CN107574278B - Method for preparing ferronickel by enriching nickel from laterite-nickel ore - Google Patents

Method for preparing ferronickel by enriching nickel from laterite-nickel ore Download PDF

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CN107574278B
CN107574278B CN201710626093.2A CN201710626093A CN107574278B CN 107574278 B CN107574278 B CN 107574278B CN 201710626093 A CN201710626093 A CN 201710626093A CN 107574278 B CN107574278 B CN 107574278B
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nickel
laterite
ferronickel
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reduction
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CN107574278A (en
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杭桂华
薛正良
肖承鹏
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Wuhan University of Science and Engineering WUSE
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Abstract

The invention discloses a method for preparing ferronickel by enriching nickel from laterite-nickel ore, which comprises the steps of uniformly mixing crushed laterite-nickel ore powder with a reducing agent and a fluxing agent, pressing into blocks, heating in a high-temperature furnace for prereduction, performing selective oxidation, and finally obtaining ferronickel with high nickel content by a melting separation method. The method realizes the selective oxidation of the metallic iron and nickel in the pre-reduction product, can greatly improve the nickel content in the ferronickel, and simultaneously realizes high nickel recovery rate, and the obtained high-quality ferronickel is beneficial to the smelting of stainless steel. The method has the characteristics of strong raw material adaptability, simple process flow, strong operability, high product quality, good nickel recovery effect, low energy consumption and treatment cost and the like. Provides a new direction for enriching nickel from laterite-nickel ore.

