CN105483381A - Comprehensive utilization method of nickel and iron slags - Google Patents

Comprehensive utilization method of nickel and iron slags Download PDF

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Publication number
CN105483381A
CN105483381A CN201510835842.3A CN201510835842A CN105483381A CN 105483381 A CN105483381 A CN 105483381A CN 201510835842 A CN201510835842 A CN 201510835842A CN 105483381 A CN105483381 A CN 105483381A
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China
Prior art keywords
nickel
caustic soda
slag
solution
filter
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CN201510835842.3A
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Chinese (zh)
Inventor
赵昌明
宁哲
王一雍
王国承
汪琦
艾新港
李继东
黄亮
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University of Science and Technology Liaoning USTL
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University of Science and Technology Liaoning USTL
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Priority to CN201510835842.3A priority Critical patent/CN105483381A/en
Publication of CN105483381A publication Critical patent/CN105483381A/en
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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
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • C22B7/008—Wet processes by an alkaline or ammoniacal leaching
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • 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
    • C22B23/04—Obtaining nickel or cobalt by wet processes
    • C22B23/0407—Leaching processes
    • C22B23/0446—Leaching processes with an ammoniacal liquor or with a hydroxide of an alkali or alkaline-earth metal
    • 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
    • C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
    • C22B26/20—Obtaining alkaline earth metals or magnesium
    • C22B26/22—Obtaining magnesium
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Abstract

The invention discloses a comprehensive utilization method of nickel and iron slags and aims at utilizing waste resources and protecting environment. The method comprises the following steps: crushing and roasting nickel and iron slags, and obtaining an ammonia water solution; fully dissolving roasting products by water and then filtering so as to obtain a magnesium sulfate solution and filter residues; blowing carbon dioxide gas into a sodium silicate solution and carrying out carbonation so as to obtain a sodium carbonate solution and a filter cake; washing and drying the filter cake so as to obtain a white carbon black product; adding calcium oxide into the sodium carbonate solution, and causticizing so as to obtain a caustic soda solution and calcium carbonate residues; and returning the caustic soda solution back to a filter residue leaching procedure, and calcinating the calcium carbonate residues so as to obtain calcium oxide and carbon dioxide. Through an ammonium sulfate/ ammonium bisulfate roasting-leaching technology, magnesium resources in the nickel and iron slags are recycled; iron and nickel in the enriched nickel and iron slags are leached through the alkalinity of the filter residues; and at the same time, silicon resources in the nickel and iron slags are recycled. Ammonium sulfate/ ammonium bisulfate and caustic soda are cyclically used, and no pollutants are emitted in the whole technical process.

