CN114317954A - Method for cooperatively treating and utilizing stainless steel pickling sludge and blast furnace dust - Google Patents
Method for cooperatively treating and utilizing stainless steel pickling sludge and blast furnace dust Download PDFInfo
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Abstract
The invention discloses a method for cooperatively treating and utilizing stainless steel pickling sludge and blast furnace dust, which is characterized by comprising the following steps of (1) placing dried stainless steel pickling sludge and blast furnace dust in a stirring device according to the mass ratio of 10:2-5, uniformly mixing, transferring the mixed material to a disc pelletizer, pelletizing, and preparing into a granular material with the granularity of 5-15 mm; (2) placing the granular material and the blast furnace cloth bag dedusting ash in a furnace according to the mass ratio of 10:1-5, and drying at 100-200 ℃ for 10-120 min; carrying out medium-temperature reduction roasting at the temperature of 500-750 ℃ for 0-60min, carrying out high-temperature reduction roasting at the temperature of 1000-1400 ℃ for 10-30min, and collecting the solid particle product of the roasting smoke in the whole process; (3) and (3) screening after the roasted product is cooled to obtain the sulfur-containing metallized furnace charge with proper granularity, directly returning to a blast furnace for smelting, slagging and desulfurizing, and preparing the stainless steel molten iron.
Description
Technical Field
The invention relates to the field of metallurgy and environmental protection, in particular to the technical field of resource utilization of metallurgical dust and mud. .
Background
The stainless steel pickling sludge is a dangerous solid waste generated in the stainless steel pickling and passivating process, and accounts for 2.5-5% of the stainless steel yield. The stainless steel pickling sludge contains a large amount of valuable metal elements such as Cr, Fe, Ni and the like which are necessary for stainless steel smelting. At present, typical resource utilization technologies of stainless steel pickling sludge mainly comprise: preparing sintered ore, preparing pellet ore, direct reduction, preparing auxiliary materials for steelmaking, wet leaching, material preparation and the like. According to different pickling processes, pickling sludge generally contains high-concentration sulfur or chlorine elements, so that the problem of sulfur load or chlorine corrosion of a furnace charge is inevitably caused when the pickling sludge is directly returned to a production and recycling process. The direct reduction of the stainless steel pickling sludge can solve the problem of sulfur or chlorine in the raw materials, reduce valuable metal oxides, and prepare ferroalloy through magnetic separation or melting separation, so that the direct reduction method is a main development direction for resource utilization of the stainless steel pickling sludge in the future.
Patent CN201711218446.1 discloses a stainless steel pickling sludge treatment process, and the technical scheme disclosed in the patent application adopts a rotary kiln low-temperature hydrocarbon combined reduction composite treatment process to treat stainless steel pickling sludge, iron oxide scales and reduction coal according to the mass ratio of 50: 50: 10-20 of mixing and granulating, feeding the granular materials into a rotary kiln for reduction roasting, spraying high-volatility granular coal accounting for 10-15% of the weight of the mixed raw materials and high-grade hematite accounting for 15-20% of the weight of the mixed raw materials into the kiln at the middle and later stages for combined reduction of carbon and hydrogen and carbon circulation oxygenation reduction, and carrying out dry magnetic separation on the roasted materials in a magnetic separator by using the magnetic field intensity to obtain a metalized product. The process is lengthy and complex to operate; meanwhile, the tail gas containing carbon, hydrogen, sulfur and oxygen is generated by the reduction of the hydrocarbon, the components are complex and difficult to process, and the environmental protection property needs to be evaluated.
Patent CN202010225343.3 discloses a method for returning stainless steel acid-washing sludge to a rotary kiln-submerged arc furnace process for utilization. The technical scheme disclosed in the patent application is that stainless steel pickling sludge is mixed with laterite-nickel ore and a reducing agent, sulfate of the stainless steel pickling sludge is reduced into sulfur dioxide through rotary kiln pre-reduction, the sulfur dioxide is removed in a gaseous form, the obtained calcine enters an ore heating furnace to be smelted and separated, and valuable metals such as iron, nickel and chromium are recovered. In the process, the mass ratio of the laterite-nickel ore to the stainless steel pickling sludge to the reducing agent is 100: 20-50: 2-6; the mass ratio of the green pellets to the laterite-nickel ore to the reducing agent is 5-20: 100: 5-10, the reducing agent is coke powder and/or anthracite with the sulfur content of less than or equal to 0.8 wt%, the consumption of acid-washing sludge is small, and the energy consumption of the rotary kiln and the submerged arc furnace is high in two-step method.
