CN112536154B - Reagent group for flotation separation of micro-fine lead oxide and ferrite and application thereof - Google Patents

Reagent group for flotation separation of micro-fine lead oxide and ferrite and application thereof Download PDF

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CN112536154B
CN112536154B CN202010917328.5A CN202010917328A CN112536154B CN 112536154 B CN112536154 B CN 112536154B CN 202010917328 A CN202010917328 A CN 202010917328A CN 112536154 B CN112536154 B CN 112536154B
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flotation
lead
ferrite
inhibitor
sodium
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CN112536154A (en
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唐鸿鹄
王丽
李梦闪
胡岳华
孙伟
韩海生
杨越
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Central South University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION 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
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00Flotation
    • B03D1/001Flotation agents
    • B03D1/018Mixtures of inorganic and organic compounds
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00Compounds of iron
    • C01G49/02Oxides; Hydroxides
    • C01G49/06Ferric oxide [Fe2O3]
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION 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
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2201/00Specified effects produced by the flotation agents
    • B03D2201/005Dispersants
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION 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
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2201/00Specified effects produced by the flotation agents
    • B03D2201/02Collectors
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION 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
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2201/00Specified effects produced by the flotation agents
    • B03D2201/06Depressants
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION 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
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2203/00Specified materials treated by the flotation agents; Specified applications
    • B03D2203/02Ores
    • B03D2203/04Non-sulfide ores

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Abstract

The invention relates to the field of comprehensive utilization of resources, and relates to a reagent set for separating micro-fine lead oxide compounds and ferrite compounds by flotation and application thereof. The reagent group comprises a wetting dispersant, a collector and an inhibitor; the wetting dispersant is a surfactant; the collecting agent is alkyl sulfate; the inhibitor is at least one selected from phosphate, dihydrogen phosphate, pyrophosphate, tripolyphosphate, polyphosphate and hexametaphosphate. The chemical group designed by the invention is used in the flotation process, and micro-fine lead oxide compounds and ferrite compounds can be efficiently separated by flotation. The agent group can achieve the effects of remarkable agglomeration of fine particle flotation concentrate, high flotation rate and excellent filtering performance. The invention solves the problems of long concentrate flotation time and difficult product dehydration in the traditional separation process.

Description

Reagent group for flotation separation of micro-fine lead oxide and ferrite and application thereof
Technical Field
The invention relates to the field of comprehensive utilization of resources, in particular to a reagent group for separating micro-fine lead oxide compounds and ferrite compounds by flotation and application thereof; in particular to a method for flotation, separation and recovery of smoke dust containing micro-fine lead oxide and iron oxide in the steel smelting process.
Background
The method is characterized in that iron and steel smelting smoke dust, such as electrostatic precipitator dust and gas ash of a sintering machine, is one of main solid wastes in the sintering and iron-making links of iron and steel enterprises, because the content of alkali metals such as potassium and sodium in the sintering electrostatic precipitator dust or gas ash is high, and the content of zinc in the gas ash of an iron-making cloth bag is high, if the electrostatic precipitator dust or the gas ash and the gas ash are directly reused for sintering a mixture, the circulating enrichment of elements such as potassium, sodium and zinc can bring negative effects to the operation of a blast furnace. The dust or gas ash contains iron, carbon and a small amount of nonferrous metal such as lead, silver and copper, belongs to precious secondary resources, and if the dust or gas ash cannot be effectively treated and utilized, not only is the resources wasted, but also the environment is greatly polluted. The gas ash is comprehensively utilized, so that the method has good economic benefit and high environmental and social benefits. Therefore, how to adopt advanced and practical high and new technology to carry out harmless and resource comprehensive treatment on the electro-precipitator dust or the gas ash and the gas ash is an important subject to be researched by the steel enterprises at present. Because the fly ash or the gas ash has the characteristics of complex components, fine granularity, small density, high ash content, complex mineral structure and close symbiotic relationship, the recovery rate of elements such as lead and silver recovered from the fly ash or the gas ash is low, and the waste of resources such as lead and silver is caused, a new technology is developed from the physicochemical properties of the fly ash or the gas ash to realize the recovery of valuable elements such as lead and silver, and the like, so that the method has great significance for the resource comprehensive utilization of the fly ash or the gas ash.
The conventional lead oxide and iron oxide flotation separation process is usually carried out by adopting a sulfide-xanthate flotation process and a sulfide-melanophore flotation process, even an expensive long-chain mercapto (such as dodecyl mercaptan) collecting agent, however, the agents are often poor in effect in the separation process of micro-fine lead oxide and iron oxide minerals, although a certain flotation separation effect is achieved, the recovery rate is low, and the traditional agents have the following defects in the process of treating iron and steel smelting dust; the development of a novel drug group which is separated efficiently, has industrial application value and is environmentally friendly and a method for using the novel drug group scientifically becomes urgent.
