CN1237641A - Technological process for extracting Ni, Cu, Co and Mg from nickel sulfide preparation concentrate and making nickelferrite - Google Patents
Technological process for extracting Ni, Cu, Co and Mg from nickel sulfide preparation concentrate and making nickelferrite Download PDFInfo
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- CN1237641A CN1237641A CN99108701A CN99108701A CN1237641A CN 1237641 A CN1237641 A CN 1237641A CN 99108701 A CN99108701 A CN 99108701A CN 99108701 A CN99108701 A CN 99108701A CN 1237641 A CN1237641 A CN 1237641A
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- nickel
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Abstract
The present invention includes the following steps: sulfatizing roasting nickel ore concentrate in fluidized roasting furnace, then heating, strirring and leaching-out by using sulfuric acid solution, filtering, solid-liquid separating, stoving residue, high-temp. reducing, adding calcium oxide slagging constituent, and then smelting and obtaining crude nickelferrite, then adopting the processes of soda desulfurization and converting to remove impurity so as to obtain refined nickelferrite, then using yellow sodium iron vitriol method to remove iron from leach liquor, and producing electrolytic copper, then using chlorine oxidizing process to remove cobalt, and making the cobalt slag undergo the processes of dissolution and extraction to obtain cobalt powder or cobalt oxide, then making the residual solution undergo the processes of precipitation and separation, and using the precipitated nickel carbonate to produce electrolytic nickel, using precipitated basic magnesium carbonate to produce magnesium carbonate. The total recovery of nickel and copper is up to above 97%.
Description
The present invention relates to improvement to non-ferrous metal metallurgy technologies such as nickel, copper, cobalt, magnesium.
China's nickel resources is abundant, and wherein 86% is the nickelous sulfide mineral deposit, and association has copper, cobalt, magnesium, gold and silver, sulphur and platinum metals, can be for development and use.
Smelting for nickel ore concentrate has two kinds of pyrogenic process and wet methods at present.Pyrometallurgical smelting is about to nickel ore concentrate and is smelted directly into ice nickel, make electrolytic nickel through electrolysis again, its cost height, other non-ferrous metal such as magnesium, cobalt etc. do not reclaim: hydrometallurgy has been seen report abroad, nickel ore concentrate is soaked reduction extraction nickel by the sulfurization roasting leaching or with ammonia, but the nickel leaching yield is low.
Nickel is widely used in making stainless steel, steel alloy.Along with the development of steel-smelting technology, having seen has nickel oxide ore to carry out prereduction abroad, and the technology of smelting ferronickel report replaces producing stainless steel, steel alloy with expensive electrolytic nickel, nickel block or nickel powder again.The output proportion of western developed country sintering oxidation nickel and ferronickel accounts for more than 40%, and China still utilizes electrolytic nickel, nickel block or nickel powder to produce stainless steel, steel alloy.
From looking into new result, after leaching by sulfurization roasting by nickel sulfide concentrate, soak the technology of slag melting ferronickel and do not see that both at home and abroad reported in literature is arranged.
The object of the present invention is to provide and a kind ofly can improve the rate of recovery of non-ferrous metal by extracting nickel, copper, cobalt, magnesium in the nickel sulfide concentrate and making the technology of ferronickel, reduce production costs, economic benefit obviously increases.
The present invention realizes so in conjunction with the accompanying drawings.After being leached by sulfurization roasting by nickel sulfide concentrate, soak slag and be used for smelting ferronickel, immersion liquid is used to extract nickel, copper, cobalt, magnesium.
Concrete technology is: nickel ore concentrate carries out sulfurization roasting in fluidized roaster, makes nickel contained in the washed ore, copper, cobalt etc. change water soluble sulfate into.For making the abundant oxidation of iron, reach the purpose that selectivity leaches, and be lower than the decomposition temperature of single nickel salt, roasting is in that to contain oxygen higher, is 500-700 ℃ under the lower condition of maturing temperature and carries out.Then calcining is leached with the sulphuric acid soln heated and stirred, more after filtration, make solid-liquid separation.40% nickel and other non-ferrous metal are leached, and 60% nickel is stayed and soaked in the slag.
