CN113355511A - Method for selectively reducing vanadium and titanium content in vanadium-titanium magnetite concentrate through ammonium-ammonia oxidation leaching system - Google Patents
Method for selectively reducing vanadium and titanium content in vanadium-titanium magnetite concentrate through ammonium-ammonia oxidation leaching system Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/12—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic alkaline solutions
- C22B3/14—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic alkaline solutions containing ammonia or ammonium salts
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1236—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by wet processes, e.g. by leaching
- C22B34/1254—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by wet processes, e.g. by leaching using basic solutions or liquors
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
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Abstract
The invention provides a method for selectively reducing the content of vanadium and titanium in vanadium-titanium magnetite concentrate by an ammonium-ammonia oxidation leaching system, which comprises the following steps: s1, preparing an ammonium-ammonia system composite leaching agent; s2, grinding the minerals, mixing the ground minerals with the ammonium-ammonia system composite leaching agent obtained in the step S1, and carrying out selective alkaline hydrolysis leaching reaction to obtain a reacted mixture; s3, performing magnetic separation on the mixture obtained in the step S2 to obtain vanadium-titanium magnetite concentrate and tailing pulp, performing solid-liquid separation on the tailing pulp to obtain filtrate, and returning the filtrate to the step S2 for recycling; the method provided by the invention can effectively transfer impurities such as vanadium, titanium and the like in the minerals to the liquid phase, and the iron is retained in the solid phase, so that the high-efficiency separation of the impurities such as iron, vanadium, titanium and the like is realized; and finally, the separation of the vanadium-titanium magnetite concentrate from gangue minerals is realized through a magnetic separation mode, the method is simple to operate, low in requirement on raw materials, low in operation cost and good in treatment effect, the content of iron in the vanadium-titanium magnetite concentrate can be fully increased, and high-quality iron concentrate is provided for blast furnace smelting.
Description
Technical Field
The invention relates to the technical field of metallurgy, in particular to a method for selectively reducing the content of vanadium and titanium in vanadium-titanium magnetite concentrate by an ammonium-ammonia oxidation leaching system.
Background
Vanadium-titanium magnetite is a multi-metal-element composite ore, and mainly contains symbiotic magnetite containing iron, vanadium and titanium as main elements, and various impurities exist in the ore, so that the vanadium-titanium magnetite is not easy to remove. At present, the methods for removing impurities from vanadium titano-magnetite include the following steps: alkaline leaching process, roasting-alkaline leaching process, physical separation process and roasting-magnetic separation process.
For the conventional alkaline leaching process at present, the sodium silicate/potassium and the sodium aluminate/potassium generated in the alkaline leaching process have high viscosity, so that the filtration is difficult, the process also relates to the processes of washing a filter cake with acid, desliming and the like, and a large amount of salt is generated by acid-base neutralization, so that the process still has the defects of high energy consumption, high cost and the like, and is difficult to popularize and apply in industrial production; for the roasting-alkaline leaching process, the defects of high production cost, flow plants, difficulty in industrial popularization and application and the like still exist, and particularly, a large amount of sodium hydroxide or potassium hydroxide is adopted as alkali, so that the generated soluble silicate solution has high viscosity and is difficult to pass, and industrial tests are difficult to develop; for the physical separation process, the method is a method for gradually improving the grade of the iron ore concentrate and has the defect of long time consumption; for the roasting-magnetic separation process, the method can effectively reduce the impurity content in the vanadium-titanium magnetite concentrate, and ore blending is not needed, but the problems of high roasting energy consumption, long flow, environmental pollution and the like exist, and industrial production is difficult to further develop.
In conclusion, although a great deal of research is carried out on the impurity removal method of the vanadium-titanium magnetite concentrate, the problems of high energy consumption, high cost, environmental friendliness and the like still exist. Therefore, the method for reducing the vanadium-titanium content from the vanadium-titanium magnetite concentrate with low cost, high efficiency and environmental friendliness is developed, and has important significance for the clean and efficient preparation of the vanadium-titanium magnetite concentrate resource.