1) When the traditional vulcanization-xanthate and vulcanization-black flotation is used for separating micro-fine particle lead oxide and iron oxide, the problems of foam vacuity, extremely long flotation time and the like often exist; in the prior art, the flotation time is usually more than half an hour in order to ensure the recovery rate of lead;
2) in the traditional vulcanization-xanthate and vulcanization-black flotation, the amount of sodium sulfide and the vulcanization time are difficult to control, and the time operation is inconvenient; particularly, when the steel smelting smoke dust is treated, the vulcanization time is long, and generally 20-40 min is needed;
3) the flotation separation of fine particle lead oxide and iron oxide by conventional oleic acid and other oxidized ore agents has the problems of poor selectivity, difficult control of the flotation process and the like.
Meanwhile, the problem that the micro-fine particle lead oxide and iron oxide are difficult to separate by flotation is not only in the separation process of natural minerals, but also in lead oxide, iron oxide waste residues and waste dust generated in the hydrometallurgy and pyrometallurgy processes, particularly in electrostatic precipitator dust of a steel smelting sintering machine, wherein the lead content is 1.5-30%, and the iron content is 10-50%. If the minerals, waste residues and waste dust containing lead and other heavy metals are not properly treated, the environment is threatened; meanwhile, the lead mineral and the lead waste slag and dust often contain considerable content of noble metals such as silver and the like, so that the method has a high recycling value. The implementation of the value environmental protection method, the treatment and recovery of lead-containing waste materials are urgent for a plurality of smelting enterprises.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a reagent set for separating micro-fine lead oxide compounds and ferrite compounds by flotation and application thereof. When the medicament set designed by the invention is used, the process is simple, the operation is convenient, and the recovery rate is high. When the treated object is steel smelting smoke dust such as dust removal ash or gas ash; the effect and benefit are more obvious.
The invention relates to a reagent group for flotation separation of micro-fine lead oxide and ferrite; the reagent group comprises a wetting dispersant, a collector and an inhibitor;
the wetting dispersant is a nonionic surfactant;
the collecting agent is alkyl sulfate;
the inhibitor is at least one selected from phosphate, dihydrogen phosphate, pyrophosphate, tripolyphosphate, polyphosphate and hexametaphosphate.
Preferably, the invention relates to a reagent group for flotation separation of micro-fine lead oxide and ferrite; the collecting agent is selected from at least one of sodium dodecyl sulfate, sodium tetradecyl sulfate, sodium hexadecyl sulfate and sodium octadecyl sulfate;
the inhibitor is at least one selected from sodium pyrophosphate, sodium tripolyphosphate and sodium polyphosphate.
Preferably, the invention relates to a reagent group for flotation separation of micro-fine lead oxide and ferrite; the wetting dispersant is at least one selected from the group consisting of a nonionic surfactant Trion X-100, OP series and NP series. The dosage of the wetting dispersant is 5ppm to 150 ppm. Namely, 5g to 150g of wetting dispersant is needed to be added into 1 ton of ore pulp.
Preferably, the Trion X-100 comprises polyethylene glycol octyl phenyl ether; the OP series comprises octylphenol polyoxyethylene ether; the NP series includes nonylphenol polyoxyethylene ether. The dosage of the wetting dispersant is 5ppm to 150 ppm. Namely, 5g to 150g of wetting dispersant is needed to be added into 1 ton of ore pulp.
Preferably, the dosage range of the collecting agent is as follows: 50 g/t-300 g/t.
Preferably, the dosage range of the inhibitor is as follows: 50 g/t-300 g/t.
In the technical development process of the invention, cationic collectors dodecylamine and CTAB are tried, and dodecyl mercaptan and sodium dodecyl sulfate are also tested as the collectors for separating micro-fine lead oxide and iron oxide, but the separation effect is not ideal, and the foam mineralization is not good in many times.
In the technical development process, the strength of the action of the groups and lead ions and iron ions is preliminarily analyzed according to the group radius and the theory of the soft and hard acids, the phosphate and the polyphosphate can be selectively inhibited through experiments, and the results of experimental verification show that the inhibition effect of sodium dihydrogen phosphate, sodium pyrophosphate, sodium tripolyphosphate, sodium polyphosphate, sodium hexametaphosphate and sodium fluosilicate on iron oxide is better. The dosage of the inhibitor is usually low, 50-300 g/t, and the inhibiting effect is as follows: sodium pyrophosphate, sodium polyphosphate, sodium tripolyphosphate, sodium dihydrogen phosphate and sodium hexametaphosphate, wherein the sodium pyrophosphate and the sodium polyphosphate basically do not inhibit the flotation of lead oxide, and the sodium hexametaphosphate has a larger separation effect but also inhibits the flotation of lead oxide, so that the flotation effect of lead oxide and iron oxide is reduced.