Soak the raw material of making smelting ferronickel after the slag drying.The smelting of ferronickel is a reduction process at high temperature.Can in blast furnace, rotary kiln or electric furnace, carry out.Soaking slag carries out prereduction and adds an amount of coke powder or coal and control reduction under 900 ℃ of temperature, furnace charge contacts with the furnace gas that contains carbon monoxide, carbonic acid gas, nickel oxide becomes metallic state with iron oxide reduction, adds the calcium oxide slag former of suitable proportion, produces thick ferronickel at 1550 ℃.Adopt the soda ash desulfurization, get smart ferronickel through the blowing removal of impurities again.Smart ferronickel can be 1650 ℃ of temperature lower mold, nickeliferous 20-40%, and sulfur-bearing is less than 0.02%.
At first with the yellow sodium ferrum vanadium process deironing, scum returns sulfurization roasting in immersion liquid.Solution electrodeposition copper powder after the deironing is produced electrolytic copper.After removing cobalt with chlorine oxidation again, the cobalt slag is produced products such as cobalt powder or cobalt oxide through dissolution extraction.Solution carries out nickel, magnesium separation through two sections nickel precipitator method again.Sedimentary nickelous carbonate is produced electrolytic nickel through dissolving.Sedimentary magnesium basic carbonate is used to produce magnesiumcarbonate.Hydrometallurgic recovery copper, cobalt, nickel are moulding process, are not repeated at this.
Technology provided by the invention reaches more than 97% the total yield of nickel, copper.The melting of ferronickel reduces production costs for we have opened up a new approach, and economic benefit obviously increases.
Description of drawings:
Fig. 1 is by the process flow diagram that extracts nickel, copper, cobalt, magnesium and manufacturing ferronickel in the nickel sulfide concentrate
Embodiment: 1, make the son material with the red plate in Jilin Province pine nickel minerals, it is as follows that institute synthesizes part:
Press flow process shown in the accompanying drawing, each step process parameter is as follows: 1, sulfurization roasting-leaching
Form | Ni | ?Co | ?Cu | ?Fe | ?S | ?SiO 2 | MgO | ?CaO |
Content % | 5.53 | ?0.087 | ?1.31 | ?22.07 | ?15.47 | ?26.63 | 10.91 | ?2.41 |
90 ℃ of former ore particle of roasting granularity and extraction temperatures
680 ℃ of extraction times of maturing temperature 2 hours
Additive 4%Na
2SO
4Leached liquid-solid ratio 3: 1
Leach acidity 100g/l and leach two sections adverse currents leachings of mode
Leach the result
2, deironing
????Ni | ?Cu | ?Co | ?Fe | ?Mg | ?S | |
Immersion liquid composition g/l | ????6.46 | ????4.19 | ????0.163 | ????7.05 | ????- | ????- |
Soak slag ingredient % | ????4.30 | ????0.06 | ????0.045 | ????23.95 | ????2.32 | ????2.10 |
Leaching yield % | ????35.16 | ????96.21 | ????56.65 | ????9.62 | ????70.48 | ????- |
90 ℃ of alkali concns 7% of temperature
2 hours terminal point pH values 2.4 of churning time
Deironing rate 95.38% 3, copper removal
50 ℃ of strength of current 300A of temperature
Bath voltage 1.5-2.0V current density 120-150A/m
2
Sulfuric acid concentration 25-30g/l
Copper removal rate 98.78% electrolytic copper content 99.99%4, remove cobalt
60 ℃ of pH values 5.0 of temperature
Remove cobalt rate 96.77%5, the separation of nickel magnesium
Heavy nickel pH value 7.0 precipitation agent yellow soda ash
Heavy two sections precipitator method of magnesium pH value 11.0 separate modes
Nickel deposition rate 99.33% magnesium precipitate rate 98.20%
Nickel magnesium separation rate 99.40%6, electrolytic nickel production
Strength of current 1500-1700A catholyte pH value 3
Current density 180-204A/m
2Ni
2+Concentration>60g/l
Temperature 55-60 ℃ of Na
+Concentration≤50g/l
Bath voltage 3.5-3.8V
Electrolytic nickel content 99.99%7, smelting ferronickel
900 ℃ of sweetening agent yellow soda ash of prereduction temperature
1650 ℃ of reductive agent brown coal ingot casting temperature
1550 ℃ of slag former unslaked limes of smelting temperature
Ferronickel composition such as following table
Element | Ni | ????Cu | ????Co | ????Fe | ????S | ?C | ?P | ?Si |
Content % | 27.20 | ????0.53 | ????0.53 | ????67.94 | ????0.02 | ?0.25 | ?0.01 | ?0.11 |
Be respectively by above-mentioned technology Ni, Cu, the total rate of recovery of Co, Mg: 97.92%97.54%91.68%56.50%.The melting of ferronickel reduces production costs for we have opened up a new approach, and economic benefit obviously increases.
