CN107572596B - Method for preparing high-purity iron oxide red from high-phosphorus oolitic hematite - Google Patents
Method for preparing high-purity iron oxide red from high-phosphorus oolitic hematite Download PDFInfo
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- CN107572596B CN107572596B CN201710824640.8A CN201710824640A CN107572596B CN 107572596 B CN107572596 B CN 107572596B CN 201710824640 A CN201710824640 A CN 201710824640A CN 107572596 B CN107572596 B CN 107572596B
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Abstract
The invention discloses a method for preparing high-purity iron oxide red from high-phosphorus oolitic hematite. Mixing high-phosphorus oolitic hematite and coal powder, roasting for 90-150min at the temperature of 1000-1100 ℃ to obtain mixed ore, grinding the obtained mixed ore until the ore with the particle size of-74 mu m accounts for 90%, carrying out magnetic separation under the magnetic field strength condition of 0.1-0.15T to obtain magnetic separation concentrate, mixing 17-20% of sulfuric acid with the obtained magnetic separation concentrate according to the volume-mass ratio of 9:1-11:1ml/g, and reacting for 25-35min at normal temperature under the condition that the stirring speed is 100-300r/min to obtain a solid-liquid mixture; adding ammonia water to adjust pH to 5-5.5, and filtering to obtain filtrate; adding an oxidant into the obtained filtrate for oxidation, adding ammonia water to precipitate under the condition of keeping the pH value at 4, filtering and washing; the obtained precipitate is roasted at the temperature of 750-850 ℃ for 40-60min to obtain the high-purity iron oxide red. The high-purity iron oxide red is prepared by taking the high-phosphorus oolitic hematite which is difficult to utilize as a raw material, so that waste is changed into valuable; the problem that the utilization is influenced due to the overhigh phosphorus content in the high-phosphorus oolitic hematite is solved; the problem of leaching of the high-phosphorus oolitic hematite is solved.
Description
Technical Field
The invention belongs to the technical field of comprehensive utilization of resources, and particularly relates to a method for preparing high-purity iron oxide red from high-phosphorus oolitic hematite.
Background
The high-phosphorus oolitic hematite reserves in China are rich and reach 37.2 hundred million tons. The iron ore mainly contains iron minerals such as hematite, and part of iron and silicon aluminum are combined to exist in the form of oolitic chlorite and other silicates. Hematite mainly exists in oolitic concentric ring belt structures, and the particle size of oolitic particles is generally 0.01-0.30 mm. Most hematite and oolitic green mud stone form a concentric ring structure, and oolitic stones are mainly quartz and hematite. Apatite is the most important phosphorite in the ore and is mainly irregularly embedded in gaps of other gangue minerals or in gaps of oolitic hematite particles, so that the apatite exists in the form of oolitic granule cores, and the apatite forms oolitic granules in the form of oolitic rings and forms a concentric ring structure with the hematite; the apatite in the first two parts has relatively thick granularity, and can be removed by a mechanical ore dressing method after proper grinding, and the apatite in the latter two forms has very thin granularity, generally less than 0.015mm, is difficult to be completely dissociated with hematite in the grinding process and is easy to enter iron ore concentrate.
Steels containing a large amount of phosphorus are susceptible to embrittlement when used at room temperature or below.
At present, the comprehensive utilization methods of the high-phosphorus oolitic hematite mainly comprise two methods: one is to obtain iron ore concentrate with low phosphorus content by using a treatment process with magnetic roasting-magnetic separation-dephosphorization as a core, and the other is to obtain reduced iron powder for electric furnace smelting by adding a dephosphorization agent to carry out dephosphorization treatment while carrying out direct reduction roasting-magnetic separation process. Although the iron ore concentrate with the phosphorus content of about 0.2 percent and the iron grade of about 60 percent can be obtained by adopting dephosphorization processes such as reverse flotation dephosphorization, acid leaching dephosphorization, ultrasonic acid leaching dephosphorization, microbial leaching and the like; firstly, the grade of the iron ore concentrate is not high, and secondly, the problem of dephosphorization is still faced in the subsequent treatment process. While the second treatment method can obtain reduced iron powder with a phosphorus content of about 0.08%, which is still high in phosphorus content when used in electric furnace smelting.
Due to the special oolitic structure of the high-phosphorus oolitic hematite, higher leaching rate cannot be obtained when single sulfuric acid, hydrochloric acid and nitric acid are used for leaching, and the iron leaching rate is less than 40%; increasing the mass fraction of acid can increase the leaching rate to 60%. Although the high-phosphorus oolitic hematite can be leached by mixing a plurality of strong acids, a higher leaching rate is obtained; however, mixed acid leaching causes equipment corrosion and a large amount of impurities enter the leachate, so that the equipment maintenance cost and the leachate impurity removal cost are increased. The direct acid leaching after the pre-enrichment of the raw ore has the problems of low iron recovery rate, adverse effect of oolitic structure on acid leaching and the like.