Description

Method for preparing ferronickel by enriching nickel from laterite-nickel ore
Technical Field
The invention belongs to the technical field of metallurgy, and particularly relates to a method for preparing ferronickel by enriching nickel from laterite-nickel ore.
Background
Laterite-nickel ore is used as a main source of the current primary nickel resource, the nickel content is far lower than the iron content, the nickel and the iron have similar physical and chemical characteristics, the nickel and the iron are attached to the silicate containing aluminum and magnesium, the embedding is very fine, and the nickel and the iron are difficult to effectively separate by physical ore dressing and other methods. Therefore, how to effectively enrich nickel in the laterite-nickel ore becomes a hot spot and a difficult point of further processing research on the laterite-nickel ore. At present, the enrichment of the pyro-treatment laterite-nickel ore on nickel is mainly concentrated in the pre-reduction process, and the main methods comprise: (1) selective reduction (reducing atmosphere is controlled by reducing internal carbon ratio) (Jianman, Sunzhang Chang, Liu Shi, etc. coal types and additive influence law [ J ] of the selective direct reduction of the laterite-nickel ore, mining and metallurgy engineering, 2012, 32 (5): 77-81); (2) in the pre-reduction process, an additive is added to inhibit the reduction of iron oxide (the ferrous oxide is vulcanized by a sulfur-containing additive to realize selective reduction, or sodium salt is added to inhibit the reduction of iron oxide) (Liguanghe, Naomingjun, Jiantao and the like, a mechanism of reduction roasting-magnetic separation of sodium salt of laterite nickel ore [ J ], Chinese nonferrous metals academic newspaper, 2012 and 22, (1): 27-280; Naomingjun, a basic and new process research [ D ], Changsha, Zhongnan university, 2014 ] for preparing crude ferronickel by selective reduction/vulcanization of laterite nickel ore. The technical solutions reported in the literature relating to the two methods mentioned above are also:
the one-step reduction roasting-magnetic separation process for preparing the ferronickel researches the influence of the addition of the reduction coal on the roasting effect, and the laterite-nickel ore has the following chemical components: ni1.52 percent, Fe14.08 percent and Ni/(Ni + Fe) 9.74 percent; adding a certain amount of reduced coal and additive, introducing N at 1200 deg.C2And (3) protective roasting for 180min to selectively reduce most of nickel oxide and a small amount of iron oxide in the raw ore to prepare nickel-iron fine powder containing 10.74% of Ni, wherein the recovery rate of Ni is 86.23%. The phase analysis only had 81.46% metallic nickel phase, another 13.25% nickel silicate phase, and the remainder nickel oxide phase. The content of nickel, nickel and nickel in nickel iron can be improved by selective reduction, but the effect is not obvious, and nickel oxide existing in nickel silicate phase in raw ore is not fully reduced due to insufficient carbon blending, so that the recovery rate of metal nickel is influenced. (Liangwei, royal glory, charm and the like.) high-efficiency recovery of ferronickel [ J ] from low-grade laterite-nickel ore]School newspaper of south and middle university (nature science edition), 2011, 42, (8): 2173 to 2177).
The invention patent (CN 102146511A 2011.08.10) discloses a process method for recovering nickel and iron in laterite-nickel ore by selective reduction roasting, which comprises the steps of crushing a certain amount of laterite-nickel ore into-10 mm, adding 10-20% of reducing agent and 5-15% of fluxing agent, roasting at 1100-1150 ℃ for 40-80 min after mixing, naturally cooling, grinding by a ball mill to obtain ore pulp with the concentration of 60% and the granularity of-0.074 mm accounting for 85-95%, and carrying out magnetic separation under the condition of the magnetic field intensity of 150-200 KA/m. 1.43% of nickel in raw ore, 13.21% of iron, 7.61% of nickel in ferronickel powder and 83.71% of nickel recovery rate. Although the process is simple, the content of nickel, iron and nickel in the final product is not high, and the recovery rate of nickel is low.
The invention patent (CN 102605174A 2012.07.25) discloses a process method for respectively recovering nickel and iron from low-nickel high-iron laterite-nickel ore, which respectively obtains two products of ferronickel powder and iron powder through two-step direct reduction roasting, wherein the raw ore contains 1.48% of Ni1, 33.56% of FeFe, 5% of reducing agent coal powder, 20% of additive, and the additive is a mixture of sodium hydroxide and calcium chloride, and the proportion is 1: 0.5, reducing and roasting the mixed sample at 1100 ℃ for 40min, grinding the sample to 90% of granularity of-0.074 mm when the mass concentration is about 60% after cooling, and carrying out magnetic separation under the magnetic field strength of 1.8KGs to obtain ferronickel powder containing 10.61% of nickel, wherein the nickel recovery rate is 80.71%; and continuously adding 25% of coal dust and 8% of binder into the magnetic separation tailings, reducing and roasting for 50min at 1200 ℃, cooling, and performing secondary magnetic separation to obtain iron powder. The process comprises twice material preparation, reduction roasting and magnetic separation, and has the advantages of complex process flow, difficult operation, large additive consumption, high energy consumption and cost and low nickel recovery rate.