Description

A kind of method of comprehensive utilization of ferronickel slag
Technical field
The present invention relates to the treatment process of ferroalloy slag, particularly a kind of method of comprehensive utilization of ferronickel slag.
Background technology
The solid slag that ferronickel Zha Shi Rhometal factory produces when adopting red soil nickel ore electrothermal reduction to produce ferronickel.At present, the industrial nickel of world's nickel, mainly from nickel sulfide ore resource, account for 60% of ultimate production, all the other are from red soil nickel ore.But the minimizing of nickel sulfide ore resource of easily exploiting along with high-quality (nickeliferous of high grade), the impact on the raising of environmental requirement, the progress of red soil nickel ore extractive technique and nickel price factor etc., the nickel amount of being produced by red soil nickel ore can constantly increase.Along with the continuous growth of nickel market demand, red soil nickel ore pyrometallurgical smelting is produced Rhometal scale and is progressively expanded, and the quantity discharged of smelting ferronickel from red soil nickel ore waste residue (being called for short ferronickel slag) increases gradually.Compared with other metallurgical slag, ferronickel slag valuable metal recovery is worth low, and bed drain purge is large, progressively becomes a great problem of metallurgical slag process.The common processing mode of ferronickel slag is mainly to store up and landfill.Banking up and landfill of a large amount of electrosmelting ferronickel slag, not only land occupation, contaminate environment, the Sustainable development of returning nickel-iron smelting brings severe challenge.The red soil nickel ore slag overwhelming majority is that the laterite of humic soil type produces in the technological process of electric furnace reduction melting ferronickel, its raw material and production technique are substantially identical, so the composition that different manufacturers produces electric furnace nickel-iron smelting slag is substantially identical, its main component is FeO, MgO and SiO 2, submember is Al 2o 3, Cr 2o 3, CaO etc., its main mineral composition is 2FeOSiO 2, FeOSiO 2and MgOSiO 2.For reducing the ecotope harm of red soil nickel ore slag, the research of utilization of red soil nickel ore slag is strengthened gradually with application.Because red soil nickel ore slag and blast furnace granulated slag possess similar smelting technology and physicochemical characteristic, the comprehensive utilization achievement of blast furnace granulated slag can be used for reference, replace clay, sandstone or part of cement to be used as gelling material or aggregate, prepare the products such as concrete segment, autoclaved brick, devitrified glass with red soil nickel ore slag; Utilize the feature that in red soil nickel ore slag, Mg content is high, the application of exploitation red soil nickel ore slag in refractory brick, lagging material etc.
At present, the processing mode of ferronickel slag mainly to store up and landfill, to the research of the comprehensive utilization of ferronickel slag with utilize and mainly concentrate on the aspects such as building materials raw material and mineral wool.Added value of product is low, and the usage quantity of ferronickel slag is little, and the resource such as Mg, Si, Ni, Fe in ferronickel slag cannot fully utilize.
Ferronickel slag, after being finely ground to micro mist, can being added in cement clinker and producing cement mixture.According to the requirement of silicate cement national standard, the addition of ferronickel slag is less than 8%, limits the usage quantity of ferronickel slag.As compared to metallurgical slags such as slag, blast furnace slag and ferromanganese slags, silicon in ferronickel slag, Mg content are high, calcium contents is low, wherein magnesium content is about 30% (MgO) left and right, activity index is lower than 50%, the gelling of serious restriction ferronickel slag, may there is swelling problem in the building materials causing ferronickel slag to be produced.
Summary of the invention
The invention provides a kind of method of comprehensive utilization of ferronickel slag, be intended to utilize waste resource, protection of the environment.
A method of comprehensive utilization for ferronickel slag, the method comprises the following steps:
A. ferronickel slag is crushed to below 100 orders, ferronickel slag after fragmentation mixes according to ammonium ore deposit mass ratio 1:1-6:1 with ammonium sulfate or monoammonium sulfate, roasting is carried out under 300-600 DEG C of condition, soaking time 1-4 hour, the ammonia produced in roasting process obtains ammonia soln through multistage absorption, or be pressed into liquefied ammonia, for follow-up workshop section;