Disclosure of Invention
The invention provides a method for selectively reducing the content of vanadium and titanium in vanadium-titanium magnetite concentrate by an ammonium-ammonia oxidation leaching system, which can effectively solve the problems.
The embodiment of the invention is realized by the following technical scheme:
a method for selectively reducing the content of vanadium and titanium in vanadium-titanium magnetite concentrate by an ammonium-ammonia oxidation leaching system comprises the following steps:
s1, preparing an ammonia-ammonium oxidation system composite leaching agent;
s2, grinding the minerals, mixing the ground minerals with the ammonium-ammonia system composite leaching agent obtained in the step S1, and carrying out selective alkaline hydrolysis leaching reaction to obtain a reacted mixture;
s3, performing magnetic separation on the mixture obtained in the step S2 to obtain vanadium-titanium magnetite concentrate and tailing pulp, performing solid-liquid separation on the tailing pulp to obtain filtrate, and returning the filtrate to the step S2 for recycling (when vanadium and titanium in the circulating liquid reach certain concentrations, vanadium and titanium are recovered).
The technical scheme of the embodiment of the invention at least has the following advantages and beneficial effects:
according to the method for selectively reducing the vanadium and titanium content in the vanadium-titanium magnetite concentrate by using the ammonium hydroxide oxidation leaching system, the minerals are treated by using the composite leaching agent of the ammonium hydroxide oxidation leaching system, so that V, Ti and other impurities in the minerals can be effectively transferred to a liquid phase, and iron is retained in a solid phase, so that the high-efficiency separation of the iron and V, Ti and other impurities is realized; and finally, separating the vanadium titano-magnetite from the gangue minerals by a magnetic separation mode by utilizing the magnetic difference between the vanadium titano-magnetite concentrate and the gangue minerals. The method has the advantages of simple operation, low requirement on raw materials, low operation cost and good treatment effect, can fully improve the iron content in the vanadium-titanium magnetite concentrate, and provides high-quality iron concentrate for blast furnace smelting.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The invention provides a method for selectively reducing the content of vanadium and titanium in vanadium-titanium magnetite concentrate by an ammonium-ammonia oxidation leaching system, which comprises the following steps:
s1, preparing an ammonium sulfate oxidation leaching system composite leaching agent;
s2, mixing the ground minerals (the granularity is less than 0.106mm) with the ammonium carbamate oxidation leaching system composite leaching agent obtained in the step S1 to perform selective alkaline hydrolysis leaching reaction to obtain a reacted mixture;
s3, performing magnetic separation on the mixture obtained in the step S2 to obtain vanadium-titanium magnetite concentrate and tailing pulp, performing solid-liquid separation on the tailing pulp to obtain filtrate, and returning the filtrate to the step S2 for recycling (when vanadium and titanium in the circulating liquid reach certain concentrations, vanadium and titanium are recovered). When the concentration of the related ammonium-ammonia-oxidant in the circulating leaching liquid is insufficient, the concentrations of the ammonium salt, the ammonia water and the oxidant are kept by additionally adding the ammonium salt, the ammonia water and the oxidant, so that the required concentration of the leaching agent is achieved.
Further, in step S1, the raw materials of the ammonium hydroxide oxidation leaching system composite leaching agent include ammonia water, ammonium salt and an oxidizing agent.
Further, the ammonium salt is an organic salt composed of organic acid radical ions and ammonium radical ions or an inorganic salt composed of inorganic acid radical ions and ammonium radical ions.
Further, the oxidant is permanganate, chlorate, hypochlorite, persulfate, oxygen, ozone, hydrogen peroxide and the like
Further, the organic acid radical ion is a carboxylate ion or an organic phosphonate ion.
