CN110863103B - Steel slag treatment method for improving recovery rate of iron in steel slag - Google Patents
Steel slag treatment method for improving recovery rate of iron in steel slag Download PDFInfo
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- CN110863103B CN110863103B CN201911144387.7A CN201911144387A CN110863103B CN 110863103 B CN110863103 B CN 110863103B CN 201911144387 A CN201911144387 A CN 201911144387A CN 110863103 B CN110863103 B CN 110863103B
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- steel slag
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/005—Preliminary treatment of scrap
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21B—MANUFACTURE OF IRON OR STEEL
- C21B3/00—General features in the manufacture of pig-iron
- C21B3/04—Recovery of by-products, e.g. slag
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
Abstract
The invention discloses a steel slag processing method for improving the recovery rate of iron in steel slag, which can effectively improve the porosity in the steel slag and increase the inner diameter of pores by pretreating the steel slag before solid-phase modification, introducing nitrogen into the original steel slag in a molten state, cooling the steel slag, and then carrying out liquid nitrogen low-temperature crushing and grinding on the cooled steel slag, and simultaneously fully contacting oxygen in a high specific surface area state, so that oxygen in the air can enter the steel slag to fully react when the steel slag is modified in a solid phase, the cold steel slag is calcined in the air, iron oxide and magnesium oxide in the steel slag are promoted to be more fully converted into the strong-magnetism pleonaste, further improves the iron recovery rate of the treated steel slag during magnetic separation, and after the iron and magnesium impurities in the steel slag are converted into strong magnetic magnesium iron spinel, the grindability of the steel slag can reach a more ideal level, and the strength of the tailings used as cement can be improved to a great extent.
Description
Technical Field
The invention relates to a steel slag treatment method, in particular to a steel slag treatment method for improving the recovery rate of iron in steel slag.
Background
The steel slag is a byproduct generated in the steel-making process, and the discharge amount of the steel slag is huge, so that the steel slag is not effectively utilized for a long time. The steel slag piled up not only occupies limited land resource seriously and pollutes water and soil, but also is a huge resource waste. On one hand, the steel slag contains partial gelled minerals and can be used as partial raw materials of cement concrete; on the other hand, the steel slag also contains ferrous oxide with higher content and free calcium oxide and magnesium oxide with certain mass, and the ferrous oxide can not be directly separated by magnetic separation and is easy to cause the reduction of the strength of the steel slag cement.
The iron is generally FeO and Fe in the steel slag2O3And elementary substance Fe which exists in a form of elementary substance and occupies a considerable proportion (10-25 percent by mass), the elementary substance Fe with larger particles can be separated by magnetic separation, and the FeO and Fe with weak magnetism2O3And a small part of simple substance Fe still exists in the tailings after magnetic separation. Directly abandoning the iron in the tailings is a great waste of resources, and the existence of iron oxide can cause the easy grindability of the tailings to be poor, so that the tailings serving as raw materials of cement, ceramic and the like are limited in the application process. Therefore, the recovery of iron in the tailings has long-term practical significance on the aspects of recycling the steel slag, saving enterprise resources, reducing environmental pollution, increasing economic benefits of enterprises and the like.
Based on the research foundation of an oxidation method, the solid-phase modification process of converter steel slag is provided at present, iron oxide and magnesium oxide in the steel slag are converted into strong magnetic hercynite by calcining cold steel slag in air, the strong magnetic hercynite can be separated by magnetic separation, and gases generating greenhouse effect cannot be discharged in the whole process of the process that the steel slag is subjected to solid-phase modification to form the hercynite. However, in the solid-phase modification process of the converter steel slag, the converter steel slag is difficult to be in sufficient contact with oxygen in the air, so that the conversion of the steel slag iron oxide and the magnesium oxide to the strong-magnetic magnesium-iron spinel is insufficient, and further, the iron recovery rate in the steel slag is low.
Disclosure of Invention
The solid-phase modification process of converter steel slag adopts a mode of calcining the steel slag in an oxidizing atmosphere to finish the conversion of nonmagnetic ferrous oxide and magnesium oxide in raw ore of the steel slag to magnetic iron-rich phase aggregation, and enough holes must exist on the surface of the steel slag to ensure that oxygen molecules can enter the deep part of a product layer to be combined with the residual reactants. In the existing solid-phase modification process of converter steel slag, because the converter steel slag is difficult to fully contact with oxygen in the air, the conversion of steel slag iron oxide and magnesium oxide to strong-magnetism magnesium iron spinel is insufficient, and the iron recovery rate in the steel slag is low.