Disclosure of Invention
The invention aims to explore a new way for utilizing high-phosphorus oolitic hematite and provide a method for preparing high-purity iron oxide red from the high-phosphorus oolitic hematite, aiming at the problems of the existing comprehensive utilization method of the high-phosphorus oolitic hematite resource.
The invention provides a method for preparing iron oxide red by utilizing high-phosphorus oolitic hematite, which changes iron phases by utilizing a direct reduction technology at a lower temperature (about 1050 ℃). At the temperature, collophanite is partially decomposed, a few phosphorus enters an iron phase to form Fe/P alloy, and other phosphorus oxides are relatively stable; there is no need to pay attention to the transfer of phosphorus during leaching.
The invention provides a method for preparing iron oxide red by utilizing high-phosphorus oolitic hematite, which improves the leaching rate of iron. Firstly, direct reduction treatment changes iron phase, so that the magnetic concentrate has good leaching rate when being leached by single sulfuric acid, and a large amount of impurities enter leaching slag; meanwhile, most oolitic structures are damaged, and cracks appear between iron mineral particles and gangue minerals, so that the leaching efficiency is improved. The iron leaching rate of the treated magnetic concentrate can reach more than 90 percent.
In order to realize the purpose of the invention, the technical solution of the invention is as follows: mixing high-phosphorus oolitic hematite and coal powder, roasting at the temperature of 1000-1100 ℃ for 90-150min to obtain mixed ore, grinding the obtained mixed ore until the ore accounts for 90-74 mu m, magnetically separating under the magnetic field strength condition of 0.1-0.15T to obtain magnetic concentrate, mixing 17-20% of sulfuric acid and the obtained magnetic concentrate according to the volume-mass ratio of 9:1-11:1ml/g, and reacting at normal temperature for 25-35min under the condition of stirring speed of 100-300r/min to obtain a solid-liquid mixture; adding ammonia water to adjust pH to 5-5.5, and filtering to obtain filtrate; adding an oxidant into the obtained filtrate for oxidation, adding ammonia water to precipitate under the condition of keeping the pH value at 4, filtering and washing; the obtained precipitate is roasted at the temperature of 750-850 ℃ for 40-60min to obtain the high-purity iron oxide red.
Specifically, the mixing ratio of the phosphorus oolitic hematite and the coal powder is as follows: 100 parts of high-phosphorus oolitic hematite and 30-40 parts of coal powder.
Preferably, the roasting temperature of the mixture of the high-phosphorus oolitic hematite and the coal powder is 1050 ℃, and the roasting time is 120 min.
Preferably, the mass concentration of the sulfuric acid is 18%; the volume mass ratio of the sulfuric acid to the magnetic concentrate is 10:1 ml/g.
Preferably, the mixed normal-temperature reaction time of the sulfuric acid and the magnetic concentrate is 30 min.
Preferably, the filtered precipitate is oxidized at a calcination temperature of 800 ℃ for 60 min.
Specifically, the oxidizing agent is hydrogen peroxide.
The invention has the beneficial effects that: the high-purity iron oxide red is prepared by taking the high-phosphorus oolitic hematite which is difficult to utilize as a raw material, so that waste is changed into valuable; the problem that the utilization is influenced due to the overhigh phosphorus content in the high-phosphorus oolitic hematite is solved; the problem of leaching of the high-phosphorus oolitic hematite is solved.
Drawings
FIG. 1 is a flow chart of the production process of the present invention.
Detailed Description
The invention is further described below with reference to the accompanying drawings.
Example 1, comprising the steps of: mixing high-phosphorus oolitic hematite with a total iron grade of 42.3% and coal powder with fixed carbon of 47.6% according to the mass ratio of Fe to C of 2.39:1, namely, the mass ratio of the high-phosphorus oolitic hematite to the coal powder is 100: 37; placing in a laboratory electric furnace, roasting at 1050 deg.C for 120min, taking out, and water cooling; directly grinding the roasted ore until the particle size of-74 mu m accounts for 90%, and carrying out magnetic separation by using a cylindrical magnetic separator under the condition that the field intensity is 0.12T to obtain magnetic separation concentrate with the iron grade of 61.25%, wherein the main component is simple substance iron; mixing 18% sulfuric acid according to the ratio of the sulfuric acid solution to the magnetic concentrate of 10:1ml/g for reaction for 25 min; adding ammonia water into the mixed solution to adjust the pH value to 5, and filtering to obtain filtrate; adding an oxidizing agent to oxidize hydrogen peroxide while maintaining the pH at 4, filtering the precipitate and washing; placing the precipitate in an electric furnace in a laboratory, and roasting at 750 deg.C for 50min to obtain final product, Fe2O3The content reaches 98.23 percent.