Preferably, the invention relates to the application of a reagent group for flotation separation of micro-fine lead oxide and ferrite; the application comprises the following steps: the method comprises the steps of using a reagent set in the flotation process, and separating micro-fine lead oxide compounds and iron oxide compounds in a treatment object through flotation, wherein the particle size of the treatment object is 1-40 microns.
Preferably, the invention relates to the application of a reagent group for flotation separation of micro-fine lead oxide and ferrite;
when the C content in the treated object is less than 5wt%, the application thereof comprises the following steps:
step A
Uniformly mixing the treated object with the wetting dispersant in the medicament group to obtain slurry to be separated;
step B
Adding a collecting agent and an inhibitor in a reagent group into the slurry to be separated, carrying out flotation separation on micro-fine particle lead oxide and iron oxide, and carrying out flotation to obtain concentrate and tailings;
when the C content in the treated object is more than or equal to 5wt%, the application comprises the following steps:
step one
Uniformly mixing the treated object with the wetting dispersant in the medicament group to obtain slurry to be separated;
step two
Taking the slurry to be separated in the step as a raw material, taking neutral oil as a carbon collecting agent and MIBC or terpineol as a foaming agent, and performing flotation and decarburization;
step three
Adding a collecting agent and an inhibitor in the reagent group into the decarbonized ore pulp, and performing flotation to obtain concentrate and tailings;
the collecting agent is alkyl sulfate;
the inhibitor is at least one selected from phosphate, dihydrogen phosphate, pyrophosphate, tripolyphosphate, polyphosphate and hexametaphosphate.
The invention relates to the application of a reagent group for flotation separation of micro-fine lead oxide and ferrite; the object to be treated is preferably a smoke containing a fine lead oxide compound and a ferrite compound generated in a steel smelting process.
The invention relates to the application of a reagent group for flotation separation of micro-fine lead oxide and ferrite; the lead-oxygen compound is at least one selected from lead sulfate, lead hydroxychloride and lead oxide. The ferrite compound is at least one selected from iron sesquioxide (which can be produced in natural minerals, hydrometallurgical or pyrometallurgical engineering) and magnetite. In the present invention the lead oxide may be a natural mineral or may be produced in hydrometallurgical and/or pyrometallurgical processes. The iron oxide compounds in the present invention may be natural minerals or may be produced in hydrometallurgical and/or pyrometallurgical processes.
The invention relates to the application of a reagent group for flotation separation of micro-fine lead oxide and ferrite; according to the difference of iron content in the feed, the flotation tailings can be directly used as iron ore concentrate to return to the iron and steel smelting process or be continuously used as iron extraction raw materials.
Preferably, the invention relates to the application of a reagent group for flotation separation of micro-fine lead oxide and ferrite; in the step A and/or the step one, when the treatment target has a large amount of soluble alkali metal salt, the concentrated solution may be circulated and the alkali metal salt may be recovered therefrom.
When the processing object is smoke dust containing micro-fine lead oxide and ferrite generated in the steel smelting process, the main components are as follows: the grain size of the alkali metal chloride salt KCl, NaCl and iron oxide (mainly ferric oxide after high-temperature treatment) is generally 5-40 microns, the Fe content fluctuates 5-40%, the lead content of lead salt (mostly lead oxide such as hydroxyl lead chloride and lead sulfate) fluctuates 1-20% (due to the difference of iron ore raw materials used in sintering and the different content of the alkali metal chloride salt generated in the sintering process), and the grain size is generally 1-10 microns.
Preferably, the invention relates to the application of a reagent group for flotation separation of micro-fine lead oxide and ferrite; during the flotation decarburization, the carbon collecting agent is selected from one or more of kerosene and diesel oil, and the using amount of the carbon collecting agent is 100 g/t-300 g/t;
the amount of the foaming agent is 200 g/t-500 g/t when flotation decarburization is carried out.
As a preferable scheme, the invention relates to the application of a reagent group for separating micro-fine lead oxide compounds and ferrite compounds by flotation; in the step B or the step III, the pH value of the slurry is controlled to be 5.0-7.0, preferably 5.5-6.5 during flotation; controlling the dosage range of the collecting agent to be 50 g/t-300 g/t; the dosage of the inhibitor is controlled to be 50 g/t-300 g/t.
The agent group can achieve the effects of remarkable agglomeration of fine particle flotation concentrate, high flotation rate and excellent filtering performance. And further solves the problems of long concentrate flotation time and difficult product dehydration in the traditional separation process.
