CN112871458A - Combined reagent for desulfurizing fine iron powder under alkaline condition and method for desulfurizing pyrrhotite by using combined reagent - Google Patents

Combined reagent for desulfurizing fine iron powder under alkaline condition and method for desulfurizing pyrrhotite by using combined reagent Download PDF

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CN112871458A
CN112871458A CN202011579211.7A CN202011579211A CN112871458A CN 112871458 A CN112871458 A CN 112871458A CN 202011579211 A CN202011579211 A CN 202011579211A CN 112871458 A CN112871458 A CN 112871458A
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combined
activator
activating agent
desulfurizing
stirring
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CN112871458B (en
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韩西鹏
陈永伟
李金梁
张伟
邢汉明
王涛
王乃强
刘呈增
王超
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Shandong Jinling Mining 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
    • 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
    • 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
    • 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
    • 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
    • B03D2203/00—Specified materials treated by the flotation agents; specified applications
    • B03D2203/02—Ores

Abstract

The invention relates to a reagent for mineral flotation, in particular to a combined reagent for fine iron powder desulfurization under an alkaline condition and a method for desulfurizing pyrrhotite by adopting the combined reagent. The combined reagent for desulfurizing the fine iron powder under the alkaline condition comprises a combined activator and a combined collector, wherein the combined activator comprises an activator 1, an activator 2 and an activating agentAgent 3, activator 1 is FeSO4·7H2O, activator 2 is NH4Cl, activating agent 3 is CuSO4·5H2O; the combined collector comprises butyl xanthate and butyl ammonium blackant; the mass ratio of the activating agent 1 to the activating agent 2 to the activating agent 3 is 3:1: 0.8-1.2; the mass ratio of the butyl xanthate to the ammonium buterate is 3: 1. The combined reagent can achieve the purpose of reducing sulfur in fine iron powder by flotation under an alkaline condition, and the invention also provides a method for desulfurizing pyrrhotite by adopting the combined reagent, so that the defects of flotation under an acidic condition are avoided, and the desulfurization effect is good.

