CN108251659B - Method for preparing ferronickel by strengthening direct reduction process of laterite-nickel ore - Google Patents
Method for preparing ferronickel by strengthening direct reduction process of laterite-nickel ore Download PDFInfo
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- CN108251659B CN108251659B CN201810040918.7A CN201810040918A CN108251659B CN 108251659 B CN108251659 B CN 108251659B CN 201810040918 A CN201810040918 A CN 201810040918A CN 108251659 B CN108251659 B CN 108251659B
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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
- C22B23/00—Obtaining nickel or cobalt
- C22B23/02—Obtaining nickel or cobalt by dry processes
- C22B23/023—Obtaining nickel or cobalt by dry processes with formation of ferro-nickel or ferro-cobalt
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21B—MANUFACTURE OF IRON OR STEEL
- C21B13/00—Making spongy iron or liquid steel, by direct processes
- C21B13/006—Starting from ores containing non ferrous metallic oxides
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Abstract
The invention discloses a method for preparing ferronickel by a reinforced laterite-nickel ore direct reduction process, which is to prepare a ferronickel product by adding a certain mass proportion of alkaline flux into laterite-nickel ore and adopting a rotary kiln direct reduction process. In the process of reduction roasting, the contents of calcium oxide and ferrous oxide in the laterite-nickel ore are controlled through the combined action of a flux and a reducing agent, a proper low-melting-point eutectic phase is generated, and the reduction roasting temperature of a rotary kiln is reduced; the liquid phase yield of the reduction process is improved, the mass transfer process among the ferronickel particles is improved, and the aggregation growth of the ferronickel particles is promoted, so that the separation effect of the magnetic ferronickel product and the non-magnetic tailings is enhanced. The method can reduce the operation temperature of the rotary kiln by about 200 ℃, greatly improve the recovery rate of nickel and iron and obviously improve the separation effect of nickel and iron.
Description
Technical Field
The invention discloses a method for preparing ferronickel by strengthening a direct reduction process of laterite-nickel ore, belonging to the technical field of metallurgy.
Background
The global land-based nickel ore resources are divided into nickel sulfide ores and nickel laterite ores. Wherein the nickel sulfide ore accounts for about 40 percent, and the rest 60 percent is the laterite-nickel ore. Limited by the dressing and smelting technology of the laterite-nickel ore, the nickel sulfide ore is the main source for nickel production in a long period in the past, and the high-grade nickel sulfide ore is adopted as the raw material to produce nickel-containing products so as to meet the requirements of various industries on nickel. Along with the continuous consumption of the explored nickel sulfide ore and the continuous reduction of the reserves of the newly explored nickel sulfide ore, the resource of the nickel sulfide ore which can be exploited in the global scope is gradually exhausted, and the requirement of the continuously increased nickel production amount on the raw materials is difficult to meet. How to develop the laterite-nickel ore resources with high efficiency and low cost has great significance for the healthy development of the nickel industry.
The process for preparing the ferronickel by directly reducing the laterite-nickel ore has the advantages of short flow, low energy consumption, strong adaptability to laterite-nickel ore raw materials and the like. According to the process, bituminous coal and anthracite are generally used as reducing agents and fuels, about 80-85% of total energy consumption is provided by coal, and the process is the most economical method for treating high-grade laterite-nickel ore at present. Drying, crushing and screening the laterite-nickel ore, mixing the laterite-nickel ore with a reducing agent to prepare a briquette, reducing and roasting the briquette in a rotary kiln to generate ferronickel, and separating the ferronickel from slag of the roasted product by water quenching, cooling, crushing, screening, magnetic separation or gravity separation to obtain a magnetic ferronickel product.
The process is originally developed from a German Krupp-Renn direct reduction iron-making process, a Japanese Dajiang mountain smelting plant firstly uses a rotary kiln direct reduction process to produce ferronickel in the 30 s of the 20 th century, and continuously operates to the present, and the quantity of the ferronickel produced annually is about 1.5 ten thousand tons (calculated by metallic nickel) at present. In recent years, some domestic nickel-iron factories successively put into production part of rotary kiln direct reduction production lines, such as north hechnode nickel industry ltd, baotongdeph stainless steel ltd, and the like, and Shanghai Pantayo group, Dafenggang (Indonesia), Shunxi nickel industry ltd, and the like, will also newly build direct reduction production lines abroad.