When the reagent set designed by the invention is used for flotation separation of micro-fine lead oxide and ferrite, the alkyl sulfate collecting agent is extremely small in dosage, most of the alkyl sulfate collecting agent is adsorbed on the surface of particles, so that the pollution to water is less, and the biodegradability of the collecting agent is high. Meanwhile, the inhibitor is low in dosage and can be recycled, so that the scheme of the invention has the advantages of environmental protection and sustainable application; meanwhile, the separation effect and the recovery rate of each material are extremely high, and the method has obvious industrial application value.
Principles and advantages
According to the invention, the strength of the action of the group with lead ions and iron ions is preliminarily analyzed according to the group radius and the theory of the stearic acid, and the phosphate and the polyphosphate can be selectively inhibited through experiments. Under the condition of lower usage amount of 50-300 g/t, the inhibition effect is explored; specifically, sodium pyrophosphate, sodium polyphosphate, sodium tripolyphosphate, sodium dihydrogen phosphate and sodium hexametaphosphate, sodium pyrophosphate and sodium polyphosphate basically do not inhibit the flotation of lead oxide, and sodium hexametaphosphate has a larger separation effect but also inhibits the flotation of lead oxide, so that the flotation effect of lead oxide and iron oxide is reduced. Therefore, the optimized inhibitor of the invention is sodium pyrophosphate and/or sodium polyphosphate.
When the reagent set designed by the invention is used for flotation separation of micro-fine lead oxide and ferrite, the alkyl sulfate as the collecting agent is extremely small in dosage, most of the alkyl sulfate is adsorbed on the surface of particles, so that the pollution to water is little, and the biodegradability of the collecting agent is high. Meanwhile, the inhibitor is low in dosage and can be recycled, so that the scheme of the invention has the advantages of environmental protection and sustainable application; meanwhile, the separation effect and the recovery rate of each material are extremely high, and the method has obvious industrial application value.
Drawings
Fig. 1 is a process flow diagram of a method for recycling precipitator dust or gas ash according to an embodiment of the present invention.
FIG. 2 is a Gaudin selectivity index profile obtained when experiments were performed on different collectors in example 1 and comparative examples 1.1-1.4;
FIG. 3 is a graph showing the Gaudin selectivity index distribution obtained when experiments were performed on the different inhibitors of example 2 and comparative examples 2.1-2.4.
Detailed Description
In order to facilitate clear understanding of the technical solution of the present invention, the following detailed description is given with reference to the embodiments.
Example 1
In the process of research on pure mineral flotation in a laboratory, micron-sized lead oxide (lead hydroxychloride PbOHCl and lead sulfate PbSO) is respectively carried out by adopting different types of collecting agents4) And micron-sized iron oxide (Fe)2O3) And calculating a Gaudin Selectivity index (Selectivity index) based on the optimum separation effect of each agentThe flotation separation effect is measured in a homogenization mode, and the larger the selectivity index is, the better the flotation separation effect of the used reagent groups is.
The Gaudin selectivity index calculation formula is as follows:
Figure BDA0002665474150000061
wherein epsilonPb-KRepresenting the recovery of lead in the concentrate, epsilonPb-XRepresenting the recovery of lead from the tailings,. epsilonFe-KRepresenting the recovery of iron, epsilon, from the concentrateFe-XRepresenting the recovery of iron from the tailings.
In the flotation separation experiment, the using amount of the collecting agent is 60g/t, and the flotation pH value is controlled to be 6.0-6.5.
When sodium dodecyl sulfate (SLS) is used as collecting agent, micron-class hydroxy lead chloride PbOHCl and lead sulfate PbSO4With micron-sized iron oxide (Fe)2O3) The Gaudin selectivity indices of 5.4 and 5.1, respectively.
Comparative example 1.1: when dodecylamine (DDA) is used as collecting agent, micron-class hydroxy lead chloride PbOHCl or lead sulfate PbSO4With micron-sized iron oxide (Fe)2O3) The Gaudin selectivity indices of (1) are 3.4 and 3.3, respectively.
Comparative example 1.2: when Cetyl Trimethyl Ammonium Bromide (CTAB) is adopted as a collecting agent, micron-sized lead hydroxychloride PbOHCl and lead sulfate PbSO4With micron-sized iron oxide (Fe)2O3) The Gaudin selectivity indices of 4.6 and 2.1, respectively.
Comparative example 1.3: when sodium oleate (NaOl) is used as a collecting agent, micron-sized lead hydroxychloride PbOHCl and lead sulfate PbSO4With micron-sized iron oxide (Fe)2O3) The Gaudin selectivity index of (1) is 2.9 and 1.9 respectively.
Comparative example 1.4: when Sodium Dodecyl Sulfate (SDS) is used as collecting agent, micron-class hydroxy lead chloride PbOHCl and lead sulfate PbSO4With micron-sized iron oxide (Fe)2O3) The Gaudin selectivity indices of (1) were 3.2 and 3.3, respectively.