The invention patent (CN 104498733A 2015.04.08) discloses a method for improving carbothermic selective reduction of laterite-nickel ore. By adding the sulfur-containing auxiliary agent, under a proper carbon thermal reduction system, sulfur in the sulfur-containing auxiliary agent preferentially reacts with an intermediate product FeO of the iron oxide to generate FeS, so that the reduction of ferrous oxide into metallic iron is inhibited. In the embodiment, the raw ore contains 1.90 percent of Ni and 22.10 percent of Fe22, the Ni content and the Fe content in the obtained ferronickel are respectively 10.39 percent and 81.91 percent, and the recovery rates of the Ni and the Fe are respectively 90.83 percent and 68.84 percent. The method has small improvement range of nickel-iron content, still has higher recovery rate of iron, and simultaneously, the sulfur content in the nickel-iron is inevitably improved greatly due to the addition of the sulfur-containing auxiliary agent, and the difficulty of stainless steel smelting is inevitably increased due to high-sulfur nickel-iron serving as a raw material nickel-iron for stainless steel smelting.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for preparing ferronickel by enriching nickel from laterite-nickel ore, aiming at the enrichment of medium-low grade laterite-nickel ore, the method adopts a coal-based pre-reduction-selective oxidation-melting separation process to prepare ferronickel, breaks through the traditional idea that the selective reduction method is adopted to enrich nickel, realizes the selective oxidation of metallic iron and metallic nickel by controlling the oxidation atmosphere and the oxidation time in the oxidation process on the basis of different oxygen affinity of the iron and the nickel, and obtains the ferronickel with high nickel content by melting separation at low temperature (1350-1500 ℃).
The invention adopts the following technical scheme to realize the purpose:
A method for preparing ferronickel by enriching nickel with lateritic nickel ore comprises the following steps: uniformly mixing the crushed laterite-nickel ore with reducing agent coal powder and/or coke powder and fluxing agent fluorite powder and/or boric acid, pressing into blocks, heating in a high-temperature furnace, pre-reducing, selectively oxidizing, and finally obtaining the ferronickel with high nickel content by a melting separation method.
In the technical scheme, the addition amount of the reducing agent must ensure that 10 to 40 percent of excessive carbon exists in the pre-reduction product while the nickel and iron oxides in the laterite-nickel ore are fully reduced; the adding amount of fluorite is 3-15% of the mass of the laterite-nickel ore, and the adding amount of boric acid is 0-1.5% of the mass of the laterite-nickel ore.
In the technical scheme, the internal carbon ratio is the ratio of the mole number of fixed carbon in the reducing agent to the mole number of oxygen of nickel and iron oxides in the laterite-nickel ore is more than 1.0.
In the technical scheme, the selective oxidation of the pre-reduction product is used for oxidizing the metallic iron at high temperature of 800-1200 ℃. The condition is to ensure that only the metallic iron is oxidized in the selective oxidation process, but the metallic nickel is not oxidized, and the oxidizing atmosphere and the oxidizing time are controlled until the excessive carbon in the reduction product is fully combusted.
In the technical scheme, the product after selective oxidation is melted and separated at 1350-1500 ℃, so that the slag and the gold are fully separated, and the ferronickel with high nickel content is obtained.
The mechanism of the invention is as follows: under the action of sufficient reducing agent, the oxide of iron and the oxide of nickel are fully reduced into metallic iron and metallic nickel. The metal iron and metal nickel particles in the pre-reduction product are dispersed and distributed in the slag phase, and the specific surface area is large. Because the affinity of iron and oxygen is greater than that of nickel and oxygen, under the oxidizing atmosphere, metallic iron preferentially reacts with oxygen to generate iron oxide; at the beginning of the oxidation process, because the pre-reduction product contains excessive reducing agent, the metal nickel is not oxidized in the early stage of oxidation, and the high-efficiency recovery of the metal nickel is ensured. Because the product after secondary oxidation contains a large amount of FeO with a low melting point and fluorite and/or boric acid serving as a fluxing agent added into the briquetting before pre-reduction, the slag with high content of iron oxide is separated from the metal with high content of nickel by melting separation at 1350-1500 ℃. The nickel in the ferronickel is greatly enriched.