Example 2, comprising the steps of: mixing high-phosphorus oolitic hematite with a total iron grade of 42.3% and coal powder with fixed carbon of 47.6% according to the mass ratio of Fe to C of 2.7:1, namely, the mass ratio of the high-phosphorus oolitic hematite to the coal powder is 100: 33; placing in a laboratory electric furnace, roasting at 1000 deg.C for 150min, taking out, and water cooling; directly grinding the roasted ore until the ore with the particle size of-74 mu m accounts for 90%, and carrying out magnetic separation by using a cylindrical magnetic separator under the condition that the field intensity is 0.12T to obtain magnetic concentrate with the iron grade of 60.85%; mixing 18% sulfuric acid according to the ratio of the sulfuric acid solution to the magnetic concentrate of 11:1ml/g for reaction for 35 min; adding ammonia water into the mixed solution to adjust the pH value to 5.5, and filtering to obtain filtrate; adding an oxidant for oxidation while maintaining the pH at 4, filtering the precipitate and washing; placing the precipitate in an electric furnace in a laboratory, and roasting at 800 deg.C for 60min to obtain final product, Fe2O3The content reaches 99.23 percent.
Example 3, comprising the steps of: mixing high-phosphorus oolitic hematite with a full-iron grade of 40.3% and coal powder with fixed carbon of 49.6% according to the mass ratio of Fe to C of 2.6:1, namely, the mass ratio of the high-phosphorus oolitic hematite to the coal powder is 100: 31; placing in a laboratory electric furnace at 1050 deg.CRoasting for 120min, taking out and cooling with water; directly grinding the roasted ore until the ore with the particle size of-74 mu m accounts for 90%, and carrying out magnetic separation by using a cylindrical magnetic separator under the condition that the field intensity is 0.10T to obtain magnetic separation concentrate with the iron grade of 61.85%; mixing 20% sulfuric acid according to the ratio of the sulfuric acid solution to the magnetic concentrate of 11:1ml/g for reaction for 30 min; adding ammonia water into the mixed solution to adjust the pH value to 5.5, and filtering to obtain filtrate; adding an oxidant for oxidation while maintaining the pH at 4, filtering the precipitate and washing; placing the precipitate in an electric furnace in a laboratory, and roasting at 850 deg.C for 60min to obtain final product, Fe2O3The content reaches 99.36 percent.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (7)
1. A method for preparing high-purity iron oxide red from high-phosphorus oolitic hematite comprises the steps of mixing the high-phosphorus oolitic hematite with coal powder, roasting for 90-150min at the temperature of 1000-1100 ℃ to obtain mixed ore, grinding the obtained mixed ore until the mixed ore accounts for 90% with a particle size of-74 microns, and performing magnetic separation under the condition of a magnetic field strength of 0.1-0.15T to obtain magnetic separation concentrate, and is characterized by further comprising the following steps:
mixing 17-20% of sulfuric acid with mass concentration with the obtained magnetic concentrate according to the volume-mass ratio of 9:1-11:1ml/g, and reacting at normal temperature for 25-35min under the condition that the stirring speed is 100-; adding ammonia water to adjust pH to 5-5.5, and filtering to obtain filtrate; adding an oxidant into the obtained filtrate for oxidation, adding ammonia water to precipitate under the condition of keeping the pH value at 4, filtering and washing; the obtained precipitate is roasted at the temperature of 750-850 ℃ for 40-60min to obtain the high-purity iron oxide red.
2. The method for preparing high-purity iron oxide red from the high-phosphorus oolitic hematite according to claim 1, wherein the mixing mass ratio of the high-phosphorus oolitic hematite to the coal powder is as follows: 100 parts of high-phosphorus oolitic hematite and 30-40 parts of coal powder.
3. The method for preparing high-purity iron oxide red from the high-phosphorus oolitic hematite according to claim 1, wherein the roasting temperature for mixing the high-phosphorus oolitic hematite and the coal powder is 1050 ℃, and the roasting time is 120 min.
4. The method for preparing high-purity iron oxide red from the high-phosphorus oolitic hematite according to claim 1, wherein the mass concentration of sulfuric acid is 18%; the volume mass ratio of the sulfuric acid to the magnetic concentrate is 10:1 ml/g.
5. The method for preparing high-purity iron oxide red from high-phosphorus oolitic hematite according to claim 1, wherein the reaction time of the sulfuric acid and the magnetic concentrate at normal temperature is 30 min.
6. The method for preparing high-purity iron oxide red from high-phosphorus oolitic hematite according to claim 1, wherein the oxidant is hydrogen peroxide.
7. The method for preparing high-purity iron oxide red from the high-phosphorus oolitic hematite according to claim 1, wherein the filtered precipitate is oxidized, and the roasting temperature is 800 ℃ and the roasting time is 60 min.
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Application publication date: 20180112 Assignee: Wuhan University of science and Technology Business Incubator Co.,Ltd. Assignor: WUHAN University OF SCIENCE AND TECHNOLOGY Contract record no.: X2020420000003 Denomination of invention: A method for preparing high purity iron oxide red from high phosphorus oolitic hematite Granted publication date: 20200218 License type: Common License Record date: 20201021 |
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