Description

Combined reagent for desulfurizing fine iron powder under alkaline condition and method for desulfurizing pyrrhotite by using combined reagent
Technical Field
The invention relates to a reagent for mineral flotation, in particular to a combined reagent for fine iron powder desulfurization under an alkaline condition and a method for desulfurizing pyrrhotite by adopting the combined reagent.
Background
Fine iron powder with high sulfur content can have adverse effects on subsequent smelting and steel products. The higher sulfur grade causes hot shortness of the steel, reduces ductility and toughness of the steel, and causes cracks during forging and rolling. Sulfur is also detrimental to the welding performance and reduces the corrosion resistance of the steel. Meanwhile, SO is easily generated in the smelting process2Causing environmental pollution. The reduction of the sulfur content of the iron concentrate is an important scientific research task in the field of mineral separation, and has positive effects on national economy and environmental protection career of China.
The sulfur-containing magnetite deposit has complex ore components, generally contains magnetite as a main component and associated pyrite, chalcopyrite, pyrrhotite and the like. The traditional desulfurization process of the ore is generally a combined floating magnetic process. And simultaneously carrying out flotation and desulfurization, simultaneously selecting the rest valuable metals, and separating the valuable metals from sulfur by utilizing a high-alkali ore pulp environment. Due to the addition of lime, the ore pulp is alkaline and the calcium ion is too high, a large amount of hydroxyl and calcium ions are adsorbed on the surfaces of the pyrite and pyrrhotite, the floatability is inhibited, and particularly the pyrrhotite is difficult to activate. When the pyrrhotite is more, the natural floatability of the pyrrhotite is poor due to the fact that the surface of the pyrrhotite is easy to oxidize and argillization and the chemical composition and the lattice structure of the pyrrhotite are determined, the pyrrhotite and the monoclinic pyrrhotite cannot float upwards by a traditional flotation method, and meanwhile, the sulfur content of fine iron powder is increased.
Currently, an effective method for desulfurizing magnetite containing pyrrhotite is to activate pyrrhotite and perform flotation desulfurization under an acidic condition. For example, the Chinese invention patent CN 108097452A discloses a mineral processing technology for producing high-quality iron ore concentrate from iron ore, which takes aluminum sulfate or a mixture of aluminum sulfate and ammonium fluorosilicate with a mass ratio of 3-1:1-2 or a mixture of aluminum sulfate and sodium phosphate with a mass ratio of 1-2:3-2 as a pH regulator and an activator of pyrrhotite, and carries out flotation desulfurization under the condition of adjusting the pH to 4.5-5.5, but the acidic condition seriously corrodes flotation equipment, pipelines and the like, and has large consumption and higher industrial application cost.
Disclosure of Invention
The invention aims to provide a combined reagent for desulfurizing iron concentrate under an alkaline condition, which achieves the aim of reducing sulfur in the iron concentrate through flotation and has good desulfurization effect; the invention also provides a method for desulfurizing pyrrhotite by using the same.
The combined reagent for desulfurizing the fine iron powder under the alkaline condition comprises a combined activator and a combined collector, wherein the combined activator comprises an activator 1, an activator 2 and an activator 3, and the activator 1 is FeSO4·7H2O, activator 2 is NH4Cl, activating agent 3 is CuSO4·5H2O; the combined collector comprises butyl xanthate and butyl ammonium blackant;
the mass ratio of the activating agent 1 to the activating agent 2 to the activating agent 3 is 3:1: 0.8-1.2;
the mass ratio of the butyl xanthate to the ammonium buterate is 3: 1.
The method for desulfurizing pyrrhotite by adopting the combined reagent comprises the following steps:
(1) size mixing:
carrying out primary grinding on magnetite containing pyrrhotite, wherein the grinding concentration is 65-70%, and the grinding fineness of-0.074 mm is 50-55%; adjusting the concentration of the obtained ore pulp to 19-23%, adding lime with the dosage of 2-10kg/t, adjusting the pH value of the ore pulp to 8-14, and stirring for 4 min;
(2) roughing:
in the stirring process, adding the activating agent 1 with the dosage of 300-700g/t, and stirring for 1 min; adding the solution prepared by the activating agents 2 and 3 with the dosage of 300-500g/t, and stirring for 3 min; adding a combined collecting agent with the dosage of 100-140g/t, adding a foaming agent with the dosage of 6-10g/t, stirring for 2min, and performing rough concentration for 12-14min to obtain rough concentration foam concentrate and rough concentration tailings;
(3) sweeping:
scavenging the roughed tailings, adding an activating agent 3 with the dosage of 60-80g/t, and stirring for 3 min; adding a combined collecting agent with the use amount of 50-70g/t, adding a foaming agent with the use amount of 6-10g/t, stirring for 2min, and scavenging for 10-12min to obtain scavenging foam and scavenging tailings;
(4) magnetic separation:
and carrying out magnetic separation on the scavenged tailings with the magnetic field intensity of 1400-1600Oe to obtain iron ore concentrate and tailings.
Wherein:
and the solution prepared by adding the activating agent 2 and the activating agent 3 is prepared in advance according to the mass ratio of 1:0.8-1.2, and the reaction time is 15-60min, so that the copper ammonia complex ions are fully reacted to form the copper ammonia complex ions.
The foaming agent is 2# oil.
Compared with the prior art, the invention has the following beneficial effects:
(1) the flotation environment used in the invention is an alkaline environment. The corrosion of acidic conditions to equipment and pipelines and the potential safety risk of concentrated acid in the preparation and dilution process are effectively avoided, and toxic and harmful gases such as hydrogen sulfide and the like are easily generated in the adding process.
(2) In the present invention, NH4Cl and CuSO4·5H2O is prepared into solution in advance, so that the full reaction of the O and the O is ensured, copper ammonia complex ions are formed, and firstly, the adsorption on the surface of the mineral is realized, so that the active sites on the surface of the mineral are increased, and the adsorption of the collecting agent on the surface of the mineral is improvedThe additive amount achieves the effect of strengthening flotation; and secondly, the copper ammonia complex ions have a complexing effect on hydrophilic compound films such as calcium, iron and the like on the surface of pyrrhotite, so that the hydrophilic film on the surface of the mineral can be selectively dissolved to expose the fresh surface of the mineral, active sites are provided for xanthate, or lattice defects are generated on the surface of the mineral, so that the porosity is increased, and the adsorption effect is enhanced.
(3) According to the invention, the butyl xanthate and the ammonium nitrate are combined to be used as the collecting agent, the butyl xanthate and the ammonium nitrate generate co-adsorption in the flotation process, and compared with a single type of collecting agent, the collecting effect is improved.