Flotation separation of micron-sized lead oxide (lead hydroxychloride PbOHCl, lead sulfate PbSO) by using several collecting agents4) And micron-sized iron oxide (Fe)2O3) A comparison of Gaudin selectivity indices is shown in FIG. 2.
Example 2
In the process of research on pure mineral flotation in a laboratory, sodium dodecyl sulfate (SLS) is used as a collecting agent and different types of inhibitors are used for respectively carrying out micron-sized lead oxide (lead hydroxychloride PbOHCl and lead sulfate PbSO)4) And micron-sized iron oxide (Fe)2O3) And calculating a Gaudin Selectivity index (Selectivity index) based on the optimal separation effect of each medicament to uniformly measure the separation effect, wherein the larger the Selectivity index is, the better the flotation separation effect of the used medicament groups is.
The Gaudin selectivity index calculation formula is as follows:
Figure BDA0002665474150000071
wherein epsilonPb-KRepresenting the recovery of lead in the concentrate, epsilonPb-XRepresenting the recovery of lead from the tailings,. epsilonFe-KRepresenting the recovery of iron, epsilon, from the concentrateFe-XRepresenting the recovery of iron from the tailings.
In the flotation separation experiment, the using amount of the collecting agent is 60g/t, the using amount of the inhibitor is 100g/t, and the flotation pH value is controlled to be 6.0-6.5.
When only sodium dodecyl sulfate (SLS) is used as a collecting agent, micron-sized lead hydroxychloride PbOHCl and lead sulfate PbSO4With micron-sized iron oxide (Fe)2O3) The Gaudin selectivity indices of 5.4 and 5.7, respectively.
Example 2.1: when sodium dihydrogen phosphate (P1) is used as an inhibitor and sodium dodecyl sulfate (SLS) is used as a collecting agent, micron-sized lead hydroxychloride PbOHCl and lead sulfate PbSO are adopted4With micron-sized iron oxide (Fe)2O3) The Gaudin selectivity indices of 8.9 and 8.3, respectively.
Example 2.2: when sodium pyrophosphate (P2) is used as an inhibitor and sodium dodecyl sulfate (SLS) is used as a collecting agent, micron-sized lead hydroxychloride PbOHCl and lead sulfate PbSO4With micron-sized iron oxide (Fe)2O3) Has a Gaudin selectivity index of 15.4 and13.5。
example 2.3: when sodium tripolyphosphate (P3) is used as inhibitor and Sodium Lauryl Sulfate (SLS) is used as collector, micron-sized lead hydroxychloride PbOHCl and lead sulfate PbSO4With micron-sized iron oxide (Fe)2O3) The Gaudin selectivity indices of 11.2 and 12.6, respectively.
Example 2.4: when sodium hexametaphosphate (P4) is used as an inhibitor and sodium dodecyl sulfate (SLS) is used as a collecting agent, micron-sized lead hydroxychloride PbOHCl and lead sulfate PbSO are adopted4With micron-sized iron oxide (Fe)2O3) The Gaudin selectivity indices of 6.8 and 7.03, respectively.
Flotation separation of micron-sized lead oxide (lead hydroxychloride PbOHCl, lead sulfate PbSO) by using several inhibitors4) And micron-sized iron oxide (Fe)2O3) A comparison of Gaudin selectivity indices is shown in FIG. 3.
Example 3
The method is adopted to treat the electrostatic precipitator dust of the steel smelting sintering machine of Wuhan steel containing 43.13% of iron, 6.06% of carbon, 1.20% of lead, 96g/t of silver and 15.88% of soluble salt. a) Wetting and dispersing the fly ash by using a 5ppm Trion X-100 solution, and mixing the slurry for 5min to obtain dispersed ore slurry; b) after solid-liquid separation, the solution part can be used as an extraction raw material of alkali metals such as potassium, sodium and the like, the solid part is added with water and stirred to be 30 percent of ore pulp solution, and the flotation is continuously carried out; c) using kerosene as a collecting agent and terpineol as a foaming agent to remove carbon in the raw materials by flotation, and obtaining decarburized ore pulp and carbon concentrate, wherein the using amounts of the collecting agent and the foaming agent are respectively 50g/t and 200 g/t; d) adding collecting agents sodium dodecyl sulfate and inhibitor sodium pyrophosphate into the decarbonized ore pulp, wherein the using amounts of the collecting agents and the inhibitors are respectively 50g/t and 200g/t, carrying out flotation separation on micro-fine lead oxide and micro-fine iron oxide at the pH value of 5.5, and carrying out rough separation for 5min to obtain lead-silver concentrate and iron concentrate, wherein the water content of the concentrate is lower than 10%. The final experimental results are shown in table 1.
