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 PDFInfo
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- 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
- sulfide concentrate
- nickel
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- 239000012141 concentrate Substances 0.000 title claims abstract description 28
- WWNBZGLDODTKEM-UHFFFAOYSA-N sulfanylidenenickel Chemical compound [Ni]=S WWNBZGLDODTKEM-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000000696 magnetic material Substances 0.000 title claims abstract description 14
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 38
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 19
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 238000002386 leaching Methods 0.000 claims abstract description 8
- 238000002360 preparation method Methods 0.000 claims abstract description 5
- 239000002253 acid Substances 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 229920002401 polyacrylamide Polymers 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000010703 silicon Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims 3
- 238000001354 calcination Methods 0.000 claims 1
- 238000001914 filtration Methods 0.000 claims 1
- 238000000227 grinding Methods 0.000 claims 1
- 229910052596 spinel Inorganic materials 0.000 abstract description 11
- 239000011029 spinel Substances 0.000 abstract description 11
- 230000008569 process Effects 0.000 abstract description 8
- 239000000126 substance Substances 0.000 abstract description 8
- 229910052751 metal Inorganic materials 0.000 abstract description 5
- 238000000975 co-precipitation Methods 0.000 abstract description 4
- 239000012535 impurity Substances 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 239000011707 mineral Substances 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract 1
- 150000002739 metals Chemical class 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- NQNBVCBUOCNRFZ-UHFFFAOYSA-N nickel ferrite Chemical compound [Ni]=O.O=[Fe]O[Fe]=O NQNBVCBUOCNRFZ-UHFFFAOYSA-N 0.000 description 5
- 238000009413 insulation Methods 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 238000010792 warming Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 241000143437 Aciculosporium take Species 0.000 description 3
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 239000012467 final product Substances 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000002893 slag Substances 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- 238000003723 Smelting Methods 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 229910001308 Zinc ferrite Inorganic materials 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910001447 ferric ion Inorganic materials 0.000 description 1
- 230000005307 ferromagnetism Effects 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000000411 inducer Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 230000001902 propagating effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- -1 transformer Substances 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- WGEATSXPYVGFCC-UHFFFAOYSA-N zinc ferrite Chemical compound O=[Zn].O=[Fe]O[Fe]=O WGEATSXPYVGFCC-UHFFFAOYSA-N 0.000 description 1
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Abstract
一种用硫化镍精矿直接制备磁性材料的方法，涉及尖晶石型软磁铁氧体材料的制备。本发明利用低品位硫化镍精矿为原料，硫化镍精矿中镍的质量百分含量≤10％，经过氧化焙烧，热酸浸出，除杂，共沉淀，焙烧等工艺得到铁氧体磁性材料。整个工艺过程不需要再配入其它矿物或纯物质，综合利用了硫化镍精矿中的多种有价金属，工艺简单，成本低廉，能耗少，污染小，适宜工业化生产，在磁性材料等领域有广泛的应用前景。
The invention discloses a method for directly preparing magnetic materials from nickel sulfide concentrate, which relates to the preparation of spinel type soft magnetic ferrite materials. The invention uses low-grade nickel sulfide concentrate as raw material, and the nickel content in the nickel sulfide concentrate is less than or equal to 10%. Ferrite magnetic materials are obtained through oxidation roasting, hot acid leaching, impurity removal, co-precipitation, roasting and other processes. . The whole process does not need to be mixed with other minerals or pure substances, and a variety of valuable metals in nickel sulfide concentrate are comprehensively utilized. The process is simple, the cost is low, the energy consumption is low, the pollution is small, and it is suitable for industrial production. It is used in magnetic materials, etc. The field has broad application prospects.
Description
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)
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008102388035A CN101439965B (en) | 2008-12-03 | 2008-12-03 | Method for directly preparing magnetic material from nickel sulfide ore concentrate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008102388035A CN101439965B (en) | 2008-12-03 | 2008-12-03 | Method for directly preparing magnetic material from nickel sulfide ore concentrate |
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| Publication Number | Publication Date |
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| CN101439965A true CN101439965A (en) | 2009-05-27 |
| CN101439965B CN101439965B (en) | 2011-04-20 |
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Cited By (5)
| 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 | Preparation of (Ni, Mg, Cu) Fe2O4 Heterogeneous Fenton-like Catalyst with Nickel Sulfide Concentrate 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)
| 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 |
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2008
- 2008-12-03 CN CN2008102388035A patent/CN101439965B/en not_active Expired - Fee Related
Cited By (7)
| 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 method for synthesizing co-doped nickel ferrite soft magnetic material with laterite nickel 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 | Preparation of (Ni, Mg, Cu) Fe2O4 Heterogeneous Fenton-like Catalyst with Nickel Sulfide Concentrate 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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| CN101439965B (en) | 2011-04-20 |
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