(4) The ammonium nitrate black powder added in the invention also has a foaming effect, can enhance the foam strength, reduces the probability of falling of ore particles from the foam in the flotation process, and improves the desulfurization effect.
(5) By adopting the combined medicament and the method for desulfurizing pyrrhotite, the sulfur content can be reduced to be below 0.18 percent.
Drawings
FIG. 1 is a flow chart of the fine iron powder desulfurization method under alkaline conditions of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer and clearer, the present invention will be further described in detail with reference to specific examples.
The activator 1 described in the examples is FeSO4·7H2O, activator 2 is NH4Cl, activating agent 3 is CuSO4·5H2O; the combined collecting agent comprises butyl xanthate and butylammonium melanophore, and the mass ratio of the butyl xanthate to the butylammonium melanophore is 3: 1.
The foaming agent is 2# oil.
The raw materials used in the examples were all commercially available materials except for those specifically mentioned.
Example 1
The experiment is carried out by adopting the pyrrhotite-containing iron ore of a certain mine, and most of the S element in the mine ore is distributed in the pyrrhotite, accounting for 60 percent. The method comprises the following specific steps:
(1) and (6) size mixing. The iron ore containing pyrrhotite is subjected to primary grinding, the grinding concentration is 69%, and the grinding fineness (-0.074mm) is 54%. Adjusting the concentration of the obtained ore pulp to 22%, adding lime with the dosage of 3kg/t, adjusting the pH value of the ore pulp to 9, and stirring for 4 min;
(2) and (6) roughing. Adding the activating agent 1 with the dosage of 450g/t during stirring, and stirring for 1 min; adding a solution (reaction time is 30min) prepared by the activators 2 and 3 according to the mass ratio of 1:1.2, wherein the dosage is 330g/t, and stirring for 3 min; adding a combined collecting agent with the use amount of 120g/t, adding a foaming agent with the use amount of 8g/t, stirring for 2min, and performing rough concentration for 12.5min to obtain rough concentration foam concentrate and rough concentration tailings.
(3) And (6) scavenging. And (4) carrying out scavenging on the roughed tailings obtained in the step. Adding an activating agent 3 with the dosage of 70g/t, and stirring for 3 min; adding the combined collecting agent with the use amount of 60g/t, adding the foaming agent with the use amount of 8g/t, stirring for 2min, and scavenging for 11min to obtain scavenging foam and scavenging tailings.
(4) And (6) magnetic separation. And (4) carrying out magnetic separation on the scavenged tailings obtained in the previous step, wherein the magnetic field intensity is 1500Oe, and obtaining iron ore concentrate and tailings.
For comparison, according to the sorting process flow shown in the flow chart of fig. 1, the existing chemical system of the mine is used as a comparative example 1, no activating agent is used in the flotation stage, the used collecting agent is butyl xanthate, and other test conditions are the same as those in example 1.
As another comparison, according to the selection process shown in the flow chart of FIG. 1, the activator 2 and the activator 3 mentioned in the step (2) of the above example 1 were added separately in the order mentioned, and were not prepared into a solution, and the amount of the activator 2 was 150g/t and the amount of the activator 3 was 180g/t, and the other conditions were the same as those of the example 1, and were set as the comparative example 2.
The results of the three sets of conditions are shown in Table 1.
TABLE 1
Figure BDA0002863969430000041
As can be seen from the above table: (1) the invention has obvious iron concentrate desulfurization effect in alkaline environment. (2) The activating agent 2 and the activating agent 3 are added after being prepared into a solution, the activating effect on pyrrhotite is better than that of a single adding mode, and the effect of copper ammonia complex ions in the activating process is verified.
Example 2
Selecting high-sulfur raw ore containing pyrrhotite in a certain mine for testing, wherein S element of the raw ore distributed in the pyrrhotite accounts for 45 percent, and the specific implementation steps are as follows:
(1) and (6) size mixing. Carrying out primary grinding on the magnetite containing the pyrrhotite, wherein the grinding concentration is 65%, and the grinding fineness (-0.074mm) is 52%. Adjusting the concentration of the obtained ore pulp to 22%, adding lime with the dosage of 7kg/t, adjusting the pH value of the ore pulp to 11, and stirring for 4 min;
(2) and (6) roughing. Adding the activating agent 1 with the dosage of 660g/t during stirring, and stirring for 1 min; adding a solution (reaction time is 30min) prepared by activating agents 2 and 3 according to the mass ratio of 1:1.1, wherein the use amount is 470g/t, and stirring for 3 min; adding a combined collecting agent with the dosage of 130g/t, adding a foaming agent with the dosage of 9g/t, stirring for 2min, and performing rough concentration for 13min to obtain rough concentration foam concentrate and rough concentration tailings.
(3) And (6) scavenging. And (4) carrying out scavenging on the roughed tailings obtained in the step. Adding an activating agent 3 with the dosage of 80g/t, and stirring for 3 min; adding the combined collecting agent with the use amount of 70g/t, adding the foaming agent with the use amount of 8g/t, stirring for 2min, and scavenging for 11.5min to obtain scavenging foam and scavenging tailings.
(4) And (6) magnetic separation. And (4) carrying out magnetic separation on the scavenged tailings obtained in the previous step, wherein the magnetic field intensity is 1500Oe, and obtaining iron ore concentrate and tailings.
For comparison, according to the sorting process flow shown in the flow chart of FIG. 1, butyl xanthate is used as the collecting agent in the roughing in step (2) and the scavenging in step (3) of the flotation stage, and the amounts of the butyl xanthate are 130g/t and 70g/t respectively, and the rest of the test conditions are the same as those in example 2 and serve as comparative example 3.
As another comparison, according to the sorting process shown in the flow chart of FIG. 1, the ammonium nitrate black pigment is used as the collecting agent in the roughing in step (2) and the scavenging in step (3) of the flotation stage, and the amounts are 130g/t and 70g/t respectively, and the rest of the test conditions are the same as those in example 2 and serve as comparative example 4.
The results of the three sets of conditional tests are shown in table 2.
TABLE 2
Figure BDA0002863969430000051
As can be seen from the above table, the fine iron powder in example 2 of the present invention has a good desulfurization effect, and the flotation desulfurization effect of the combined collector using the butyl xanthate and the butylammonium melanophore according to the present invention is better than the test effect of using the single collector using the butyl xanthate and the butylammonium melanophore alone, and the mechanism that the collection effect can be enhanced by using the butyl xanthate and the butylammonium melanophore in combination according to a certain ratio is verified.
The embodiment 1 and the embodiment 2 show that the combined medicament of the invention can reduce the sulfur content of the iron concentrate to be less than 0.18 percent in the alkaline ore pulp environment, thereby improving the quality of the iron concentrate.

