CN101439965A - Method for directly preparing magnetic material from nickel sulfide ore concentrate - Google Patents

Method for directly preparing magnetic material from nickel sulfide ore concentrate Download PDF

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Publication number
CN101439965A
CN101439965A CNA2008102388035A CN200810238803A CN101439965A CN 101439965 A CN101439965 A CN 101439965A CN A2008102388035 A CNA2008102388035 A CN A2008102388035A CN 200810238803 A CN200810238803 A CN 200810238803A CN 101439965 A CN101439965 A CN 101439965A
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nickel sulfide
nickel
leach liquor
magnetic material
sulfide concentrate
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CN101439965B (en
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邢献然
朱绘卉
于然波
陈骏
邓金侠
陈茜
刘桂荣
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University of Science and Technology Beijing USTB
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University of Science and Technology Beijing USTB
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Abstract

The invention discloses a method for preparing a magnetic material directly by using a nickel sulfide concentrate, which relates to the preparation of a spinel type soft magnetic ferrite material. The method makes use of a low-grade nickel sulfide concentrate as a raw material, the mass percent of nickel in the nickel sulfide concentrate is less than or equal to 10 percent, and a ferrite magnetic material is obtained through processes of oxidized roasting, hot acid leaching, impurity removal, co-precipitation, roasting and the like. The whole process does not need other mineral substances or pure substances, makes comprehensive utilization of various valuable metals in the nickel sulfide concentrate, and has the advantages of simple process, low cost, less energy consumption and small pollution, thus the method is suitable for industrial production and has wide application prospect in the field of magnetic material and the like.

