnetite concentrate according to the present invention will be described in further detail with reference to the accompanying drawings and examples.
The high-sulfur magnetite concentrate used in this example was Anhui-Chimu ore, and the results of the chemical multi-element analysis of the high-sulfur magnetite concentrate are shown in Table 1, the results of the iron phase analysis are shown in Table 2, and the results of the sulfur phase analysis are shown in Table 3.
TABLE 1 chemical multielement analysis of high-sulfur magnetite concentrates
Assay project TFe SiO2 Al2O3 CaO MgO
Content (%) 55.69 9.61 0.985 4.05 1.96
TS P K2O Na2O MnO TiO2
8.86 0.018 0.068 0.177 0.108 0.091
V2O5 CuO ZnO Cr2O3 NiO /
0.09 0.066 0.007 0.021 0.049 /
TABLE 2 iron phase analysis results of high-sulfur magnetite concentrate
Name of iron phase Iron content Distribution ratio
Magnetite 40.77 72.49
Hematite (iron ore) 1.27 2.26
Pyrrhotite 13.06 23.22
Siderite ore 0.42 0.75
Pyrite 0.12 0.21
Iron silicate 0.60 1.07
All iron 56.24 100.00
Table 3 high-sulfur magnetite concentrate sulfur phase analysis result (%)
Sulfide phase name Sulfur content Distribution ratio
Elemental sulfur 0.02 0.21
Sulfur in sulfate 0.24 2.57
Sulfur of magnetic sulfides 8.71 93.26
Sulfur of other sulfides 0.37 3.96
All sulfur 9.34 100.00
The analysis of the properties of the high-sulfur magnetite concentrate shows that the content of main impurities TS is as high as 8.86 percent, 93.26 percent of the main impurities exist in the form of pyrrhotite, and the pyrrhotite belongs to a strong magnetic mineral and enters the weak magnetic concentrate together with magnetite in the process of weak magnetic separation, so that the pyrrhotite cannot be removed by adopting single weak magnetic separation and must be removed by adopting flotation.
As shown in the principle process flow chart of the magnetic-floating separation and comprehensive utilization method of the high-sulfur magnetite concentrate shown in fig. 1, the magnetic-floating separation and comprehensive utilization method of the high-sulfur magnetite concentrate adopts the following processes and steps:
(1) grinding high-sulfur magnetite concentrate and carrying out low-intensity magnetic separation;
the ore grinding equipment adopts a fine grain tower mill developed by the Zhonggang Anhui Tianyuan science and technology Limited company, the ore grinding granularity is preferably controlled to be-0.043 mm 75% -85%, and the finally selected ore grinding granularity is-0.043 mm 80%. The grinding granularity of the tower mill is more uniform, and the phenomena of over-grinding and argillization are avoided.
The low-intensity magnetic separation equipment adopts a countercurrent permanent magnet drum magnetic separator, and the low-intensity magnetic separation process is preferably primary roughing and primary fine separation; the magnetic induction intensity of the roughing is preferably controlled within the range of 143-159 kA/m, and the magnetic induction intensity of the selecting is preferably controlled within the range of 126-143 kA/m. The magnetic induction optimized in the laboratory is as follows: roughing at 143kA/m and concentrating at 126 kA/m. The separation precision of the countercurrent permanent magnet drum magnetic separator is higher.
By the ore grinding-low-intensity magnetic separation, low-intensity magnetic separation iron ore concentrate with the TFe grade of 64.86% and the TS content of 10.65% is obtained, and low-intensity magnetic separation tailings with the yield of 15.36%, the TFe grade of 12.63% and the TS content of 2.06% are discharged.
(2) Performing rough-fine-sweeping closed flotation on the iron concentrate obtained in the step (1) by low-intensity magnetic separation to obtain high-iron sulfur concentrate;
and carrying out coarse-fine-sweeping closed-circuit separation on the low-intensity magnetic separation iron concentrate with the TFe grade of 64.86% and the TS content of 10.65% to obtain high-iron sulfur concentrate with the TS grade of 25.6% and the TFe grade of 61.3%.
The flotation in the step (2) adopts a coarse-fine-sweeping closed-circuit flotation; oxalic acid is used as a complexing agent, copper sulfate is used as an activating agent, butyl xanthate is used as a collecting agent, and No. 2 oil is used as a foaming agent.