Specifically, the organic acid ion-providing substance includes: organic acids such as formic acid, acetic acid, adipic acid, oxalic acid, succinic acid, malic acid, maleic acid, fumaric acid, citric acid, tartaric acid, phthalic acid, glycine, iminooxalic acid, gallic acid, gluconic acid, polyacrylic acid, polymethacrylic acid, and trifluoroacetic acid, and salts thereof; preferably citric acid, tartaric acid, glycine, iminodiacetic acid, gallic acid, gluconic acid, polyacrylic acid, polymethacrylic acid, polyepoxysuccinic acid, polyaspartic acid, ammonium salts of organic carboxylic acids derivatives.
Further, the inorganic acid radical ions are nitrate ions, sulfate ions or phosphate ions.
Specifically, the substance that provides the inorganic acid ion includes: sulfuric acid, nitric acid, hydrochloric acid, phosphoric acid, carbonic acid.
Further, in step S1, the specific preparation method of the ammonium-ammonia system complex leaching agent is as follows:
according to the weight portion, 100 portions of clean water is taken as a reference, the clean water is heated to 30-40 ℃ and then is kept warm, 20-30 portions of ammonium salt are added into the clean water, the mixture is stirred until the ammonium salt is completely dissolved, then 50-60 portions of ammonia water and 0.5-10 portions of oxidant are added, and the mixture is naturally cooled after being stirred.
Further, the concentration of the aqueous ammonia is 0.5 to 35 wt%.
Further, in the selective alkaline hydrolysis leaching reaction of the step S2, the reaction temperature is 20-200 ℃, and the reaction time is 0.5-720 h.
Further, in step S2, the weight ratio of the minerals to the ammine system composite leaching agent is 1: (1-10).
Further, the weight ratio of the minerals to the ammonium-ammonia system composite leaching agent is 1: (1-5).
Further, in step S2, the TFe content of the mineral is 45-56%, TiO29-20% of SiO22-10% of Al2O3The content is 2-10%.
Example 1
A method for selectively reducing the content of vanadium and titanium in vanadium-titanium magnetite concentrate by an ammonium-ammonia oxidation leaching system comprises the following steps:
s1, preparing an ammonium-ammonia system composite leaching agent;
taking 100 parts by weight of clear water as a reference, firstly heating the clear water to 35 ℃, preserving heat, then adding 25 parts by weight of ammonium polymethacrylate into the clear water, stirring until the ammonium polymethacrylate is completely dissolved, then adding 55 parts by weight of 30 wt% ammonia water and 5 parts by weight of 20 wt% hydrogen peroxide, and naturally cooling after stirring.
S2, grinding the minerals, mixing the ground minerals with the ammonium-ammonia system composite leaching agent obtained in the step S1 according to the weight ratio of 1:5, and carrying out selective alkaline hydrolysis leaching reaction at the reaction temperature of 80 ℃ for 5.5 hours to obtain a reacted mixture;
the TFe content of the mineral is 50%, TiO2Content of 15% SiO26% of Al2O3The content is 6%.
S3, performing magnetic separation on the mixture obtained in the step S2 to obtain vanadium-titanium magnetite concentrate A1 and tailing pulp, performing solid-liquid separation on the tailing pulp to obtain filtrate, and returning the filtrate to the step S2 for recycling.
Example 2
A method for selectively reducing the content of vanadium and titanium in vanadium-titanium magnetite concentrate by an ammonium-ammonia oxidation leaching system comprises the following steps:
s1, preparing an ammonium-ammonia system composite leaching agent;
taking 100 parts by weight of clear water as a reference, firstly heating the clear water to 30 ℃, preserving heat, then adding 20 parts by weight of ammonium polymethacrylate into the clear water, stirring until the ammonium polymethacrylate is completely dissolved, then adding 50 parts by weight of ammonia water with the concentration of 25 wt% and 0.5 part by weight of hydrogen peroxide with the concentration of 20 wt%, stirring, and naturally cooling.