Claims (1)
1, a kind of by extracting nickel in the nickel sulfide concentrate, copper, cobalt, the technology of magnesium and manufacturing ferronickel, it is characterized in that nickel ore concentrate carries out sulfurization roasting in fluidized roaster, leach with the sulphuric acid soln heated and stirred then, again after filtration, make solid-liquid separation, after soaking the slag drying, reduction at high temperature, add the calcium oxide slag former, produce thick ferronickel, adopt the soda ash desulfurization at 1550 ℃, get smart ferronickel through the blowing removal of impurities again, immersion liquid is with the yellow sodium ferrum vanadium process deironing, and the solution electrodeposition copper powder after the deironing is produced electrolytic copper, remove cobalt with chlorine oxidation again after, the cobalt slag is produced cobalt powder or cobalt oxide through dissolution extraction, solution carries out nickel through two sections nickel precipitator method again, magnesium separates, and sedimentary nickelous carbonate is produced electrolytic nickel through dissolving, and sedimentary magnesium basic carbonate is used to produce magnesiumcarbonate.
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CN99108701A CN1237641A (en) | 1999-06-15 | 1999-06-15 | Technological process for extracting Ni, Cu, Co and Mg from nickel sulfide preparation concentrate and making nickelferrite |
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CN99108701A CN1237641A (en) | 1999-06-15 | 1999-06-15 | Technological process for extracting Ni, Cu, Co and Mg from nickel sulfide preparation concentrate and making nickelferrite |
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Cited By (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1300352C (en) * | 2005-09-16 | 2007-02-14 | 刘沈杰 | Nickel-iron smelting process from nickel oxide ore containing crystal water through blast furnace |
CN1306049C (en) * | 2005-09-16 | 2007-03-21 | 刘沈杰 | Ferronickel smelting process of nickel oxide ore free of crystal water in blast furnace |
CN101311281B (en) * | 2007-05-24 | 2010-05-26 | 东北大学 | Green metallurgical process for integrated utilization of nickel laterite ore |
CN101328536B (en) * | 2007-06-18 | 2010-06-02 | 中国恩菲工程技术有限公司 | Process for comprehensive recovery of nickel, copper, cobalt, sulfur and magnesium from ore |
CN102015542A (en) * | 2008-02-08 | 2011-04-13 | 维尔英科有限公司 | Process for manufacturing prefluxed metal oxide from metal hydroxide and metal carbonate precursors |
CN102268546A (en) * | 2011-07-27 | 2011-12-07 | 金川集团有限公司 | Treatment method of material containing nickel carbonate |
CN101801853B (en) * | 2007-09-21 | 2012-07-04 | 浦项产业科学研究院 | Method of manufacturing Fe and Ni containing material and cobalt containing material using recycling residue of spent catalyst and method of manufacturing raw material for stainless using the Fe and Ni containing material and method of manufacturing Fe-Ni alloy |
CN104525957A (en) * | 2014-12-07 | 2015-04-22 | 金川集团股份有限公司 | Method for preparing raw material of synthesized nickel carbonyl through residual nickel poles |
CN105392907A (en) * | 2012-07-23 | 2016-03-09 | 淡水河谷公司 | Recovery of base metals from sulphide ores and concentrates |
CN107475511A (en) * | 2017-07-14 | 2017-12-15 | 上海大学 | It is a kind of by low nickel matte calcification baking acidleach high efficiency extraction nickel, copper, cobalt method |