After a plurality of condition tests, according to the dry ore amount of the flotation feeding ore, the dosage of the flotation reagent in the step (2) is finally determined as follows: 1710g/t of first-time sulfur-floating roughing oxalic acid, 650g/t of copper sulfate, 250g/t of butyl xanthate and 48g/t of foaming agent No. 2 oil; the dosage of oxalic acid for first flotation sulfur scavenging is 750g/t, the dosage of copper sulfate is 360g/t, the dosage of butyl xanthate is 250g/t, and the dosage of foaming agent No. 2 oil is 24 g/t; the dosage of the first sulfur floating and selecting butyl xanthate is 125g/t, and the dosage of the foaming agent No. 2 oil is 12g/t
(3) And (3) performing open-circuit flotation on the tank bottom product obtained in the step (2) to obtain a dense medium product for coal dressing and qualified iron ore concentrate.
And (3) performing open-circuit flotation on the tank bottom product in the step (2) to obtain a heavy medium product for coal dressing with TS 15.86% and TFe grade > 63.58%, and further obtain iron ore concentrate with TFe grade 67.5% and TS content < 1.06%. The dense medium product for coal dressing is mainly pyrrhotite, has high density, meets the requirement of the dense medium product for coal dressing on the density, has high magnetic coefficient and can be recycled by magnetic separation.
And (3) adopting one-time open-circuit flotation for flotation, adopting oxalic acid as a complexing agent, copper sulfate as an activating agent, butyl xanthate and butyl ammonium melanophore (1:1) as a collecting agent and 2# oil as a foaming agent.
The dosage of the flotation reagent in the step (3) is as follows: according to the dry ore amount of flotation feeding, the dosage of the medicament is as follows: the dosage of oxalic acid is 750g/t, the dosage of copper sulfate is 430g/t, the dosage of the butyl xanthate and the butyl ammonium nigride is 125g/t, and the dosage of the foaming agent No. 2 oil is 24 g/t.
(4) Preparation of sulfuric acid from high-iron sulfur concentrate
And (3) taking the high-iron sulfur concentrate with the TS grade of 25.6% and the TFe grade of 61.3% obtained in the step (2) as a raw material for preparing acid in a sulfuric acid plant, wherein the TFe grade of the sulfuric acid residue after preparing the acid is up to over 67.6%, and the high-iron sulfur concentrate can be directly sold as qualified iron concentrate, so that the sulfur-iron dual-resource utilization of the high-iron sulfur concentrate is realized.
The invention also adopts citric acid as complexing agent and sulfuric acid as activating agent to carry out comparison test, and the ore grinding equipment in the step (1) adopts a phi 240X 90 conical ball mill in a laboratory. Through experimental research, under the condition of optimized experimental parameters, high-iron sulfur concentrate with 24.76% of sulfur grade and 60.65% of iron grade and heavy medium product with 63.29% of iron grade can be obtained, iron concentrate with 67.08% of iron grade is also obtained, the yield of tailings is 16.61%, the TFe grade in the tailings is 13.08%, and the TS grade is 1.83%, which are lower than the experimental indexes obtained by the method. Research also finds that the dosage of the medicament is large by adopting citric acid as a complexing agent and sulfuric acid as an activating agent.
The invention is already applied to a certain high-sulfur-content magnetic ore dressing plant in Anhui, the technical index obtained by industrial tests is very close to the laboratory result, the problems of difficult separation of iron and sulfur, great resource waste and environmental pollution caused by sulfur discharged to tailings existing for many years are solved, good economic benefit and environmental benefit are obtained, and unexpected technical effect is obtained.