Because the direct reduction of the stainless steel pickling sludge can synchronously realize the reduction of valuable metals and the reduction and removal of sulfate, the economic efficiency of the stainless steel pickling sludge can be greatly improved by selecting an environment-friendly and cheap reducing agent. The blast furnace dust is discharged along with blast furnace flue gas, and the furnace charge dust collected by the dust collector contains a large amount of C particles and metal oxides such as Fe, Zn and the like, and is easy to float in the atmosphere after being dried, thereby seriously polluting the environment. The blast furnace dust is recycled, valuable elements such as C, Fe and the like in the blast furnace dust can be fully utilized, and the blast furnace dust has important economic value, but the key to the blast furnace smelting of harmful elements such as Zn and the like in the dust is separated and extracted.
Patent CN201910640514.6 discloses a method for producing nickel-chromium-iron alloy by using stainless steel dedusting ash and pickling sludge, the technical scheme disclosed in the patent application mixes and granulates stainless steel pickling sludge, stainless steel dedusting ash and granular coal or carbon fine powder, the mixed granules are sintered in a vertical sintering kiln to obtain porous sintering reduction ore, and then coke powder, quartz, limestone and a proper amount of iron oxide sheet are added, and high-temperature melting reduction is carried out by using an ore-smelting electric furnace. However, the scheme does not relate to a disposal scheme after the removal of S in the acid-washing sludge and Zn in the dedusting ash, so that the problem of serious secondary pollution exists; meanwhile, a large amount of granulated coal (or carbon fine powder) and coke powder are needed in the scheme, the process flow is long, and the economical efficiency is low.
Patent CN202011099935.1 discloses a comprehensive utilization method of stainless steel solid waste. Compared with the patent CN202010225343.3, one of the main points of the method is that the treatment process is a combination of rotary kiln reduction and submerged arc furnace melting separation, and one of the main points of the method is that the method disclosed by the patent CN202011099935.1 needs to use an adhesive. Patent CN202110733228.1 discloses a high-efficiency rotary hearth furnace direct reduction treatment process for zinc-containing dust and sludge in steel plants, but high volatile coal and bentonite are also required to be additionally added, and the use of inorganic binders such as bentonite and the like can reduce the iron grade of raw materials, which is not beneficial to the production of ferroalloy. Patent CN201910220083.8 discloses a stainless steel pickling sludge press ball and a preparation method and application thereof, wherein a composite cellulose type binder is used, and one or more of aluminum powder, silicon-aluminum-iron powder, silicon-manganese powder, carbon powder particles, continuous casting/hot rolling/annealing oxide skin, silicon carbide and fluorite particles are additionally added, so that the economy is poor.
Disclosure of Invention
Aiming at the problems of long process flow, need of additionally adding adhesive or coal reducing agent and flue gas SO existing in the resource utilization of the existing stainless steel acid-washing sludge and blast furnace dust2The invention provides a synergistic treatment technology for stainless steel pickling sludge and blast furnace fly ash, and realizes triple targets of sulfur fixation of the stainless steel pickling sludge, dezincification of the fly ash and direct preparation of a metallized furnace charge from a mixed material.
The invention aims to provide a method for preparing sulfur-fixing agent, which comprises the steps of mixing stainless steel acid-washing sludge with blast furnace gravity dedusting ash (with low zinc content) for materialization granulation, then mixing with cloth bag dedusting ash (with high zinc content), and converting calcium sulfate into sulfides such as FeS, CaS and the like in a medium-temperature reduction roasting stage by using the mixed material to realize sulfur fixation; the metal oxide is reduced in the high-temperature reduction roasting stage to realize the reduction removal of zinc and the metallization of Fe, Cr and Ni, and crude zinc can be recovered and extracted through flue gas treatment. The sulfur-containing metal melting furnace material directly returns to the blast furnace, slag forming and desulfurization are carried out, stainless steel molten iron is smelted, and the synergistic treatment and high-value utilization of valuable metals of the stainless steel pickling sludge and the blast furnace dedusting ash are realized. The invention passes a large number of experimentsThe research finds that: the stainless steel acid-washing sludge is mixed with the blast furnace gravity ash, on one hand, the coarse and fine particle size matching is adopted, and particularly, the coarse particle size carbon particles in the gravity ash can be used as a pelletizing framework to promote powder pelletizing; on the other hand, the blast furnace gravity fly ash with low zinc content is used as the pellet internal carbon, and the blast furnace cloth bag fly ash with high zinc content is used as the external carbon, so that the dezincification rate, the sulfur fixation rate and the metallization rate are improved. The sulfur in the metallized furnace charge mainly exists stably in the form of sulfides such as FeS, CaS and the like, and enters the slag phase through the smelting procedures such as a subsequent blast furnace and the like, thereby solving the problem of high-concentration SO in the pyrogenic process treatment process of the prior stainless steel pickling sludge2And (4) the problem of smoke emission.