TABLE 1 Wuhan iron and Steel smelting sintering machine electrostatic precipitator dust flotation experimental results
Figure BDA0002665474150000081
Comparative example 2: other conditions and steps are consistent with those of example 3, only the step d) is changed into the step using the activating agent sodium sulfide and the collecting agent potassium butyl xanthate, the using amounts are 2.5kg/t and 500g/t respectively, when the similar flotation effect is achieved, the action time of the sodium sulfide needs to be increased by 25min, in addition, the roughing time needs to be increased to 20min, and finally, the water content of the lead-silver concentrate is 21%, and the water content of the iron concentrate is 18%.
Example 4
The method is adopted to treat electrostatic precipitator dust of the steel smelting sintering machine of new Wuan steel containing iron 39.13%, lead 1.41%, silver 86g/t and soluble salt 19.80%. a) Wetting and dispersing the fly ash by adopting 20ppm octyl phenol polyoxyethylene ether OP-10 solution, and mixing the slurry for 5min to obtain dispersed ore slurry; b) after solid-liquid separation, the solution part can be used as an extraction raw material of alkali metals such as potassium, sodium and the like, the solid part is added with water and stirred to 25 percent of ore pulp solution, and the flotation is continuously carried out; c) adding collecting agent sodium dodecyl sulfate and inhibitor sodium polyphosphate into the ore pulp, wherein the using amounts of the collecting agent and the inhibitor are 75g/t and 300g/t respectively, carrying out flotation separation on the micro-fine particle lead oxide and the micro-fine particle iron oxide at the pH value of 6.5, and carrying out rough concentration for 6min to obtain lead-silver concentrate and iron concentrate, wherein the water content of the concentrate is about 11%. The final experimental results are shown in table 2.
TABLE 2 New Wuan iron and steel smelting sintering machine electrostatic dust removal flotation experimental results
Figure BDA0002665474150000091
Comparative example 3: the other conditions and steps are identical to those of example 4, the addition of octylphenol polyoxyethylene ether OP-10 is eliminated only in step a), and the concentrate yield increases significantly during flotation: 17.50 percent, lead grade in the lead-silver concentrate is only 8.19 percent, silver content is only 368g/t, iron concentrate grade is only 41.96 percent, recovery rate is 70.85 percent, and separation effect is obviously reduced.
Example 5
The method is adopted to treat the electrostatic dust removal ash of the steel smelting sintering machine, wherein the sunshine steel contains 39.47% of iron, 1.39% of lead, 82g/t of silver and 19.56% of soluble salt. a) Wetting and dispersing the fly ash by adopting a 50ppm nonylphenol polyoxyethylene ether NP-10 solution, and mixing the slurry for 5min to obtain dispersed ore slurry; b) after solid-liquid separation, the solution part can be used as an extraction raw material of alkali metals such as potassium, sodium and the like, the solid part is added with water and stirred to be 30 percent of ore pulp solution, and the flotation is continuously carried out; c) adding collecting agents, namely sodium tetradecyl sulfate and inhibitor potassium pyrophosphate, into the ore pulp, wherein the using amounts of the collecting agents and the inhibitor are respectively 50g/t and 200g/t, carrying out flotation separation on micro-fine particle lead oxide and micro-fine particle iron oxide at the pH value of 6.5, and carrying out rough concentration for 6min to obtain lead-silver concentrate and iron concentrate, wherein the water content of the concentrate is lower than 12%. The final experimental results are shown in table 3.
TABLE 3 Electrostatic precipitator dust flotation experiment results of sunshine steel smelting sintering machine
Figure BDA0002665474150000092
Figure BDA0002665474150000101
Comparative example 4: the other conditions and steps are identical to those of example 5, only in step c) the amount of sodium pyrophosphate is reduced to 25g/t and the concentrate yield during flotation is increased to: 11.40 percent, the lead grade in the lead-silver concentrate is 14.21 percent, the silver content is 543g/t, the iron concentrate grade is 43.26 percent, the iron recovery rate is 78.11 percent, and the separation effect is reduced.