Compared with the prior art for enriching nickel from laterite-nickel ore: the method breaks through the habitual thinking of enriching nickel in the process of reducing the laterite-nickel ore, and avoids the problems of unsatisfactory effect of selectively reducing and enriching nickel and low nickel recovery rate. The method does not add other sulfur-containing and sodium-containing additives, thereby avoiding the pollution of the additives to the ferronickel product and the corrosion to equipment.
In summary, the present invention has the following advantages: strong raw material adaptability, simple process flow, strong operability, high nickel content of the ferronickel product, good nickel recovery effect, low energy consumption and treatment cost and the like. Opens a new direction for enriching nickel from the laterite-nickel ore.
Drawings
FIG. 1 is a flow chart of the method for preparing ferronickel by enriching nickel from laterite-nickel ore.
Detailed Description
The present invention is further illustrated with reference to the following specific examples, but the scope of the present invention is not limited to the following specific examples.
The chemical components of the lateritic nickel ore are shown in table 1, the lateritic nickel ore is dried in advance and crushed to-5 mm to obtain lateritic nickel ore powder, and the preparation flow is shown in fig. 1.
Table 1 lateritic nickel ore chemical composition (%)
The process of preparing ferronickel by using the lateritic nickel ore powder is shown in fig. 1, wherein the Ni/(Fe + Ni) content of the lateritic nickel ore is 7.96%, and the details are described in the following specific examples.
example 1
Drying and crushing the laterite-nickel ore to be-5 mm, adding a reducing agent into coal powder according to 40% of excessive internal carbon, wherein the adding amount of fluorite in a fluxing agent is 5% of the amount of the laterite-nickel ore, and the adding amount of boric acid is 0.5% of the amount of the laterite-nickel ore. The method comprises the following steps of fully and uniformly mixing various raw materials, pressing the raw materials into blocks, fully pre-reducing the raw materials in a tunnel kiln at the temperature of 1100-1200 ℃, oxidizing a pre-reduced product in an atmosphere along with a furnace, carrying out secondary oxidation at the temperature of 1000-1150 ℃ for 120 minutes, and melting the oxidized product in an ore furnace at the temperature of 1450-1500 ℃ for 30 minutes to separate slag and gold to obtain ferronickel. Through experimental analysis, the nickel and iron contents in the ferronickel product are respectively 12.97% and 79.97%, and the nickel and iron recovery rates are respectively 92.64% and 49.43%.
Example 2
Drying and crushing the laterite-nickel ore to-5 mm, adding a reducing agent into coal powder according to 20% of the excess internal carbon, wherein the adding amount of fluorite in a fluxing agent is 8% of the amount of the laterite-nickel ore, and the adding amount of boric acid is 1.5% of the amount of the laterite-nickel ore. The method comprises the following steps of fully and uniformly mixing various raw materials, pressing the raw materials into blocks, fully pre-reducing the raw materials in a rotary kiln at the temperature of 1100-1200 ℃, selectively oxidizing a pre-reduced product at the temperature of 900-1100 ℃ for 30 minutes in an atmospheric atmosphere, and melting the oxidized product for 30 minutes at the temperature of 1400-1450 ℃ by a submerged arc furnace to separate slag and gold to obtain ferronickel. Through experimental analysis, the nickel and iron contents in the ferronickel product are respectively 13.56% and 81.46%, and the nickel and iron recovery rates are respectively 91.86% and 48.88%.
Example 3
Drying and crushing the laterite-nickel ore to be-5 mm, adding a reducing agent into coal powder according to 20% of the excess internal carbon, wherein the adding amount of fluorite in a fluxing agent is 15% of the amount of the laterite-nickel ore, and the adding amount of boric acid is 1.0% of the amount of the laterite-nickel ore. The method comprises the following steps of fully and uniformly mixing various raw materials, pressing the raw materials into blocks, fully pre-reducing the raw materials in a rotary kiln at the temperature of 1100-1150 ℃, selectively oxidizing the pre-reduced products at the temperature of 800-1150 ℃ for 30 minutes in the atmosphere, and melting the oxidized products for 30 minutes at the temperature of 1350-1400 ℃ through a submerged arc furnace to separate slag and gold to obtain ferronickel. Through experimental analysis, the nickel and iron contents in the ferronickel product are 14.94% and 81.2% respectively, and the nickel and iron recovery rates are 98.6% and 46.37% respectively.
In the embodiments 1, 2 and 3, the recovery rate of nickel after the pre-reduction product is oxidized is higher than 90%, the recovery rate of iron is lower than 50%, the content of nickel in the nickel iron reaches 13-15%, and the nickel is greatly improved compared with 7.96% of Ni/(Fe + Ni) in laterite-nickel ore, and the nickel metal enrichment effect is obvious.