Description

A kind of method with directly preparing magnetic material from nickel sulfide ore concentrate
Technical field
The present invention relates to the preparation of spinel type soft magnetic ferrite, particularly directly prepare the method for ferrite magnetic material by nickel sulfide concentrate.
Background technology
The range of application of spinel type ferrite soft magnetic materials is extremely extensive, has irreplaceable effect on products such as transformer, inducer, wave filter, deflector coil.The spinel type ferrite nano particle also has high-ratio surface, high reactivity, special physical and chemical performance, makes it to be applied to fields such as catalyzer, chemical sensor.Nickel ferrite based magnetic loaded is a kind of as the spinel type ferrite soft magnetic materials, have inverse spinel structure, by tetrahedron and octahedra the composition, wherein nickel ion all occupies octahedral interstices, then half is in octahedral interstices for ferric ion, and second half is arranged in the tetrahedron space.Exist the superexchange interaction between the intensive A-B in the nickel ferrite based magnetic loaded, compare with zinc ferrite etc., nickel ferrite based magnetic loaded has than ferromagnetism.
At present, the preparation method of nickel ferrite based magnetic loaded magneticsubstance has coprecipitation method, hydrothermal method, sol-gel method, self propagating high temperature synthesis method etc.These methods all are to be raw material with nickeliferous pure substance, and these nickel all derive from nickel ores.Because it is low that nickel sulfide ores and concentrate have grade, complicated component, the association gangue is many, belong to characteristics such as infusibility material, the production method more complicated of nickel, usually adopt matte smelting earlier, make the main metallic sulfide in the nickel ore concentrate be enriched in the low nickel matte, nickel matte is hanged down in blowing then, make wherein iron and other impurity and quartzy slag making, discharge with flue gas after part sulphur and the some other volatile impunty oxidation, thereby obtain containing valency metal (Ni, Cu, Co etc.) higher high nickel matte and contain the lower converter slag of valency metal, the converter slag that density is little floats on the upper strata and is excluded, the Ni in the high nickel matte, the Cu major part still exists with the metallic sulfide state, and small part exists with alloy state, precious metal and part cobalt in the low nickel matte also enter in the high nickel matte, and the sulfide anode electrolysis by nickel obtains electrolytic nickel at last.Perhaps high nickel matte is carried out wet processing, obtain final product nickel by electrolytic deposition or High Pressure Hydrogen reduction.These traditional technologys are very complicated, energy consumption height, and produce a large amount of waste gas, waste water and waste residue in the process, and environmental pollution is serious, and then makes that to prepare the overall craft process of nickel ferrite based magnetic loaded functional materials by pure substance many and complicated, and cost is very high.
The patent application of publication number 1126359A proposes to utilize manganese ore, iron ore and zinc ore to be the feedstock production Mn-Zn ferrite.This method finally obtains Mn-Zn ferrite by steps such as leaching simultaneously, common purification and impurity removal, co-precipitation, roasting, sintering.This method still need be allocated a certain proportion of pure substance into and replenish the metal ion of not enough proportion requirement in leach liquor.
Summary of the invention
The object of the present invention is to provide a kind of method that simply directly prepares the spinel type soft magnetic ferrite with nickel sulfide concentrate.Utilize low-grade nickel sulfide concentrate to be raw material, obtain ferrite magnetic material, do not need to allocate into again other pure substance, simplify technology, reduce and pollute, reduce cost through technologies such as oxidizing roasting, hot acid leaching, removal of impurities, co-precipitation, roastings.
Technical scheme of the present invention is:
A. selecting nickel sulfide concentrate for use is raw material, wherein the content of nickel≤10% (mass percent);
B. nickel sulfide concentrate is ground, make its uniform particles, be warming up to 700~800 ℃ of insulations with 1~5 ℃/min then and carry out roasting after 3~5 hours, obtain the raw material that next step hot acid leaches;
C. working concentration is the hydrochloric acid soln leaching of 1~4mol/l, and liquid-solid ratio is 100~500, and temperature is 90~105 ℃, reacts 3~5 hours, obtains leach liquor;
D. leach liquor is filtered, add concentration then and be 1~5 ‰ polyacrylamide flocculant, remove the silicon in the leach liquor;
E. the sodium hydroxide solution that with concentration is 1~4mol/l is heated to 90~100 ℃, add the leach liquor that purified through steps d fast, the volume ratio of sodium hydroxide solution and leach liquor is 2~1, react after 0.5~1 hour, the precipitation that produces in the reaction process is centrifugal, and be used alternatingly distilled water and absolute ethanol washing is precipitated to pH=7;
F. throw out is obtained the spinel type ferrite magneticsubstance in 800~1000 ℃ of roastings after 3~5 hours.
Compared with prior art, the invention has the advantages that:
(1) directly with the nickel sulfide concentrate be raw material, i.e. the product of nickel sulfide ore after ore dressing do not need to allocate other mineral again in the whole process or pure substance replenishes metallic element, compares with existing method, and be simpler to the requirement of raw material, reduced cost.
(2) fully utilize the multiple valuable metal element in the nickel sulfide concentrate, made full use of limited Mineral resources.
(3) compare with traditional smelting technology of nickel sulfide concentrate, technology of the present invention is simplified greatly, saves a large amount of energy, and has reduced in the process pollution to environment.
(4) with respect to the preparation method of traditional ferrite magnetic material, raw material sources of the present invention are extensive, and are cheap, and technical process is simple, and suitability for industrialized production is expected to be used widely in fields such as magneticsubstances.
Description of drawings
Fig. 1 is the X ray diffracting spectrum of the embodiment of the invention 1 prepared ferrite magneticsubstance.
Fig. 2 is the test result figure of final product magnetic property.
Embodiment
Adopting raw material is the nickel sulfide concentrate of Jinchuan company, and the content of its main component (mass percent) is Ni 6.83%, Cu3.23%, and Co 0.20%, and Fe 39.22%, SiO 210.30%, S 19.69%.
Embodiment 1:
A. take by weighing 2g and grind uniform nickel sulfide concentrate, put into alumina crucible, be warming up to 700 ℃ of insulations with 2 ℃/min and carried out roasting in 5 hours.
B. take by weighing the nickel sulfide concentrate after the 1.8005g roasting, adding 360ml concentration is the hydrochloric acid soln of 1mol/l, and temperature is 100 ℃, reacts 5 hours, obtains leach liquor.
C. leach liquor is filtered, add concentration then and be 1 ‰ polyacrylamide flocculant and remove silicon in the leach liquor.
D. the sodium hydroxide solution 100ml that gets concentration and be 1mol/l is heated to 100 ℃, adds the leach liquor 50ml that purified fast, reacts after 1 hour, and the precipitation that produces in the reaction process is centrifugal, and is used alternatingly distilled water and absolute ethanol washing is precipitated to pH=7.
E. throw out is obtained the spinel type ferrite magneticsubstance in 800 ℃ of roastings after 5 hours.This material X-ray diffraction (XRD) collection of illustrative plates is seen Fig. 1.As seen from the figure, the ferrite magnetic material purity that is directly prepared by nickel sulfide concentrate is very high.
Embodiment 2:
A. take by weighing 12g and grind uniform nickel sulfide concentrate, put into alumina crucible, be warming up to 800 ℃ of insulations with 5 ℃/min and carried out roasting in 3 hours.
B. take by weighing the nickel sulfide concentrate after the 2.5018g roasting, adding 500ml concentration is the hydrochloric acid soln of 4mol/l, and temperature is 102 ℃, reacts 3 hours, obtains leach liquor.
C. leach liquor is filtered, add concentration then and be 5 ‰ polyacrylamide flocculant and remove silicon in the leach liquor.
D. the sodium hydroxide solution 90ml that gets concentration and be 2mol/l is heated to 100 ℃, adds the leach liquor 50ml that purified fast, reacts after 1 hour, and the precipitation that produces in the reaction process is centrifugal, and is used alternatingly distilled water and absolute ethanol washing is precipitated to pH=7.
E. throw out is obtained the spinel type ferrite magneticsubstance in 1000 ℃ of roastings after 3 hours.
Fig. 2 is the test result figure of final product magnetic property, and as shown in Figure 2, product has good ferromegnetism.
Embodiment 3:
A. take by weighing 10g and grind uniform nickel sulfide concentrate, put into alumina crucible, be warming up to 750 ℃ of insulations with 5 ℃/min and carried out roasting in 4 hours.
B. take by weighing the nickel sulfide concentrate after the 2.5003g roasting, adding 500ml concentration is the hydrochloric acid soln of 2mol/l, and temperature is 100 ℃, reacts 5 hours, obtains leach liquor.
C. leach liquor is filtered, add concentration then and be 1 ‰ polyacrylamide flocculant and remove silicon in the leach liquor.
D. the sodium hydroxide solution 50ml that gets concentration and be 4mol/l is heated to 100 ℃, adds the leach liquor 50ml that purified fast, reacts after 1 hour, and the precipitation that produces in the reaction process is centrifugal, and is used alternatingly distilled water and absolute ethanol washing is precipitated to pH=7.
E. throw out is obtained the spinel type ferrite magneticsubstance in 800 ℃ of roastings after 5 hours.