Claims (4)

1. A magnetic-floating separation and comprehensive utilization method of high-sulfur magnetite concentrate is characterized by adopting the following processes:
(1) high-sulfur magnetite concentrate ore grinding-low intensity magnetic separation
Sorting high-sulfur magnetite concentrate with the TFe grade of 55-60%, the TS content of 8-10% and the sulfur occupation rate of pyrrhotite of more than 90% of the total sulfur, carrying out ore grinding-low intensity magnetic separation on the high-sulfur magnetite concentrate to obtain low intensity magnetic separation iron concentrate with the TFe grade of more than or equal to 64.0% and the TS of more than or equal to 10.0%, and discharging low intensity magnetic separation tailings;
the low-intensity magnetic separation adopts primary low-intensity magnetic rough separation and primary low-intensity magnetic fine separation;
(2) low-intensity magnetic separation iron ore concentrate rough-fine-sweeping closed-circuit sulfur floating operation
Carrying out primary sulfur flotation roughing, primary sulfur flotation fine selection and primary sulfur flotation scavenging on the low-intensity magnetic iron ore concentrate obtained in the step (1) to obtain high-iron sulfur ore concentrate with the TS grade of more than 24.0% and the TFe grade of more than 60.0%, and discharging primary scavenging sulfur flotation tailings; combining the tailings subjected to the primary sulfur flotation concentration and the concentrate subjected to the primary sulfur flotation scavenging, and returning to the primary sulfur flotation roughing;
in the sulfur floating operation, oxalic acid is used as a complexing agent, copper sulfate is used as an activating agent, butyl xanthate is used as a collecting agent, and 2# oil is used as a foaming agent, and the dosage of the agent is as follows according to the dry ore amount of flotation feeding: the using amount of the first sulfur-floating roughing oxalic acid is 1200-2000 g/t, the using amount of copper sulfate is 400-1200 g/t, the using amount of butyl xanthate is 200-300 g/t, and the using amount of foaming agent No. 2 oil is 40-50 g/t; the dosage of the first flotation sulfur scavenging oxalic acid is 400-1200 g/t, the dosage of the copper sulfate is 300-500 g/t, the dosage of the butyl xanthate is 200-300 g/t, and the dosage of the foaming agent No. 2 oil is 20-30 g/t; the dosage of the first sulfur floating selection butyl xanthate is 100-150 g/t, and the dosage of the foaming agent No. 2 oil is 5-15 g/t;
(3) open-circuit flotation of once scavenging sulfur tailings
Feeding the primary scavenging sulfur flotation tailings discharged in the step (2) into a sulfur flotation scavenging open circuit operation to respectively obtain a heavy medium product for coal dressing with iron grade of 63.0% and iron ore concentrate with iron grade of 67.0% and TS content of 1.1%;
in open-circuit flotation operation, oxalic acid is used as a complexing agent, copper sulfate is used as an activating agent, a mixed medicine of butyl xanthate and butyl ammonium blackant is used as a collecting agent, and No. 2 oil is used as a foaming agent; according to the dry ore amount of flotation feeding, the dosage of the medicament is as follows: the dosage of oxalic acid is 400-1000 g/t, the dosage of copper sulfate is 300-500 g/t, the dosage of butyl xanthate and butyl ammonium nigride is 100-200 g/t, and the dosage of foaming agent No. 2 oil is 20-30 g/t;
(4) preparation of sulfuric acid from high-iron sulfur concentrate
And (3) taking the high-iron sulfur concentrate with the TS grade of more than 24.0% and the TFe grade of more than 60.0% obtained in the step (2) as a raw material for preparing acid in a sulfuric acid plant, and directly taking sulfuric acid residue after acid preparation as qualified iron concentrate to realize the sulfur-iron dual-resource utilization of the high-iron sulfur concentrate.
2. The magnetic-floating separation and comprehensive utilization method of the high-sulfur magnetite concentrate as recited in claim 1, characterized in that:
in the step (2), according to the dry ore amount of flotation feeding, the dosage of the medicament is as follows: the dosage of the first sulfur-floating roughing oxalic acid is 1600-1800 g/t, the dosage of the copper sulfate is 600-800 g/t, the dosage of the butyl xanthate is 200-300 g/t, and the dosage of the foaming agent No. 2 oil is 40-50 g/t; the dosage of the first flotation sulfur scavenging oxalic acid is 400-1200 g/t, the dosage of the copper sulfate is 300-500 g/t, the dosage of the butyl xanthate is 200-300 g/t, and the dosage of the foaming agent No. 2 oil is 20-30 g/t; the dosage of the first sulfur floating selection butyl xanthate is 100-150 g/t, and the dosage of the foaming agent No. 2 oil is 5-15 g/t;
in the step (3), according to the dry ore amount of the flotation feeding, the dosage of the medicament is as follows: the dosage of oxalic acid is 700-900 g/t, the dosage of copper sulfate is 400-450 g/t, the dosage of butyl xanthate and butyl ammonium nigride is 100-200 g/t, and the dosage of foaming agent No. 2 oil is 20-30 g/t.
3. The magnetic-floating separation and comprehensive utilization method of high-sulfur magnetite concentrate as recited in claim 1 or 2, characterized in that: in the mixed medicine of the butyl xanthate and the butyl ammonium nigride, the ratio of the butyl xanthate to the butyl ammonium nigride is 1: (0.8 to 1.2).
4. The magnetic-floating separation and comprehensive utilization method of the high-sulfur magnetite concentrate, according to claim 3, is characterized in that: in the step (1), a tower type grinding machine is adopted for grinding ores, and the granularity of the ground ores is controlled to be-0.043 mm 78% -83%; the low-intensity magnetic separation adopts a countercurrent permanent magnet drum magnetic separator, the magnetic induction intensity of primary roughing is controlled within the range of 135-150 kA/m, and the magnetic induction intensity of primary fine separation is controlled within the range of 120-135 kA/m.
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