In order to realize the purpose, the invention provides a method for cooperatively treating and utilizing stainless steel pickling sludge and blast furnace dust, which comprises the following steps:
(1) placing the dried stainless steel acid-washing sludge and the blast furnace gravity dedusting ash in a stirring device according to the mass ratio of 10:2-5, uniformly mixing, transferring the mixed material to a disc pelletizer, pelletizing, and preparing into granular materials with the granularity of 5-15 mm;
(2) placing the granular material and the blast furnace cloth bag dedusting ash in a furnace according to the mass ratio of 10:1-5, and drying at 100-200 ℃ for 10-120 min; carrying out medium-temperature reduction roasting at the temperature of 500-750 ℃ for 0-60min, carrying out high-temperature reduction roasting at the temperature of 1000-1400 ℃ for 10-30min, and collecting the solid particle product of the roasting smoke in the whole process;
(3) and (3) screening after the roasted product is cooled to obtain the sulfur-containing metallized furnace charge with proper granularity, directly returning to a blast furnace for smelting, slagging and desulfurizing, and preparing the stainless steel molten iron.
Further, the water content of the granular mixed material is controlled to be less than 30% in the step (1).
Further, the zinc content of the blast furnace gravity dust in the step (1) is lower than 1%.
Further, in the step (2), the granular mixed material and the blast furnace cloth bag dedusting ash are subjected to layered distribution.
Further, the heating mode of the kiln in the step (2) comprises microwave heating, resistance heating and induction heating.
And (3) further, the solid particle product of the roasting smoke collected in the step (2) is condensed and settled to obtain a crude zinc product.
Further, in the step (3), the blast furnace smelting adopts a blast furnace smelting method of laterite nickel ore.
And (3) further, mixing the fine-grained particles crushed and sieved in the step (3) with the blast furnace gravity dedusting ash, and returning to the step (1).
According to the method for the cooperative treatment and high-value utilization of the stainless steel pickling sludge and the blast furnace dust, the metallization rate of iron, nickel and chromium of the mixed material after reduction roasting can exceed 70%, the proportion of the calcium sulfate converted into the metal sulfide (the sulfur fixation rate) exceeds 50%, and the removal rate of zinc exceeds 90%.
According to the invention, after optimization, the metallization rates of iron, nickel and chromium of the mixed material after reduction roasting can exceed 85%, the proportion of calcium sulfate converted into metal sulfide (sulfur fixation rate) exceeds 95%, and the removal rate of zinc exceeds 99.9%.
The technical key points of the invention are as follows: (1) mixing and granulating the water-containing stainless steel pickling sludge and the blast furnace gravity dedusting ash to create conditions for full contact between calcium sulfate in the stainless steel pickling sludge and carbon particles in the blast furnace gravity dedusting ash and promote the reduction and conversion of the calcium sulfate into sulfide; (2) the medium-temperature roasting can utilize calcium sulfate and carbon to react to generate FeS and CaS, the roasting temperature is controlled within 750 ℃, the sulfur fixation rate can be greatly improved, and SO is reduced2Generating gas; (3) the high-temperature roasting process mainly comprises the reduction of iron, nickel, chromium and zinc, and the metal sulfide can react with iron oxide to generate SO at the temperature of 1100-1300 DEG C2Gas, wherein the roasting temperature is controlled to be higher than 1300 ℃ in order to improve the sulfur fixation rate; (4) the sulfur content of the metallized furnace charge prepared by the synergistic treatment of the stainless steel acid-washing sludge and the blast furnace dust can be regulated and controlled by the mixture ratio and the roasting temperature system, so that the metallized furnace charge meeting the sulfur load of the blast furnace can be obtained.