Claims (2)

1, a kind of method with directly preparing magnetic material from nickel sulfide ore concentrate is characterized in that preparation process is:
A) nickel sulfide concentrate is ground, make its uniform particles, be warming up to 700~800 ℃ of insulations with 1~5 ℃/min then and carry out roasting after 3~5 hours, obtain the raw material that hot acid leaches;
B) the raw material concentration that step a) is obtained is that the hydrochloric acid soln of 1~4mol/l leaches, and liquid-solid ratio is 100~500, and temperature is 90~105 ℃, reacts 3~5 hours, obtains leach liquor;
C) leach liquor is filtered, add concentration then and be 1~5 ‰ polyacrylamide flocculant, remove the silicon in the leach liquor;
D) be that the sodium hydroxide solution of 1~4mol/l is heated to 90~100 ℃ with concentration, add the leach liquor that purified through step c) fast, the volume ratio of sodium hydroxide solution and leach liquor is 2~1, react after 0.5~1 hour, the precipitation that produces in the reaction process is centrifugal, and be used alternatingly distilled water and absolute ethanol washing is precipitated to pH=7;
E) throw out is obtained the spinel type ferrite magneticsubstance in 800~1000 ℃ of roastings after 3~5 hours.
2, the method with directly preparing magnetic material from nickel sulfide ore concentrate as claimed in claim 1 is characterized in that quality percentage composition≤10% of nickel in the described nickel sulfide concentrate.
CN2008102388035A 2008-12-03 2008-12-03 Method for directly preparing magnetic material from nickel sulfide ore concentrate Expired - Fee Related CN101439965B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103951406A (en) * 2014-04-18 2014-07-30 北京科技大学 Method for synthesizing co-doping nickel ferrite soft magnetic material by using nickel laterite ore
CN107602108A (en) * 2017-09-11 2018-01-19 中南大学 A kind of method that MnZn nickel ferrite magnetic material is prepared using low ore grade nickel resource
CN110508286A (en) * 2019-07-30 2019-11-29 北京科技大学 (Ni, Mg, Cu) Fe is prepared with nickel sulfide concentrate2O4Out-phase type Fenton catalyst and application method
CN113430368A (en) * 2021-06-10 2021-09-24 贵州理工学院 Method for preparing nickel-zinc ferrite by pressure acid leaching of sulfide ore
CN117383913A (en) * 2023-12-13 2024-01-12 河北国亮新材料股份有限公司 High-temperature-resistant iron runner castable and preparation method thereof

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100497680C (en) * 2007-01-19 2009-06-10 昆明贵金属研究所 New method for extracting nickel from enriched ore of nickel sulfide
CN101134566B (en) * 2007-09-24 2010-06-23 云南锡业集团(控股)有限责任公司 Process for preparing amino-sulfonic acid nickel by nickel sulfide concentrate

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103951406A (en) * 2014-04-18 2014-07-30 北京科技大学 Method for synthesizing co-doping nickel ferrite soft magnetic material by using nickel laterite ore
CN103951406B (en) * 2014-04-18 2015-09-09 北京科技大学 A kind of method of lateritic nickel ore synthesis codope nickel ferrite based magnetic loaded soft magnetic material
CN107602108A (en) * 2017-09-11 2018-01-19 中南大学 A kind of method that MnZn nickel ferrite magnetic material is prepared using low ore grade nickel resource
CN110508286A (en) * 2019-07-30 2019-11-29 北京科技大学 (Ni, Mg, Cu) Fe is prepared with nickel sulfide concentrate2O4Out-phase type Fenton catalyst and application method
CN113430368A (en) * 2021-06-10 2021-09-24 贵州理工学院 Method for preparing nickel-zinc ferrite by pressure acid leaching of sulfide ore
CN117383913A (en) * 2023-12-13 2024-01-12 河北国亮新材料股份有限公司 High-temperature-resistant iron runner castable and preparation method thereof
CN117383913B (en) * 2023-12-13 2024-02-06 河北国亮新材料股份有限公司 High-temperature-resistant iron runner castable and preparation method thereof

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