CN110777259A (en) * | 2019-10-23 | 2020-02-11 | 金川集团股份有限公司 | Method for pre-treating platinum group metal refining tailings to enrich precious metals by fire method |
CN111394598A (en) * | 2020-03-30 | 2020-07-10 | 龙岩紫云化学科技有限公司 | Method for extracting magnesium and co-producing calcium sulfate from magnesium-containing carbonate ore |
CN113881843A (en) * | 2021-05-31 | 2022-01-04 | 金川集团股份有限公司 | Production system and production method for reducing magnesium content in nickel concentrate |
-
1999
- 1999-06-15 CN CN99108701A patent/CN1237641A/en active Pending
Cited By (16)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1300352C (en) * | 2005-09-16 | 2007-02-14 | 刘沈杰 | Nickel-iron smelting process from nickel oxide ore containing crystal water through blast furnace |
CN1306049C (en) * | 2005-09-16 | 2007-03-21 | 刘沈杰 | Ferronickel smelting process of nickel oxide ore free of crystal water in blast furnace |
CN101311281B (en) * | 2007-05-24 | 2010-05-26 | 东北大学 | Green metallurgical process for integrated utilization of nickel laterite ore |
CN101328536B (en) * | 2007-06-18 | 2010-06-02 | 中国恩菲工程技术有限公司 | Process for comprehensive recovery of nickel, copper, cobalt, sulfur and magnesium from ore |
CN101801853B (en) * | 2007-09-21 | 2012-07-04 | 浦项产业科学研究院 | Method of manufacturing Fe and Ni containing material and cobalt containing material using recycling residue of spent catalyst and method of manufacturing raw material for stainless using the Fe and Ni containing material and method of manufacturing Fe-Ni alloy |
CN102015542A (en) * | 2008-02-08 | 2011-04-13 | 维尔英科有限公司 | Process for manufacturing prefluxed metal oxide from metal hydroxide and metal carbonate precursors |
CN102268546A (en) * | 2011-07-27 | 2011-12-07 | 金川集团有限公司 | Treatment method of material containing nickel carbonate |
CN105392907A (en) * | 2012-07-23 | 2016-03-09 | 淡水河谷公司 | Recovery of base metals from sulphide ores and concentrates |
CN104525957A (en) * | 2014-12-07 | 2015-04-22 | 金川集团股份有限公司 | Method for preparing raw material of synthesized nickel carbonyl through residual nickel poles |
CN104525957B (en) * | 2014-12-07 | 2016-05-18 | 金川集团股份有限公司 | A kind of method of utilizing nickel anode scrap to prepare synthesizing carbonyl nickel raw material |
CN107475511A (en) * | 2017-07-14 | 2017-12-15 | 上海大学 | It is a kind of by low nickel matte calcification baking acidleach high efficiency extraction nickel, copper, cobalt method |
CN107475511B (en) * | 2017-07-14 | 2019-07-23 | 上海大学 | A method of by low nickel matte calcification baking-acidleach high efficiency extraction nickel, copper, cobalt |
CN110777259A (en) * | 2019-10-23 | 2020-02-11 | 金川集团股份有限公司 | Method for pre-treating platinum group metal refining tailings to enrich precious metals by fire method |
CN111394598A (en) * | 2020-03-30 | 2020-07-10 | 龙岩紫云化学科技有限公司 | Method for extracting magnesium and co-producing calcium sulfate from magnesium-containing carbonate ore |
CN113881843A (en) * | 2021-05-31 | 2022-01-04 | 金川集团股份有限公司 | Production system and production method for reducing magnesium content in nickel concentrate |
CN113881843B (en) * | 2021-05-31 | 2024-03-22 | 金川集团股份有限公司 | Production system and production method for reducing magnesium content in nickel concentrate |
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