The invention aims to provide a steel slag treatment method for improving the recovery rate of iron in steel slag, which is characterized in that the steel slag is pretreated before solid-phase modification, nitrogen is introduced into original steel slag in a molten state, cooling is carried out simultaneously, liquid nitrogen low-temperature crushing and grinding are carried out after cooling, so that the porosity, the pore size and the specific surface area of the steel slag are improved, oxygen in air can be fully contacted with the interior of the steel slag when the steel slag is subjected to solid-phase modification, the transformation of strong-magnetic hercynite is more sufficient, and the recovery rate of iron in the steel slag is further improved.
The purpose of the invention is realized by the following technical scheme:
a steel slag treatment method for improving the recovery rate of iron in steel slag is characterized by comprising the following steps: firstly, pre-melting raw steel slag, heating the raw steel slag under the protection of inert gas to completely melt the raw steel slag, then introducing nitrogen into the molten raw steel slag, and cooling the molten raw steel slag to room temperature while introducing the nitrogen; secondly, carrying out liquid nitrogen low-temperature crushing treatment on the pre-melted steel slag obtained in the first step, crushing and further grinding until the particle size of the steel slag is less than 0.1 mm; and thirdly, introducing air into the steel slag which is crushed and ground at low temperature by using the liquid nitrogen in the second step at high temperature for calcination so as to carry out solid-phase modification treatment.
A steel slag treatment method for improving the recovery rate of iron in steel slag is characterized by comprising the following steps: the speed of introducing nitrogen into the molten raw steel slag in the first step of treatment is 4-6L/min.
A steel slag treatment method for improving the recovery rate of iron in steel slag is characterized by comprising the following steps: the inert gas in the first step of treatment is argon.
A steel slag treatment method for improving the recovery rate of iron in steel slag is characterized by comprising the following steps: in the first step, the raw steel slag is heated to 1500 ℃ so as to be completely melted.
A steel slag treatment method for improving the recovery rate of iron in steel slag is characterized by comprising the following steps: and in the first step of treatment, the molten raw steel slag is cooled to room temperature at a cooling speed of 10 ℃/min while introducing nitrogen.
A steel slag treatment method for improving the recovery rate of iron in steel slag is characterized by comprising the following steps: and the third step of solid-phase modification treatment is to fill the steel slag obtained by crushing and grinding the liquid nitrogen at low temperature in the second step in an alumina crucible in a loose manner, place the steel slag in a high-temperature box type muffle furnace, pre-introduce nitrogen into the muffle furnace to ensure that no air exists in the furnace, set the heating rate, switch the nitrogen to air when the set temperature is reached, monitor and adjust the air introduction rate, and switch the air to nitrogen again after preserving the heat for a certain time and rapidly cool the air to room temperature.
A steel slag treatment method for improving the recovery rate of iron in steel slag is characterized by comprising the following steps: in the third step of treatment, the heating rate is 10 ℃/min.
A steel slag treatment method for improving the recovery rate of iron in steel slag is characterized by comprising the following steps: the set temperature in the third step of the treatment was 1100 ℃.
A steel slag treatment method for improving the recovery rate of iron in steel slag is characterized by comprising the following steps: in the third step, the air feed rate was monitored by an LZB glass rotameter.
A steel slag treatment method for improving the recovery rate of iron in steel slag is characterized by comprising the following steps: in the third step of treatment, the air introduction rate is 7.5L/min.
The invention has the following advantages:
the steel slag is subjected to the pretreatment steps of ventilation pre-melting treatment and liquid nitrogen body temperature crushing and grinding treatment and then solid-phase modification, so that the porosity in the steel slag can be effectively improved, the inner diameter of pores is increased, and the steel slag is fully contacted with oxygen in a high specific surface area state, so that the oxygen in the air can enter the steel slag to fully react when the steel slag is subjected to solid-phase modification, the cold-state steel slag is calcined in the air, iron oxide and magnesium oxide in the steel slag are promoted to be more fully converted into strong-magnetism pleonaste, the iron recovery rate of the treated steel slag is improved when the steel slag is subjected to magnetic separation, the grindability of the steel slag can reach a more ideal level after iron and magnesium impurities in the steel slag are converted into the strong-magnetism pleonaste, and the strength of the steel slag can be greatly improved when the steel slag is used as cement,
drawings
FIG. 1 is a microstructure morphology of steel slag after treatment in example 2;
FIG. 2 shows the microstructure of the steel slag treated in example 4.
In the figure: the black dot at the circle is one of the plurality of pores.