However, the process still has problems to be solved by the prior production discovery. In order to realize the physical separation of the ferronickel and the tailings, a part of the laterite-nickel ore generation liquid phase is required to enable the material to reach a semi-molten state in the rotary kiln reduction process, so that the mass transfer condition of ferronickel particles in the material is improved, and the aggregation of the ferronickel particles is promoted. Because the laterite-nickel ore has high silicon and magnesium contents, pyroxene and olivine phases generated in the reduction roasting process have high melting points. In order to meet the semi-molten state condition of the materials, the reduction roasting temperature of the rotary kiln is high, the temperature of a high-temperature section exceeds 1400 ℃, the temperature control interval is narrow, and the operation condition is harsh. Taking the production of Nippon Dajiang mountain ferronickel factory as an example, the highest reduction roasting temperature of the rotary kiln can reach 1400-1450 ℃. On the other hand, in the production process, the generation of a liquid phase is difficult to control due to single phase generation, and when the reduction roasting temperature is lower than the melting temperature of a pyroxene or olivine phase, no liquid phase is generated or the generation of the liquid phase is small; when the reduction temperature is higher than the phase melting temperature, the liquid phase is melted to form a liquid phase, and excessive liquid phase generation causes the formation of ring-forming substances on the inner wall of the rotary kiln, thereby influencing the smooth production. Therefore, although the direct reduction process has the advantages of low energy consumption, the process is delayed and not applied on a large scale due to the reasons. Except that the real ferronickel production is realized in a Nippon Dajiang mountain ferronickel factory, other direct reduction production lines basically only utilize a rotary kiln to reduce laterite-nickel ore, and the reduced calcine can only recover large-size blocky ferronickel and partial ferronickel powder in the physical separation process, so that the ferronickel separation effect is poor, the recovery rate is low, and only 60-70% of nickel can be directly recycled as ferronickel. After the non-magnetic tailings of the residual nickel-containing calcine are removed, the residual nickel-containing calcine still needs to be smelted in an electric furnace/blast furnace to produce nickel-containing molten iron, so that the overall recovery rate of nickel and iron is improved, and the production efficiency of direct reduction of the rotary kiln is low.
Disclosure of Invention
Aiming at the problems of difficult separation of nickel iron and tailings and the like in the direct reduction process of the laterite-nickel ore, the invention provides the method for preparing the nickel iron by the reinforced direct reduction process of the laterite-nickel ore, and the method can obviously improve the separation effect of the nickel iron and has good nickel recovery effect. In addition, the method can also reduce the reduction roasting temperature of the rotary kiln, reduce the ring formation possibility of the rotary kiln and the like.
The technical scheme of the invention is as follows:
the invention relates to a method for preparing ferronickel by strengthening a direct reduction process of laterite-nickel ore, which is characterized in that calcium oxide accounting for 10-20% of the mass of laterite-nickel ore is added in the process of adopting the direct reduction process of laterite-nickel ore, meanwhile, the mass ratio of fixed carbon in a reducing agent to total iron in laterite-nickel ore is controlled to be 0.3-0.5, the nickel recovery rate is more than or equal to 80%, and the iron recovery rate is more than or equal to 80%.
The invention relates to a method for preparing ferronickel by a reinforced laterite-nickel ore direct reduction process, wherein the reduction roasting temperature of the laterite-nickel ore direct reduction process is 1200-1250 ℃, and the reduction time is 2-5 h.
The invention relates to a method for preparing ferronickel by a reinforced laterite-nickel ore direct reduction process, wherein in the laterite-nickel ore direct reduction process, diopside and fayalite are formed when materials are at 1000-1200 ℃, the diopside accounts for 10-30% of the materials by mass, and the fayalite accounts for 10-20% of the materials by mass.
According to the method for preparing ferronickel by strengthening the direct reduction process of the laterite-nickel ore, diopside and fayalite are converted into liquid phases at the reduction roasting temperature of 1200-1250 ℃, and the liquid phases account for 20-40% of the materials by mass.
The invention relates to a method for preparing ferronickel by strengthening a direct reduction process of laterite-nickel ore, wherein calcium oxide is derived from limestone and/or quicklime.