S2, grinding the minerals, mixing the ground minerals with the ammonium-ammonia system composite leaching agent obtained in the step S1 according to the weight ratio of 1:1, and carrying out selective alkaline hydrolysis leaching reaction at the reaction temperature of 70 ℃ for 5 hours to obtain a reacted mixture;
the TFe content of the mineral is 45%, TiO2Content of 9% SiO2Content of 2% Al2O3The content is 2%.
S3, performing magnetic separation on the mixture obtained in the step S2 to obtain vanadium-titanium magnetite concentrate A2 and tailing pulp, performing solid-liquid separation on the tailing pulp to obtain filtrate, and returning the filtrate to the step S2 for recycling.
Example 3
A method for selectively reducing the content of vanadium and titanium in vanadium-titanium magnetite concentrate by an ammonium-ammonia oxidation leaching system comprises the following steps:
s1, preparing an ammonium-ammonia system composite leaching agent;
taking 100 parts by weight of clear water as a reference, firstly heating the clear water to 40 ℃, preserving heat, then adding 30 parts by weight of ammonium polymethacrylate into the clear water, stirring until the ammonium polymethacrylate is completely dissolved, then adding 60 parts by weight of 35 wt% ammonia water and 10 parts by weight of 20 wt% hydrogen peroxide, and naturally cooling after stirring.
S2, grinding the minerals, mixing the ground minerals with the ammonium-ammonia system composite leaching agent obtained in the step S1 according to the weight ratio of 1:10, and carrying out selective alkaline hydrolysis leaching reaction at the reaction temperature of 90 ℃ for 6 hours to obtain a reacted mixture;
the TFe content of the mineral is 56%, TiO2Content of 20% SiO210% of Al2O3The content is 10%.
S3, performing magnetic separation on the mixture obtained in the step S2 to obtain vanadium-titanium magnetite concentrate A3 and tailing pulp, performing solid-liquid separation on the tailing pulp to obtain filtrate, and returning the filtrate to the step S2 for recycling.
Comparative example 1
The remaining characteristics were the same as in example 1, except that in step S1, no ammonia was added, and the vanadium-titanium magnetite concentrate obtained finally was designated as D1.
Comparative example 2
The remaining characteristics were the same as in example 1, except that ammonium polymethacrylate was not added in step S1, and the final vanadium-titanium magnetite concentrate was designated as D2.
Comparative example 3
The remaining characteristics were the same as in example 1, except that in step S2, the weight ratio of the mineral to the ammonium-ammonium complex leaching agent obtained in step S1 was 1:0.5, and the vanadium-titanium magnetite concentrate obtained finally was designated as D3.
Comparative example 4
The remaining characteristics were the same as in example 1, except that, in step S2, the reaction temperature was 30 ℃ and the final vanadium-titanium magnetite concentrate was designated D4.
Comparative example 5
The remaining characteristics were the same as in example 1, except that in step S2, the reaction time was 2 hours, and the final vanadium-titanium magnetite concentrate was designated as D5.
Comparative example 6
The remaining characteristics are the same as those of example 1, except that hydrogen peroxide is not added in step S1, and the final vanadium-titanium magnetite concentrate is recorded as D6.
Examples of the experiments
The contents of iron, titanium and vanadium in the vanadium-titanium magnetite concentrates obtained in the above examples and comparative examples were measured, and the results are shown in table 1.