The conception, the specific structure and the technical effects of the present invention will be further described with reference to the accompanying drawings to fully understand the objects, the features and the effects of the present invention.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a SEM-BSE data of a cross section of a metallization furnace charge product in a first preferred embodiment of the present invention;
FIG. 3 is a SEM-BSE data of a cross section of a metallization furnace charge product in a second preferred embodiment of the present invention;
FIG. 4 is a SEM-BSE data of a cross section of a metallization furnace charge product in a third preferred embodiment of the present invention;
Detailed Description
The technical contents of the preferred embodiments of the present invention will be more clearly and easily understood by referring to the drawings attached to the specification. The present invention may be embodied in many different forms of embodiments and the scope of the invention is not limited to the embodiments set forth herein.
The process flow of the present invention is shown in FIG. 1. In the implementation example, the raw material stainless steel pickling sludge, the blast furnace gravity dedusting ash and the cloth bag dedusting ash are provided by a certain stainless steel factory, wherein the water content of the stainless steel pickling sludge is about 55%, and the chemical components after drying are as follows: TFe, Ni, Cr, S and Ca were 18.4%, 0.57%, 3.13%, 4.67% and 16.97%, respectively; the blast furnace gravity dedusting ash TFe, Cr, Zn, Ni and C are respectively 17.29%, 1.05%, 0.56%, 0.38% and 43.25%; chemical components TFe, Cr, Ni, Zn and C of the blast furnace cloth bag dedusting ash are 14.71%, 1.01%, 0.26%, 5.50% and 39.07% respectively.
Example 1:
(1) 0.7kg of stainless steel acid-washing sludge and 0.3kg of blast furnace gravity dedusting ash are placed in a small mixer in a laboratory for mixing and stirring for 30min, and then transferred to a disc pelletizer for pelleting to prepare granular materials with the granularity of 5-15 mm.
(2) 0.2kg of blast furnace cloth bag dedusting ash is weighed and mixed with the granular materials, then the mixture is placed into a corundum crucible, and the corundum crucible is placed into an atmosphere resistance furnace.
(3) Setting a temperature rising system: raising the room temperature to 105 ℃, preserving heat for 60min, raising the temperature to 1250 ℃, and preserving heat for 30 min;
(4) the temperature increase procedure was started while a stream of nitrogen (100mL/min) was passed into the atmosphere furnace.
(5) And after roasting is finished, cooling the roasted product, crushing and screening to obtain a metallization furnace material product, wherein the metallization rate, the dezincification rate and the sulfur fixation rate of the mixed material are 83.5%, 99.7% and 85.5% respectively.
(6) The crude zinc product is obtained after the smoke dust collected in the roasting process is cooled and settled, wherein the grade of zinc is 87.5 percent, and the recovery rate of zinc is 87.2 percent.
(7) FIG. 2 is a SEM-BSE data plot of cross-sections of metallized charge products in this example.
Example 2
(1) Placing 0.7kg of stainless steel acid-washing sludge and 0.35kg of blast furnace gravity dedusting ash in a small mixer in a laboratory for mixing and stirring for 30min, and then transferring the mixture to a disc pelletizer for pelleting to prepare granular materials with the granularity of 5-15 mm;
(2) weighing 0.15kg of blast furnace cloth bag dedusting ash, mixing the blast furnace cloth bag dedusting ash with the granular materials, placing the mixture into a corundum crucible, and placing the corundum crucible into an atmosphere resistance furnace;
(3) setting a temperature rising system: raising the room temperature to 105 ℃, preserving heat for 60min, raising the temperature to 700 ℃, preserving heat for 30min, and finally raising the temperature to 1250 ℃, preserving heat for 30 min;
(4) starting a temperature-raising program, and simultaneously introducing nitrogen gas flow (100mL/min) into the atmosphere furnace;
(5) and after roasting is finished, cooling the roasted product, crushing and screening to obtain a metallization furnace material product, wherein the metallization rate, the dezincification rate and the sulfur fixation rate of the mixed material are 85.9%, 99.6% and 91.8% respectively.
(6) The crude zinc product is obtained after the smoke dust collected in the roasting process is cooled and settled, wherein the grade of zinc is 82.5 percent, and the recovery rate of zinc is 82.1 percent.
(7) FIG. 3 is a SEM-BSE data plot of cross-sections of metallized charge products in this example.