Detailed Description
Example 1
Firstly, pre-melting raw steel slag, loading 50g of raw steel slag loose into an alumina crucible with the volume of 100mL, placing the alumina crucible into a high-temperature box type muffle furnace, measuring the temperature by an Rh/Pt standard thermocouple, and controlling the temperature in the furnace by a programmable regulator with the precision of +/-3 ℃. Heating to 1500 ℃ under the protection of argon to completely melt the raw steel slag, then introducing nitrogen into the molten raw steel slag at a speed of 4L/min, and cooling the molten raw steel slag to room temperature at a cooling speed of 10 ℃/min while introducing the nitrogen.
And secondly, carrying out liquid nitrogen low-temperature crushing treatment on the pre-melted steel slag obtained in the first step, crushing and further grinding until the particle size of the steel slag is less than 0.1 mm.
And thirdly, loosely loading the steel slag which is subjected to low-temperature crushing and grinding by using the liquid nitrogen in the second step into an alumina crucible, placing the steel slag into a high-temperature box type muffle furnace, introducing nitrogen into the muffle furnace in advance to ensure that no air exists in the furnace, setting the heating rate to be 10 ℃/min, switching the nitrogen into air when the temperature reaches 1100 ℃, monitoring the air introduction rate by using an LZB glass rotameter, adjusting the air introduction rate to be 7.5L/min, preserving the temperature for 30min, switching the air into nitrogen again, and quickly cooling the nitrogen to the room temperature.
Example 2
Firstly, pre-melting raw steel slag, loading 50g of raw steel slag loose into an alumina crucible with the volume of 100mL, placing the alumina crucible into a high-temperature box type muffle furnace, measuring the temperature by an Rh/Pt standard thermocouple, and controlling the temperature in the furnace by a programmable regulator with the precision of +/-3 ℃. Heating to 1500 ℃ under the protection of argon to completely melt the raw steel slag, then introducing nitrogen into the molten raw steel slag at a speed of 5L/min, and cooling the molten raw steel slag to room temperature at a cooling speed of 10 ℃/min while introducing the nitrogen.
And secondly, carrying out liquid nitrogen low-temperature crushing treatment on the pre-melted steel slag obtained in the first step, crushing and further grinding until the particle size of the steel slag is less than 0.1 mm.
And thirdly, loosely loading the steel slag which is subjected to low-temperature crushing and grinding by using the liquid nitrogen in the second step into an alumina crucible, placing the steel slag into a high-temperature box type muffle furnace, introducing nitrogen into the muffle furnace in advance to ensure that no air exists in the furnace, setting the heating rate to be 10 ℃/min, switching the nitrogen into air when the temperature reaches 1100 ℃, monitoring the air introduction rate by using an LZB glass rotameter, adjusting the air introduction rate to be 7.5L/min, preserving the temperature for 30min, switching the air into nitrogen again, and quickly cooling the nitrogen to the room temperature.
Example 3
Firstly, pre-melting raw steel slag, loading 50g of raw steel slag loose into an alumina crucible with the volume of 100mL, placing the alumina crucible into a high-temperature box type muffle furnace, measuring the temperature by an Rh/Pt standard thermocouple, and controlling the temperature in the furnace by a programmable regulator with the precision of +/-3 ℃. Heating to 1500 ℃ under the protection of argon to completely melt the raw steel slag, then introducing nitrogen into the molten raw steel slag at a speed of 6L/min, and cooling the molten raw steel slag to room temperature at a cooling speed of 10 ℃/min while introducing the nitrogen.
And secondly, carrying out liquid nitrogen low-temperature crushing treatment on the pre-melted steel slag obtained in the first step, crushing and further grinding until the particle size of the steel slag is less than 0.1 mm.
And thirdly, loosely loading the steel slag which is subjected to low-temperature crushing and grinding by using the liquid nitrogen in the second step into an alumina crucible, placing the steel slag into a high-temperature box type muffle furnace, introducing nitrogen into the muffle furnace in advance to ensure that no air exists in the furnace, setting the heating rate to be 10 ℃/min, switching the nitrogen into air when the temperature reaches 1100 ℃, monitoring the air introduction rate by using an LZB glass rotameter, adjusting the air introduction rate to be 7.5L/min, preserving the temperature for 30min, switching the air into nitrogen again, and quickly cooling the nitrogen to the room temperature.
Example 4
Weighing 50g of raw steel slag, loosely loading the raw steel slag in an alumina crucible, placing the alumina crucible in a high-temperature box type muffle furnace, introducing nitrogen in the muffle furnace in advance to ensure that no air exists in the furnace, setting the heating rate to be 10 ℃/min, switching the nitrogen into air when the temperature reaches 1100 ℃, monitoring the air introduction rate through an LZB glass rotameter, adjusting the air introduction rate to be 7.5L/min, preserving the heat for 30min, switching the air into nitrogen again, and quickly cooling to the room temperature.