The invention relates to a method for preparing ferronickel by strengthening a laterite-nickel ore direct reduction process.
The invention relates to a method for preparing ferronickel by strengthening a laterite-nickel ore direct reduction process, wherein the direct reduction process is implemented in a rotary kiln.
The invention relates to a method for preparing ferronickel by a reinforced laterite-nickel ore direct reduction process.
The invention relates to a method for preparing ferronickel by strengthening a direct reduction process of laterite-nickel ore, wherein in the ferronickel product obtained after the direct reduction process treatment of laterite-nickel ore, the nickel grade is more than or equal to 7 percent, and the iron grade is more than or equal to 80 percent.
The invention relates to a method for preparing ferronickel by strengthening a direct reduction process of laterite-nickel ore, which comprises the following main chemical components:
the nickel content is more than or equal to 1.5 percent, the total iron content is more than or equal to 15 percent, the magnesium oxide content is more than or equal to 10 percent, and the silicon oxide content is more than or equal to 20 percent.
The main principle of the invention is as follows:
according to the invention, the content of calcium oxide in the laterite-nickel ore is increased by adding the flux, when the rotary kiln is used for reduction roasting at a low temperature (1000-1200 ℃), the calcium oxide reacts with magnesium and silicon minerals in the laterite-nickel ore to generate diopside, and the addition amount of the flux is controlled to enable the generation amount of the diopside to be 10-30%. In addition, the addition amount of the reducing agent is controlled, so that part of divalent iron in the laterite-nickel ore is reserved and reacts with magnesium and silicon minerals to generate fayalite, wherein the generation amount of the fayalite is controlled to be 10-20%. The diopside and the fayalite are converted into a low-melting-point solid solution phase at a high temperature and are melted to form a liquid phase at the reduction temperature of 1200-1250 ℃, so that the mass transfer process among the reduced nickel-iron particles is improved, the aggregation growth of the nickel-iron particles is promoted, and the separation of the magnetic nickel-iron product and the non-magnetic tailings is strengthened. According to the invention, by properly increasing calcium oxide and controlling the addition amount of the reducing agent, the liquid phase generation amount is ensured to reach 20-40% at the reduction temperature of 1200-1250 ℃, the growth of nickel-iron particles is promoted, and the recovery rate of nickel and iron is greatly increased.
The invention has the advantages and beneficial effects that: in the existing process for producing ferronickel by direct reduction, the laterite-nickel ore material forms enstatite and forsterite in the reduction process, the melting temperature is high, and the operation temperature of the rotary kiln reaches 1400-1450 ℃ at most. According to the invention, by adding the alkaline flux into the laterite-nickel ore and controlling the adding amount of the reducing agent, a certain amount of diopside and fayalite low-melting-point eutectic phase is generated in the reduction process, the generation amount of a liquid phase can be increased at the reduction temperature of 1200-1250 ℃, the aggregation growth of nickel-iron particles is promoted, and the separation effect of magnetic nickel-iron products and non-magnetic tailings is enhanced. Compared with the prior art, the method can also reduce the reduction roasting temperature of the rotary kiln by about 200 ℃. Meanwhile, the possibility of ring formation of the rotary kiln is reduced by controlling the generated liquid phase amount to be 20-40% of the material mass.
Drawings
FIG. 1 is a photograph showing the microstructure of a certain region in an aliquot of a reduction-calcined sample after water quenching in example 1.
In the figure, the distribution of liquid phase and solid phase is clear.
Detailed Description
The invention is further explained and illustrated below.
The main chemical components of the laterite-nickel ore used in the examples and the comparative examples of the invention are shown in table 1, and the laterite-nickel ore is dried and crushed in advance until the granularity is less than 3 mm.
TABLE 1 main chemical composition/The% of laterite-nickel ore
In the embodiment and the comparative example of the invention, the mass ratio of the liquid phase to the material in the roasting process is measured according to the following method:
and uniformly dividing the reduction roasting sample (the sample is in an ellipsoidal shape) after water quenching along the long axis to obtain a plurality of equally divided sections, and taking at least 8 equally divided sections to prepare a polished section. One of the slides was taken, and under an electron microscope, the slide was equally divided into 5 regions, and an equivalent microstructure picture was taken for each region. And (3) counting the liquid phase area of the polished section by image analysis software, and calculating the proportion of the liquid phase area to the total area of the polished section to obtain the proportion of the liquid phase at the position of the polished section in the reduction roasting sample to the total area of the bisector section. The liquid phase proportion of each equal section in the reduction roasting sample under the same condition is repeatedly counted according to the method. The arithmetic mean value is the proportion of the liquid phase in the material under a certain test condition.