Example 6
The method is adopted to treat electrostatic precipitator dust of the steel smelting sintering machine which contains iron 28.15%, carbon 12.36%, lead 6.27%, silver 210g/t and soluble salt 26.15%. a) Wetting and dispersing the fly ash by adopting a 100ppm Trion X-100 solution, and mixing the slurry for 5min to obtain dispersed ore slurry; b) after solid-liquid separation, the solution part can be used as an extraction raw material of alkali metals such as potassium, sodium and the like, the solid part is added with water and stirred to 40 percent of ore pulp solution, and the flotation is continuously carried out; c) diesel oil is used as a collecting agent, MIBC is used as a foaming agent to remove carbon in the raw materials in a flotation mode, decarburized ore pulp and carbon concentrate are obtained, and the using amounts of the collecting agent and the foaming agent are 300g/t and 500g/t respectively; d) adding collecting agents of sodium tetradecyl sulfate and inhibitor sodium tripolyphosphate into the decarbonized ore pulp, wherein the using amounts of the collecting agents and the inhibitor are 300g/t and 300g/t respectively, carrying out flotation separation on the micro-fine particle lead oxide and the micro-fine particle iron oxide at the pH value of 6.5, and carrying out rough separation for 6.5min to obtain lead-silver concentrate and iron concentrate, wherein the water content of the concentrate is about 12%. The final experimental results are shown in table 4.
TABLE 4 electrostatic precipitator dust flotation experimental results of Wuhan iron and steel smelting sintering machine
Figure BDA0002665474150000102
Example 7
The method is adopted to treat electrostatic precipitator dust of the steel smelting sintering machine, which contains Hunan pond steel, 24.65% of iron, 8.47% of lead, 242g/t of silver and 36.19% of soluble salt. a) Wetting and dispersing the fly ash by adopting a 110ppm octyl phenol polyoxyethylene ether OP-20 solution, and mixing the slurry for 5min to obtain dispersed ore slurry; b) after solid-liquid separation, the solution part can be used as an extraction raw material of alkali metals such as potassium, sodium and the like, the solid part is added with water and stirred to 20 percent of ore pulp solution, and the flotation is continuously carried out; c) adding a collecting agent sodium hexadecyl sulfate and an inhibitor sodium tripolyphosphate into the ore pulp, wherein the using amounts of the collecting agent and the inhibitor are 230g/t and 240g/t respectively, carrying out flotation separation on the micro-fine particle lead oxide and the micro-fine particle iron oxide at the pH value of 6.5, and carrying out rough concentration for 8min to obtain lead-silver concentrate and iron concentrate, wherein the water content of the concentrate is lower than 13%. The final experimental results are shown in table 5.
TABLE 5 Hunan Tan iron and steel smelting sintering machine electrostatic precipitator ash flotation experimental results
Figure BDA0002665474150000111
Example 8
The method is adopted to treat the electrostatic precipitator dust of the steel smelting sintering machine, which contains 23.72 percent of iron, 9.02 percent of lead, 248g/t of silver and 35.07 percent of soluble salt in the Panzhihua steel. a) Wetting and dispersing the fly ash by adopting a 150ppm nonylphenol polyoxyethylene ether NP-20 solution, and mixing for 5min to obtain dispersed ore pulp; b) after solid-liquid separation, the solution part can be used as an extraction raw material of alkali metals such as potassium, sodium and the like, the solid part is added with water and stirred to 20 percent of ore pulp solution, and the flotation is continuously carried out; c) adding a collecting agent potassium octadecyl sulfate and an inhibitor potassium phosphate into the ore pulp, wherein the using amounts of the collecting agent and the inhibitor are 180g/t and 260g/t respectively, performing flotation separation on the micro-fine lead oxide and the micro-fine iron oxide at the pH of 6.5 for 8min to obtain lead-silver concentrate and iron concentrate, and the water content of the concentrate is about 12.5%. The final experimental results are shown in table 6.
TABLE 6 Panzhihua iron and steel smelting sintering machine electrostatic precipitator dust flotation experimental results
Figure BDA0002665474150000112
Figure BDA0002665474150000121
Example 9
The electrostatic precipitator dust of the steel smelting sintering machine, which contains 5.14% of iron, 7.68% of lead, 285g/t of silver and 49.80% of soluble salt, is treated by the method. a) Wetting and dispersing the fly ash by adopting a 50ppm Trion X-100 solution, and mixing the slurry for 5min to obtain dispersed ore slurry; b) after solid-liquid separation, the solution part can be used as an extraction raw material of alkali metals such as potassium, sodium and the like, the solid part is added with water and stirred to 20 percent of ore pulp solution, and the flotation is continuously carried out; c) adding collecting agents of potassium dodecyl sulfate and sodium pyrophosphate and sodium tripolyphosphate 1:1 mixed inhibitor into ore pulp, wherein the using amounts of the collecting agents and the inhibitor are 150g/t and 50g/t respectively, carrying out flotation separation on micro-fine lead oxide and micro-fine iron oxide at the pH value of 6.5, and carrying out roughing for 8min to obtain lead-silver concentrate and iron concentrate, wherein the water content of the concentrate is about 12%. The final experimental results are shown in table 7.