TABLE 1 iron, vanadium, titanium content of vanadium-titanium magnetite concentrate
As can be seen from the data in Table 1, after the mineral is treated by the method provided by the invention, the iron grade of the obtained vanadium-titanium magnetite concentrate can reach more than 68%, and the contents of titanium and vanadium are far lower than 3%. The vanadium-titanium magnetite concentrates D1-D6 prepared according to the respective proportions have the iron grade below 60 percent and have higher titanium and vanadium contents.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for selectively reducing the content of vanadium and titanium in vanadium-titanium magnetite concentrate by an ammonium-ammonia oxidation leaching system is characterized by comprising the following steps:
s1, preparing an ammonia-ammonium oxidation system composite leaching agent;
s2, grinding the minerals, mixing the ground minerals with the ammonium ammonia oxidation system composite leaching agent obtained in the step S1, and carrying out selective alkaline hydrolysis leaching reaction to obtain a reacted mixture;
s3, performing magnetic separation on the mixture obtained in the step S2 to obtain vanadium-titanium magnetite concentrate and tailing pulp, performing solid-liquid separation on the tailing pulp to obtain filtrate, and returning the filtrate to the step S2 for recycling.
2. The method for selectively reducing the vanadium-titanium content in vanadium-titanium magnetite concentrate by using the ammonium hydroxide oxidation leaching system according to claim 1, wherein in step S1, raw materials of the ammonium hydroxide oxidation system composite leaching agent comprise ammonia water, ammonium salt and an oxidant;
wherein, the oxidant comprises one or more of hydrogen peroxide, permanganate, persulfate, oxygen, ozone, sodium chlorate, sodium hypochlorite and sodium perchlorate.
3. The method for selectively reducing the vanadium-titanium content in the vanadium-titanium magnetite concentrate by using the ammonia-ammonium oxidation leaching system according to claim 2, wherein the ammonium salt is an organic salt consisting of organic acid radical ions and ammonium radical ions or an inorganic salt consisting of inorganic acid radical ions and ammonium radical ions.
4. The method for selectively reducing the vanadium-titanium content in vanadium-titanium magnetite concentrate by using the ammonium hydroxide leaching system according to claim 3, wherein the organic acid radical ion is a carboxylate ion or a phosphonate ion, and the inorganic acid radical ion is a nitrate ion, a sulfate ion or a phosphate ion.
5. The method for selectively reducing the vanadium-titanium content in vanadium-titanium magnetite concentrate by using the ammonium hydroxide oxidation leaching system according to claim 2, wherein in the step S1, the specific preparation method of the ammonium hydroxide oxidation system composite leaching agent is as follows:
according to the weight portion, 100 portions of clean water is taken as a reference, the clean water is heated to 30-40 ℃ and then is kept warm, 20-30 portions of ammonium salt are added into the clean water, the mixture is stirred until the ammonium salt is completely dissolved, then 50-60 portions of ammonia water and 0.5-10 portions of oxidant are added, and the mixture is naturally cooled after being stirred.
6. The method for selectively reducing the vanadium-titanium content in vanadium-titanium magnetite concentrate by using the ammonia-ammonium oxidation leaching system according to claim 5, wherein the concentration of the ammonia water is 0.5-35 wt%.
7. The method for selectively reducing the vanadium-titanium content in the vanadium-titanium magnetite concentrate by using the ammonium hydroxide oxidation leaching system according to claim 1, wherein in the selective alkaline hydrolysis leaching reaction of step S2, the reaction temperature is 20-200 ℃, and the reaction time is 0.5-720 h.
8. The method for selectively reducing the vanadium-titanium content in vanadium-titanium magnetite concentrate by using the ammonium hydroxide leaching system according to claim 1, wherein in step S2, the weight ratio of the mineral to the ammonium hydroxide leaching system composite leaching agent is 1: (1-10).
9. The method for selectively reducing the vanadium-titanium content in vanadium-titanium magnetite concentrate by using the ammonium hydroxide oxidation leaching system according to claim 8, wherein the weight ratio of the minerals to the ammonium hydroxide system composite leaching agent is 1: (1-5).
10. The method for selectively reducing the vanadium-titanium content in vanadium-titanium magnetite concentrate by using the ammonia ammonium oxidation leaching system according to claim 1, wherein the TFe content of the ore is 45-60% and TiO is selected in step S229-20% of SiO22-10% of Al2O3The content is 2-10%.
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