Example 3
(1) Placing 0.7kg of stainless steel acid-washing sludge and 0.3kg of blast furnace gravity dedusting ash in a small mixer in a laboratory for mixing and stirring for 30min, and then transferring the mixture to a disc pelletizer for pelleting to prepare granular materials with the granularity of 5-15 mm;
(2) weighing 0.2kg of blast furnace cloth bag dedusting ash, mixing the blast furnace cloth bag dedusting ash with the granular materials, placing the mixture into a corundum crucible, and placing the corundum crucible into an atmosphere resistance furnace;
(3) setting a temperature rising system: raising the room temperature to 105 ℃, preserving heat for 60min, raising the temperature to 700 ℃, preserving heat for 30min, and finally raising the temperature to 1350 ℃ and preserving heat for 20 min;
(4) starting a temperature-raising program, and simultaneously introducing nitrogen gas flow (100mL/min) into the atmosphere furnace;
(5) and after roasting is finished, cooling the roasted product, crushing and screening to obtain a metallization furnace material product, wherein the metallization rate, the dezincification rate and the sulfur fixation rate of the mixed material are 86.5%, 99.8% and 95.4% respectively.
(6) The crude zinc product is obtained after the smoke dust collected in the roasting process is cooled and settled, wherein the grade of zinc is 80.5 percent, and the recovery rate of zinc is 80.3 percent.
(7) FIG. 4 is a SEM-BSE data plot of cross-sections of metallized charge products in this example.
The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concepts. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.
Claims (8)
1. A method for cooperatively treating and utilizing stainless steel pickling sludge and blast furnace dust is characterized by comprising the following steps:
(1) placing the dried stainless steel acid-washing sludge and the blast furnace gravity dedusting ash in a stirring device according to the mass ratio of 10:2-5, uniformly mixing, transferring the mixed material to a disc pelletizer, pelletizing, and preparing into granular materials with the granularity of 5-15 mm;
(2) placing the granular material and the blast furnace cloth bag dedusting ash in a furnace according to the mass ratio of 10:1-5, and drying at 100-200 ℃ for 10-120 min; carrying out medium-temperature reduction roasting at the temperature of 500-750 ℃ for 0-60min, carrying out high-temperature reduction roasting at the temperature of 1000-1400 ℃ for 10-30min, and collecting the solid particle product of the roasting smoke in the whole process;
(3) and (3) screening after the roasted product is cooled to obtain the sulfur-containing metallized furnace charge with proper granularity, directly returning to a blast furnace for smelting, slagging and desulfurizing, and preparing the stainless steel molten iron.
2. The method for co-processing and utilizing stainless steel pickling sludge and blast furnace dust-removing ash according to claim 1, wherein the water content quality in the granular mixed material is controlled to be less than 30% in the step (1).
3. The method for co-processing and utilizing stainless steel pickling sludge and blast furnace dust according to claim 1, wherein the zinc content of the blast furnace gravity dust in the step (1) is less than 1%.
4. The method for co-processing and utilizing stainless steel pickling sludge and blast furnace dust according to claim 1, wherein in the step (2), the granular mixed material and the blast furnace cloth bag dust are subjected to layered distribution.
5. The method for co-processing and utilizing stainless steel pickling sludge and blast furnace dust according to claim 1, wherein the heating mode of the kiln in the step (2) comprises microwave heating, resistance heating and induction heating.
6. The method for co-processing and utilizing stainless steel pickling sludge and blast furnace dust removal ash as claimed in claim 1, wherein the step (2) collects solid particle products of roasting flue gas, and crude zinc products are obtained after condensation and sedimentation.
7. The method for the cooperative disposal and utilization of stainless steel pickling sludge and blast furnace dust according to claim 1, wherein the blast furnace smelting in the step (3) adopts a blast furnace smelting method of laterite-nickel ore.
8. The method for co-processing and utilizing stainless steel pickling sludge and blast furnace dust according to claim 1, wherein the fine-grained particles crushed and sieved in the step (3) are mixed with the blast furnace gravitational dust and then returned to the step (1).
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| CN115404297A (en) * | 2022-09-22 | 2022-11-29 | 华北理工大学 | Method for co-processing fly ash and blast furnace cloth bag fly ash |
| CN115404297B (en) * | 2022-09-22 | 2023-09-19 | 华北理工大学 | Method for cooperatively disposing fly ash and blast furnace cloth bag dust removal ash |
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