B. product of roasting water fully dissolves rear filtration, obtain Adlerika and filter residue, continue to add ammoniacal liquor or liquefied ammonia in Adlerika, keep solution temperature to be 30 DEG C-75 DEG C, fully stir, until precipitation terminates after no longer producing, filter after precipitation terminates, obtain magnesium hydroxide products and filtrate, filtrate obtains ammonium sulfate or monoammonium sulfate through reduction vaporization crystallization, returns roasting workshop section and uses; Filter residue caustic soda soln leaches, caustic soda soln mass percent concentration is 20%-50%, alkali concn adds caustic soda time not enough, the solid-liquid mass ratio of filter residue and caustic soda soln is 1:2-1:8, and extraction temperature is 100 DEG C-300 DEG C, and extraction time is 0.5-2 hour, leaching terminates rear filtration, obtain sodium silicate solution and rich ferronickel slag, the chemical composition of rich ferronickel slag is mainly iron and nickel, returns ferronickel production system as raw material;
C. in sodium silicate solution, blast carbon dioxide carbon divide, controlling carbon point temperature is 50 DEG C-100 DEG C, until no longer produce precipitation, carbon filters after dividing end, obtain sodium carbonate solution and filter cake, filter cake obtains product white carbon black after washing drying, sodium carbonate solution adds calcium oxide causticization, causticization temperature is 30 DEG C-100 DEG C, abundant stirring, insulation 5-60 minute, filter after causticization and obtain caustic soda soln and calcium carbonate slag, caustic soda soln returns filter residue leaching section, calcium carbonate slag is calcined, obtain calcium oxide and carbonic acid gas, calcium oxide returns caustic room, carbonic acid gas returns Tan Fen workshop section.
The present invention compared with existing similar technique, its significantly beneficial effect be embodied in:
The present invention, by ammonium sulfate/monoammonium sulfate roasting-water logging technique, reclaims the magnesium resource in ferronickel slag; By the iron in filter residue alkaline leaching enriching nickel scum and nickel, reclaim the silicon resource in ferronickel slag simultaneously.Ammonium sulfate/monoammonium sulfate and caustic soda recycle, whole technological process non-pollutant discharge.The present invention utilizes ferronickel slag as much as possible, decreases ferronickel industrial waste slag storage, for the sustainable development of ferronickel manufacturing enterprise provides guarantee.
Accompanying drawing explanation
Fig. 1 is a kind of process flow diagram of method of comprehensive utilization of ferronickel slag.
Embodiment
More specifically the present invention is described below in conjunction with accompanying drawing embodiment.
Embodiment 1
As shown in Figure 1, a kind of method of comprehensive utilization of ferronickel slag, the step of the method is as follows:
1. check ferronickel dreg chemistry composition, result is: NiO0.16%, SiO 253.48%, Fe 2o 35.91%, CaO1.56%, MgO28.34%, Al 2o 34.62%, other are 5.93% years old;
2. ferronickel slag through broken, be finely ground to after below 100 orders, mix according to ammonium ore deposit mass ratio 4:1 with ammonium sulfate, roasting 2 hours at 400 DEG C, the ammonia water that roasting process produces absorbs, fired slags carries out solid-liquor separation, obtains magnesium sulfate filtrate and filter residue after fully dissolving with 3 times of volume water;
3. in magnesium sulfate filtrate, constantly add ammoniacal liquor, keep solution temperature to be 60 DEG C, control ph is 9, is stirred well to and no longer produces precipitation, filters, obtain magnesium hydroxide solid and filtrate to the solution after precipitation terminates.Magnesium hydroxide reaches HG/T3607-2007 industrial hydrogen magnesium oxide standard-required after drying, and filtrate obtains ammonium sulfate through reduction vaporization crystallization and returns roasting workshop section;
4. functional quality percentage concentration be 30% caustic soda soln filter residue is leached, solid-liquid mass ratio is 1:5, and extraction temperature is 200 DEG C, is incubated 1 hour, leach terminate after carry out solid-liquor separation, obtain sodium silicate solution and rich ferronickel slag.Rich ferronickel slag returns ferronickel production system;
5. blast carbon dioxide in sodium silicate solution, solution temperature is kept to be 60 DEG C, until no longer produce precipitation, solid-liquor separation is carried out after precipitation terminates, obtain sodium carbonate solution and filter cake, filter cake obtains white carbon black after washing drying, sodium carbonate solution adds calcium oxide causticization, the mass ratio of calcium oxide and sodium carbonate is 1:2, causticization temperature is 90 DEG C, abundant stirring, be incubated after 20 minutes and filter, obtain caustic soda soln and calcium carbonate slag, caustic soda soln returns filter residue leaching section, calcium carbonate slag is calcined, obtain calcium oxide and carbon dioxide, calcium oxide returns caustic room, carbonic acid gas returns Tan Fen workshop section.