Claims (2)

1. A method for preparing ferronickel by enriching nickel from laterite-nickel ore is characterized by comprising the following steps: uniformly mixing the crushed laterite-nickel ore with reducing agent coal powder and/or coke powder, fluxing agent fluorite powder and/or boric acid, pressing into blocks, heating in a high-temperature furnace, carrying out pre-reduction-selective oxidation, wherein the selective oxidation of a pre-reduction product is used for carrying out high-temperature oxidation on metallic iron, the oxidation temperature is 800-1200 ℃, and the time of selective oxidation is required to ensure that excessive carbon in the pre-reduction product is fully combusted; finally, obtaining ferronickel with high nickel content by a melting separation method;
the addition amount of the reducing agent must ensure that 10 to 40 percent of excessive carbon exists in the pre-reduction product while ensuring that the oxides of nickel and iron in the laterite-nickel ore are fully reduced; the adding amount of fluorite is 3-15% of the mass of the laterite-nickel ore, and the adding amount of boric acid is 0-1.5% of the mass of the laterite-nickel ore.
2. The method for preparing ferronickel by enriching nickel from lateritic nickel ores according to claim 1, characterized in that: and melting and separating the product after selective oxidation at 1350-1500 ℃ to realize full separation of slag and gold and obtain ferronickel with high nickel content.
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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101033515A (en) * 2007-04-16 2007-09-12 中南大学 Process for preparing nickel ferroalloy by melting and reducing laterite nickel ore
CN101311286A (en) * 2007-05-24 2008-11-26 万天骥 Process for producing nickel iron from low catarinite
CN101845530A (en) * 2009-03-26 2010-09-29 宝山钢铁股份有限公司 Process for producing nickel-containing iron alloy from laterite on fluidized bed
CN101942558A (en) * 2010-09-10 2011-01-12 平安鑫海资源开发有限公司 Method for drying and reducing low-grade latertic nickel ores by using bituminous coal
CN102643976A (en) * 2011-02-21 2012-08-22 宝山钢铁股份有限公司 Composite additive for producing nickel-iron particles by using laterite, and application method thereof
CN104232937A (en) * 2014-09-22 2014-12-24 中冶南方工程技术有限公司 Laterite-nickel ore selective reduction treatment method
CN105463185A (en) * 2015-04-13 2016-04-06 北海诚德镍业有限公司 Double-combined method for producing ferronickel through magnetic separation-rotary kiln electric furnace (RKEF)
CN106086469A (en) * 2016-08-09 2016-11-09 江苏省冶金设计院有限公司 A kind of method and system utilizing lateritic nickel ore to extract nickel oxide

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101033515A (en) * 2007-04-16 2007-09-12 中南大学 Process for preparing nickel ferroalloy by melting and reducing laterite nickel ore
CN101311286A (en) * 2007-05-24 2008-11-26 万天骥 Process for producing nickel iron from low catarinite
CN101845530A (en) * 2009-03-26 2010-09-29 宝山钢铁股份有限公司 Process for producing nickel-containing iron alloy from laterite on fluidized bed
CN101942558A (en) * 2010-09-10 2011-01-12 平安鑫海资源开发有限公司 Method for drying and reducing low-grade latertic nickel ores by using bituminous coal
CN102643976A (en) * 2011-02-21 2012-08-22 宝山钢铁股份有限公司 Composite additive for producing nickel-iron particles by using laterite, and application method thereof
CN104232937A (en) * 2014-09-22 2014-12-24 中冶南方工程技术有限公司 Laterite-nickel ore selective reduction treatment method
CN105463185A (en) * 2015-04-13 2016-04-06 北海诚德镍业有限公司 Double-combined method for producing ferronickel through magnetic separation-rotary kiln electric furnace (RKEF)
CN106086469A (en) * 2016-08-09 2016-11-09 江苏省冶金设计院有限公司 A kind of method and system utilizing lateritic nickel ore to extract nickel oxide

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