Comparative example:
the laterite-nickel ore and a certain mass of reducing agent are fully and uniformly mixed, agglomerated and dried, the reducing agent is lignite, and the mass ratio of fixed carbon in the reducing agent to total iron in the laterite-nickel ore is 0.35. The briquettes were calcined in a rotary kiln at 1200 ℃ for 3 h. The measurement shows that the mass ratio of the liquid phase to the material in the roasting process is about 4%. The reduction product is crushed and ground after water quenching until 90 percent is less than 74 mu m, and magnetic separation is carried out. The nickel and iron grades in the obtained ferronickel product are respectively 3.7 percent and 65.4 percent, and the recovery rates of nickel and iron are respectively 47.9 percent and 76.4 percent.
Example 1:
sufficiently and uniformly mixing the laterite-nickel ore powder with a certain mass of flux and a certain mass of reducing agent, agglomerating and drying, wherein the flux is quicklime, and the addition amount of calcium oxide is 10 percent of the mass of the laterite-nickel ore; the reducing agent is lignite, and the mass ratio of the fixed carbon in the reducing agent to the total iron in the laterite-nickel ore is 0.35. The briquettes were calcined in a rotary kiln at 1200 ℃ for 3h to obtain the reduced product. The measurement shows that the mass ratio of the liquid phase to the material in the roasting process is about 23%. The reduction product is crushed and ground after water quenching until 90 percent is less than 74 mu m, and magnetic separation is carried out. The nickel and iron grades in the obtained ferronickel product are respectively 7.1 percent and 82.3 percent, and the recovery rates of the nickel and the iron are respectively 82.3 percent and 81.9 percent. Compared with the comparative example, the nickel and iron grades and the recovery rate are greatly improved in the embodiment.
Example 2:
sufficiently and uniformly mixing the laterite-nickel ore powder with a certain mass of flux and a certain mass of reducing agent, agglomerating and drying, wherein the flux is quicklime, and the addition amount of calcium oxide is 15% of the mass of the laterite-nickel ore; the reducing agent is lignite, and the mass ratio of the fixed carbon in the reducing agent to the total iron in the laterite-nickel ore is 0.35. The briquettes were calcined in a rotary kiln at 1200 ℃ for 3h to obtain the reduced product. The liquid phase accounts for about 28% of the mass of the material in the roasting process. The reduction product is crushed and ground after water quenching until 90 percent is less than 74 mu m, and magnetic separation is carried out. The nickel and iron grades in the obtained ferronickel product are respectively 7.6 percent and 85.2 percent, and the recovery rates of the nickel and the iron are respectively 85.3 percent and 87.1 percent. Compared with the comparative example, the nickel and iron grades and the recovery rate are greatly improved in the embodiment.
Example 3:
sufficiently and uniformly mixing the laterite-nickel ore powder with a certain mass of flux and a certain mass of reducing agent, agglomerating and drying, wherein the flux is quicklime, and the addition amount of calcium oxide is 15% of the mass of the laterite-nickel ore; the reducing agent is lignite, and the mass ratio of the fixed carbon in the reducing agent to the total iron in the laterite-nickel ore is 0.35. The briquettes were calcined in a rotary kiln at 1250 ℃ for 3h to obtain the reduced product. The measurement shows that the mass ratio of the liquid phase to the material in the roasting process is about 35%. The reduction product is crushed and ground after water quenching until 90 percent is less than 74 mu m, and magnetic separation is carried out. The nickel and iron grades in the obtained ferronickel product are respectively 8.0 percent and 87.8 percent, and the recovery rates of the nickel and the iron are respectively 88.2 percent and 89.0 percent. Compared with the comparative example, the nickel and iron grades and the recovery rate are greatly improved in the embodiment.