Claims (4)

1. A combined reagent for desulfurizing fine iron powder under alkaline conditions is characterized in that: comprises a combined activator and a combined collector, the combined activator comprises an activator 1, an activator 2 and an activator 3, the activator 1 is FeSO4·7H2O, activator 2 is NH4Cl, activating agent 3 is CuSO4·5H2O; the combined collector comprises butyl xanthate and butyl ammonium blackant;
the mass ratio of the activating agent 1 to the activating agent 2 to the activating agent 3 is 3:1: 0.8-1.2;
the mass ratio of the butyl xanthate to the ammonium buterate is 3: 1.
2. A method of desulfurizing pyrrhotite using the combination according to claim 1, characterized in that: the method comprises the following steps:
(1) size mixing:
carrying out primary grinding on magnetite containing pyrrhotite, wherein the grinding concentration is 65-70%, and the grinding fineness of-0.074 mm is 50-55%; adjusting the concentration of the obtained ore pulp to 19-23%, adding lime with the dosage of 2-10kg/t, adjusting the pH value of the ore pulp to 8-14, and stirring for 4 min;
(2) roughing:
in the stirring process, adding the activating agent 1 with the dosage of 300-700g/t, and stirring for 1 min; adding the solution prepared by the activating agents 2 and 3 with the dosage of 300-500g/t, and stirring for 3 min; adding a combined collecting agent with the dosage of 100-140g/t, adding a foaming agent with the dosage of 6-10g/t, stirring for 2min, and performing rough concentration for 12-14min to obtain rough concentration foam concentrate and rough concentration tailings;
(3) sweeping:
scavenging the roughed tailings, adding an activating agent 3 with the dosage of 60-80g/t, and stirring for 3 min; adding a combined collecting agent with the use amount of 50-70g/t, adding a foaming agent with the use amount of 6-10g/t, stirring for 2min, and scavenging for 10-12min to obtain scavenging foam and scavenging tailings;
(4) magnetic separation:
and carrying out magnetic separation on the scavenged tailings with the magnetic field intensity of 1400-1600Oe to obtain iron ore concentrate and tailings.
3. The method of claim 2, wherein: the solution prepared by adding the activating agent 2 and the activating agent 3 is prepared in advance according to the mass ratio of 1:0.8-1.2, and the reaction time is 15-60 min.
4. The method of claim 2, wherein: the foaming agent is 2# oil.
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Publication number Priority date Publication date Assignee Title
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CN109604070A (en) * 2018-12-05 2019-04-12 遵义市博莱金矿业有限责任公司 A kind of high-sulfur magnetic iron ore ore dressing medicament and its application method
CN110201798A (en) * 2019-04-19 2019-09-06 铜陵有色金属集团股份有限公司 A kind of DC activator and the acidless craft for sorting the sulphur, iron mineral that are inhibited by high-alkali and high calcium
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