The original steel slag and the solid-phase modified steel slag are respectively subjected to wet magnetic separation, and the wet magnetic separation effect can be evaluated by the magnetic separation recovery rate when the magnetic induction intensity is 0.1T. The recovery b (%) represents the mass ratio of Fe contained in the concentrate to Fe contained in the raw ore.
And (3) recovery rate: b ═ ((Qx × β)/(q. × α)) × 100%
Wherein: and Q. Representing the raw ore mass (t); qx represents the concentrate quality (t); α represents raw ore grade (%); beta represents the concentrate grade (%).
| Sample (I) | Recovery rate b |
| Example 1 | 71.2％ |
| Example 2 | 75.3％ |
| Example 3 | 72.5％ |
| Example 4 | 62.6％ |
As can be seen from the microstructure morphology of the steel slag shown in fig. 1 and 2, the steel slag after the pretreatment before the solid-phase modification is cooled while introducing nitrogen gas into the original steel slag in a molten state, and then is subjected to liquid nitrogen low-temperature pulverization and grinding, and the size and the number of pores of the steel slag after the treatment are far higher than those of the steel slag directly subjected to the solid-phase modification without the pretreatment. From the perspective of magnetic separation recovery rate, the recovery rate of iron in the pretreated steel slag is obviously higher than that of the steel slag without pretreatment, and from another perspective, the steel slag with improved porosity and increased pore size after pretreatment can form strong magnetic hercynite more fully, so that the recovery rate of iron in the steel slag is improved.
The foregoing is illustrative of the preferred embodiments of this invention, and it is to be understood that the invention is not limited to the precise form disclosed herein and that various other combinations, modifications, and environments may be resorted to, falling within the scope of the concept as disclosed herein, either as described above or as apparent to those skilled in the relevant art. And that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (9)
1. A steel slag treatment method for improving the recovery rate of iron in steel slag is characterized by comprising the following steps: firstly, pre-melting raw steel slag, heating the raw steel slag under the protection of inert gas to completely melt the raw steel slag, then introducing nitrogen into the molten raw steel slag, and cooling the molten raw steel slag to room temperature while introducing the nitrogen; secondly, carrying out liquid nitrogen low-temperature crushing treatment on the pre-melted steel slag obtained in the first step, crushing and further grinding until the particle size of the steel slag is less than 0.1 mm; thirdly, introducing air into the steel slag which is crushed and ground at low temperature by using the liquid nitrogen in the second step at high temperature for calcination so as to carry out solid-phase modification treatment; and the third step of solid-phase modification treatment is to fill the steel slag obtained by crushing and grinding the liquid nitrogen at low temperature in the second step in an alumina crucible in a loose manner, place the steel slag in a high-temperature box type muffle furnace, pre-introduce nitrogen into the muffle furnace to ensure that no air exists in the furnace, set the heating rate, switch the nitrogen to air when the set temperature is reached, monitor and adjust the air introduction rate, and switch the air to nitrogen again after preserving the heat for a certain time and rapidly cool the air to room temperature.
2. A method for treating steel slag according to claim 1, characterized in that: the speed of introducing nitrogen into the molten raw steel slag in the first step of treatment is 4-6L/min.
3. A method for treating steel slag according to claim 2, characterized in that: the inert gas in the first step of treatment is argon.
4. A method for treating steel slag according to any one of claims 1 to 3, characterized in that: in the first step of treatment, the raw steel slag is heated to 1500 ℃ so as to be completely melted.
5. A method for treating steel slag according to any one of claims 1 to 3, characterized in that: and in the first step of treatment, the molten raw steel slag is cooled to room temperature at a cooling speed of 10 ℃/min while introducing nitrogen.
6. The steel slag treatment method according to claim 1, characterized in that: in the third step of treatment, the heating rate is 10 ℃/min.
7. The steel slag treatment method according to claim 1, characterized in that: the set temperature in the third step of the treatment was 1100 ℃.
8. The steel slag treatment method according to claim 1, characterized in that: in the third step, the air feed rate was monitored by an LZB glass rotameter.
9. The steel slag treatment method according to claim 1, characterized in that: in the third step of treatment, the air introduction rate is 7.5L/min.
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| CN113699287B (en) * | 2021-09-02 | 2022-07-08 | 南京华电节能环保股份有限公司 | Blast furnace slag dry processing device based on high-temperature slag waste heat recovery |
| CN114472464A (en) * | 2022-01-14 | 2022-05-13 | 江苏大学 | Method for efficiently recycling iron and phosphorus resources in phosphorus-containing steel slag |
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