Claims (7)
1. A method for preparing ferronickel by a reinforced laterite-nickel ore direct reduction process is characterized in that calcium oxide accounting for 10-20% of the mass of laterite-nickel ore is added in a laterite-nickel ore direct reduction process, the mass ratio of fixed carbon in a reducing agent to total iron in the laterite-nickel ore is controlled to be 0.3-0.5, the reduction roasting temperature of the laterite-nickel ore direct reduction process is 1200-1250 ℃, materials form diopside and fayalite at 1000-1200 ℃ in the laterite-nickel ore direct reduction process, the mass ratio of the diopside to the materials is 10-30%, the mass ratio of the fayalite to the materials is 10-20%, the diopside and the fayalite are converted into liquid phase at the reduction roasting temperature of 1200-1250 ℃, the mass ratio of the liquid phase to the materials is 20-40%, the nickel recovery rate is not less than 80%, and the iron recovery rate is not less than 80%.
2. The method for preparing ferronickel by strengthening the direct reduction process of lateritic nickel ore according to claim 1, is characterized in that: the reduction roasting time of the laterite nickel ore direct reduction process is 2-5 h.
3. The method for preparing ferronickel by strengthening the laterite-nickel ore direct reduction process according to claim 1 or 2, characterized by comprising the following steps: the calcium oxide is derived from limestone and/or quicklime.
4. The method for preparing ferronickel by strengthening the direct reduction process of lateritic nickel ore according to claim 3, characterized by comprising the following steps: the reducing agent is selected from at least one of lignite, bituminous coal and anthracite.
5. The method for preparing ferronickel by strengthening the direct reduction process of lateritic nickel ore according to claim 4, is characterized in that: the direct reduction process is carried out in a rotary kiln.
6. The method for preparing ferronickel by strengthening the direct reduction process of lateritic nickel ore according to claim 5, is characterized in that: in the direct reduction process, the magnetic ferronickel product and the nonmagnetic tailings are separated by means of gravity separation and magnetic separation.
7. The method for preparing ferronickel by the reinforced laterite-nickel ore direct reduction process according to claim 6, characterized by comprising the following steps: in the nickel-iron product obtained after the laterite-nickel ore direct reduction process treatment, the nickel grade is more than or equal to 7 percent, and the iron grade is more than or equal to 80 percent.
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| CN110735012B (en) * | 2019-10-23 | 2021-05-11 | 苏州工业职业技术学院 | Method for preparing electric furnace smelting ferronickel raw material by using laterite-nickel ore |
| CN114182155A (en) * | 2021-11-24 | 2022-03-15 | 中冶南方工程技术有限公司 | Method for preparing ferronickel by reinforcing laterite-nickel ore with waste gypsum |
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| DE2831827A1 (en) * | 1978-07-20 | 1980-02-07 | Metallgesellschaft Ag | METHOD FOR DIRECT REDUCTION IN TURNTUBE |
| CN101270450B (en) * | 2008-05-09 | 2010-12-22 | 李大伦 | Ferro-nickel alloy and smelting method |
| CN101418359A (en) * | 2008-10-17 | 2009-04-29 | 中南大学 | Method for extracting iron and high grade ferro-nickel alloy from laterite nickle mine |
| CN101418389B (en) * | 2008-12-16 | 2010-07-28 | 毛黎生 | Method for directly reducing grain nickel iron in rotary kiln by using laterite nickle mine |
| CN102758085B (en) * | 2012-07-17 | 2013-11-06 | 中国钢研科技集团有限公司 | Method for producing nickel-iron alloy by smelting red earth nickel mineral at low temperature |
| CN104032058A (en) * | 2014-05-14 | 2014-09-10 | 章钦成 | Method for producing nickel-iron particles by using coal-based reducing agent to directly reduce laterite nickel ore |
| CN106702177B (en) * | 2017-01-23 | 2019-08-13 | 宝钢德盛不锈钢有限公司 | The technique of direct reduction of laterite nickel mine with rotary kiln ferronickel particle |
| CN107177741A (en) * | 2017-05-18 | 2017-09-19 | 江苏省冶金设计院有限公司 | The method and system of ferronickel is prepared using lateritic nickel ore |
| CN107217154A (en) * | 2017-05-18 | 2017-09-29 | 江苏省冶金设计院有限公司 | Handle the method and system of lateritic nickel ore |
| CN107287446B (en) * | 2017-06-20 | 2019-01-29 | 中南大学 | The quick reducing process of lateritic nickel ore rotary kiln |
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