TABLE 7 electrostatic precipitator dust flotation experimental results of Shaoguan steel smelting sintering machine
Figure BDA0002665474150000122
It can be seen from embodiments 1 to 9 that the recycling method of the precipitator dust or the gas ash provided by the present invention can recycle a large amount of elements such as lead, silver, etc. in the precipitator dust or the gas ash, and has the advantages of simple process, convenient operation, high recycling rate, realization of efficient comprehensive utilization of the precipitator dust or the gas ash, and high economic benefit.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (9)

1. A reagent group for flotation separation of micro-fine lead oxide and ferrite; the method is characterized in that: using a reagent set in the flotation process, and separating micro-fine lead oxide and iron oxide compounds in a treatment object through flotation, wherein the particle size of the treatment object is 1-40 micrometers; the reagent group comprises a wetting dispersant, a collector and an inhibitor;
the wetting dispersant is at least one selected from a nonionic surfactant Trion X-100, an OP series and an NP series;
the collector is alkyl sulfate;
the inhibitor is selected from at least one of phosphate, dihydrogen phosphate, pyrophosphate, tripolyphosphate, polyphosphate and hexametaphosphate;
the dosage of the wetting dispersant is 5 ppm-150 ppm;
the dosage range of the collecting agent is as follows: 50 g/t-300 g/t;
the dosage range of the inhibitor is as follows: 50g/t to 300 g/t.
2. The reagent set of claim 1 for flotation separation of fine lead oxide compounds from ferrite compounds; the method is characterized in that:
the collecting agent is selected from at least one of sodium dodecyl sulfate, sodium tetradecyl sulfate, sodium hexadecyl sulfate and sodium octadecyl sulfate;
the inhibitor is at least one selected from sodium pyrophosphate, sodium tripolyphosphate and sodium polyphosphate.
3. Use of a set of reagents according to any one of claims 1-2 for flotation separation of finely divided lead oxide compounds from ferrite compounds; the method is characterized in that:
the application comprises the following steps: a reagent set is used in the flotation process, and micro-fine lead oxide and iron oxide compounds in a treatment object are separated through flotation, wherein the particle size of the treatment object is 5-40 micrometers.
4. Use of a set of reagents according to claim 3 for flotation separation of fine lead oxides and ferrite compounds; it is characterized in that;
when the C content in the treated object is less than 5wt%, the application thereof comprises the following steps:
step A
Uniformly mixing the treated object with the wetting dispersant in the medicament group to obtain slurry to be separated;
step B
Adding a collecting agent and an inhibitor in a reagent group into the slurry to be separated, carrying out flotation separation on micro-fine particle lead oxide and iron oxide, and carrying out flotation to obtain concentrate and tailings;
when the C content in the treated object is 5wt% or more, the application thereof comprises the following steps:
step one
Uniformly mixing the treated object with the wetting dispersant in the medicament group to obtain slurry to be separated;
step two
Taking the slurry to be separated in the step as a raw material, taking neutral oil as a carbon collecting agent and MIBC or terpineol as a foaming agent, and performing flotation and decarburization;
step three
Adding a collecting agent and an inhibitor in the reagent group into the decarbonized ore pulp, and performing flotation to obtain concentrate and tailings;
the collecting agent is alkyl sulfate;
the inhibitor is at least one selected from phosphate, dihydrogen phosphate, pyrophosphate, tripolyphosphate, polyphosphate and hexametaphosphate.
5. Use of a set of reagents according to claim 3 for flotation separation of fine lead oxides and ferrite compounds; the method is characterized in that: the treated object is preferably smoke containing micro-fine lead oxide and ferrite in the steel smelting process.
6. Use of a kit according to claim 3 for flotation separation of fine lead oxides and ferrite compounds; the method is characterized in that:
the lead-oxygen compound is at least one selected from lead sulfate, lead hydroxychloride and lead oxide;
the ferrite compound is at least one selected from iron sesquioxide and magnetite.
7. Use of a kit according to claim 3 for flotation separation of fine lead oxides and ferrite compounds; the method is characterized in that: in the step a and/or the step one, when the soluble alkali metal salt is large in the object of treatment, the concentrated solution may be circulated and the alkali metal salt may be recovered therefrom.
8. Use of a set of reagents according to claim 4 for flotation separation of fine lead oxides and ferrite compounds; the method is characterized in that:
during flotation decarburization, the carbon collecting agent is selected from one or more of kerosene and diesel oil, and the using amount of the carbon collecting agent is 100 g/t-300 g/t;
and during flotation decarburization, the using amount of the foaming agent is 200 g/t-500 g/t.
9. Use of a set of reagents according to claim 4 for flotation separation of fine lead oxides and ferrite compounds; the method is characterized in that: in the step B or the step III, the pH value of the slurry is controlled to be 5.0-7.0 during flotation;
controlling the dosage range of the collecting agent to be 50-300 g/t; the dosage of the inhibitor is controlled to be 50 g/t-300 g/t.
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