Embodiment 2
As shown in Figure 1, a kind of method of comprehensive utilization of ferronickel slag, the step of the method is as follows:
1. check ferronickel dreg chemistry composition, result is: NiO0.22%, SiO 251.78%, Fe 2o 37.06%, CaO3.39%, MgO29.17%, Al 2o 32.86%, other are 5.52% years old;
2. ferronickel slag through broken, be finely ground to after below 150 orders, mix according to ammonium ore deposit mass ratio 5:1 with monoammonium sulfate, roasting 1.5 hours at 450 DEG C, the ammonia that roasting process produces is pressurized liquefied obtains liquefied ammonia, fired slags carries out solid-liquor separation after fully dissolving with 4 times of volume water, obtains magnesium sulfate filtrate and filter residue;
3. in magnesium sulfate filtrate, constantly add liquefied ammonia, keep solution temperature to be 50 DEG C, control ph is 10, is stirred well to and no longer produces precipitation.Solution after precipitation terminates is filtered, obtains magnesium hydroxide solid and filtrate.Magnesium hydroxide reaches HG/T3607-2007 industrial hydrogen magnesium oxide standard-required after drying.Filtrate obtains monoammonium sulfate through reduction vaporization crystallization and returns roasting workshop section;
4 functional quality percentage concentrations be 40% caustic soda soln filter residue is leached, solid-liquid mass ratio is 1:4, and extraction temperature is 220 DEG C, be incubated 0.5 hour, leaching terminates rear solid-liquor separation, and obtain sodium silicate solution and rich ferronickel slag, rich ferronickel slag returns ferronickel production system;
5. in sodium silicate solution, blast carbon dioxide, solution temperature is kept to be 80 DEG C, until no longer produce precipitation, solid-liquor separation is carried out after precipitation terminates, obtain sodium carbonate solution and filter cake, filter cake obtains white carbon black after washing drying, sodium carbonate solution adds calcium oxide causticization, the mass ratio of calcium oxide and sodium carbonate is 1:3, causticization temperature is 95 DEG C, abundant stirring, be incubated after 30 minutes and filter, obtain caustic soda soln and calcium carbonate slag, caustic soda soln returns filter residue leaching section, calcium carbonate slag is calcined, obtain calcium oxide and carbon dioxide, calcium oxide returns caustic room, carbonic acid gas returns Tan Fen workshop section.
Embodiment 3
As shown in Figure 1, a kind of method of comprehensive utilization of ferronickel slag, the step of the method is as follows:
1. check ferronickel dreg chemistry composition, result is: NiO0.37%, SiO 249.65%, Fe 2o 38.33%, CaO4.75%, MgO30.62%, Al 2o 33.18%, other are 3.1% years old;
2. ferronickel slag through broken, be finely ground to after below 120 orders, mix according to ammonium ore deposit mass ratio 4:1 with ammonium sulfate and monoammonium sulfate mixture, roasting 2 hours at 460 DEG C, the ammonia water that roasting process produces absorbs and obtains ammoniacal liquor, after fired slags fully dissolves with 5 times of volume water, carry out solid-liquor separation, obtain magnesium sulfate filtrate and filter residue;
3. in magnesium sulfate filtrate, constantly add liquefied ammonia, keep solution temperature to be 55 DEG C, control ph is 10, is stirred well to and no longer produces precipitation.Solution after precipitation terminates is filtered, obtain magnesium hydroxide solid and filtrate, magnesium hydroxide reaches HG/T3607-2007 industrial hydrogen magnesium oxide standard-required after drying, and filtrate obtains ammonium sulfate through reduction vaporization crystallization and monoammonium sulfate mixture returns roasting workshop section;
4. functional quality percentage concentration be 50% caustic soda soln filter residue is leached, solid-to-liquid ratio is 1:3, and extraction temperature is 200 DEG C, is incubated 0.5 hour, leach terminate rear solid-liquor separation, obtain sodium silicate solution and rich ferronickel slag.Rich ferronickel slag returns ferronickel production system;
5. in sodium silicate solution, blast carbon dioxide, solution temperature is kept to be 90 DEG C, until no longer produce precipitation, solid-liquor separation is carried out after precipitation terminates, obtain sodium carbonate solution and filter cake, filter cake obtains white carbon black after washing drying, sodium carbonate solution adds calcium oxide causticization, the mass ratio of calcium oxide and sodium carbonate is 1:2, causticization temperature is 90 DEG C, abundant stirring, be incubated after 40 minutes and filter, obtain caustic soda soln and calcium carbonate slag, caustic soda soln returns filter residue leaching section, calcium carbonate slag is calcined, obtain calcium oxide and carbon dioxide, calcium oxide returns caustic room, carbonic acid gas returns Tan Fen workshop section.

Claims (1)

1. a method of comprehensive utilization for ferronickel slag, is characterized in that the method comprises the following steps:
A. ferronickel slag is crushed to below 100 orders, ferronickel slag after fragmentation mixes according to ammonium ore deposit mass ratio 1:1-6:1 with ammonium sulfate or monoammonium sulfate, roasting is carried out under 300-600 DEG C of condition, soaking time 1-4 hour, the ammonia produced in roasting process obtains ammonia soln through multistage absorption, or be pressed into liquefied ammonia, for follow-up workshop section;
B. product of roasting water fully dissolves rear filtration, obtain Adlerika and filter residue, continue to add ammoniacal liquor or liquefied ammonia in Adlerika, keep solution temperature to be 30 DEG C-75 DEG C, fully stir, until precipitation terminates after no longer producing, filter after precipitation terminates, obtain magnesium hydroxide products and filtrate, filtrate obtains ammonium sulfate or monoammonium sulfate through reduction vaporization crystallization, returns roasting workshop section and uses; Filter residue caustic soda soln leaches, caustic soda soln mass percent concentration is 20%-50%, alkali concn adds caustic soda time not enough, the solid-liquid mass ratio of filter residue and caustic soda soln is 1:2-1:8, and extraction temperature is 100 DEG C-300 DEG C, and extraction time is 0.5-2 hour, leaching terminates rear filtration, obtain sodium silicate solution and rich ferronickel slag, the chemical composition of rich ferronickel slag is mainly iron and nickel, returns ferronickel production system as raw material;
C. in sodium silicate solution, blast carbon dioxide carbon divide, controlling carbon point temperature is 50 DEG C-100 DEG C, until no longer produce precipitation, carbon filters after dividing end, obtain sodium carbonate solution and filter cake, filter cake obtains product white carbon black after washing drying, sodium carbonate solution adds calcium oxide causticization, causticization temperature is 30 DEG C-100 DEG C, abundant stirring, insulation 5-60 minute, filter after causticization and obtain caustic soda soln and calcium carbonate slag, caustic soda soln returns filter residue leaching section, calcium carbonate slag is calcined, obtain calcium oxide and carbonic acid gas, calcium oxide returns caustic room, carbonic acid gas returns Tan Fen workshop section.
CN201510835842.3A 2015-11-26 2015-11-26 Comprehensive utilization method of nickel and iron slags Pending CN105483381A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110564973A (en) * 2019-10-24 2019-12-13 中南大学 Method for enriching magnesium from ferronickel slag by using electric pulse
CN110629015A (en) * 2019-09-11 2019-12-31 武汉理工大学 Iron olivine type slag desiliconization method
CN110713374A (en) * 2019-11-21 2020-01-21 衡阳县海华水泥有限责任公司 Ferronickel slag-based magnesium phosphate cement and preparation method thereof
WO2023016056A1 (en) * 2021-08-13 2023-02-16 广东邦普循环科技有限公司 Method for recovering magnesium oxide from ferronickel slag

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101423897A (en) * 2008-11-26 2009-05-06 东北大学 Method for extracting nickel oxide from lateritic nickel
CN101525143A (en) * 2009-01-09 2009-09-09 东北大学 Method for preparing magnesia, silicon dioxide and nickel oxide products from lateritic nickel ore
CN102080159A (en) * 2011-01-07 2011-06-01 东北大学 Method for comprehensive exploitation and utilization of silicon, magnesium, iron, and nickel in laterite-nickel ore

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101423897A (en) * 2008-11-26 2009-05-06 东北大学 Method for extracting nickel oxide from lateritic nickel
CN101525143A (en) * 2009-01-09 2009-09-09 东北大学 Method for preparing magnesia, silicon dioxide and nickel oxide products from lateritic nickel ore
CN102080159A (en) * 2011-01-07 2011-06-01 东北大学 Method for comprehensive exploitation and utilization of silicon, magnesium, iron, and nickel in laterite-nickel ore

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110629015A (en) * 2019-09-11 2019-12-31 武汉理工大学 Iron olivine type slag desiliconization method
CN110629015B (en) * 2019-09-11 2021-01-01 武汉理工大学 Iron olivine type slag desiliconization method
CN110564973A (en) * 2019-10-24 2019-12-13 中南大学 Method for enriching magnesium from ferronickel slag by using electric pulse
CN110713374A (en) * 2019-11-21 2020-01-21 衡阳县海华水泥有限责任公司 Ferronickel slag-based magnesium phosphate cement and preparation method thereof
WO2023016056A1 (en) * 2021-08-13 2023-02-16 广东邦普循环科技有限公司 Method for recovering magnesium oxide from ferronickel slag

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Application publication date: 20160413