CN101643858A - High temperature chlorination processing method of lateritic nickel ore - Google Patents
High temperature chlorination processing method of lateritic nickel ore Download PDFInfo
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- CN101643858A CN101643858A CN200910094630A CN200910094630A CN101643858A CN 101643858 A CN101643858 A CN 101643858A CN 200910094630 A CN200910094630 A CN 200910094630A CN 200910094630 A CN200910094630 A CN 200910094630A CN 101643858 A CN101643858 A CN 101643858A
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Abstract
The invention relates to a method for high temperature chlorination and volatilization of nickel in lateritic nickel ore and collection and processing of nickel chloride in flue gas, belonging to thetechnical field of nonferrous metallurgy. The technological process of the method comprises: crushing the lateritic nickel ore, adding carbonaceous reducing agent and chlorinating agent water solutioninto the crushed lateritic nickel ore and evenly mixing together, and preparing the mixture into pellets; drying the pellets, raising the temperature inside a high temperature furnace to be the volatilization temperature of the nickel chloride, leading the nickel chloride to enter into the flue gas, washing, absorbing and dissolving the chloride in the flue gas, and obtaining solution containingthe nickel chloride; adding alkali to neutralize the nickel chloride solution, and obtaining nickel hydroxide solid and chloride waste liquid; taking the nickel hydroxide solid as the raw material forproducing nickel products, supplementing the chloride by using the chloride waste liquid, and then returning the chloride which is taken as chlorinating agent for use. The method is simple in technique, can effectively separate nickel from iron, magnesium and silicon in the lateritic nickel ore, ensures the recovery rate of nickel to reach more than 80%, and has high production efficiency and lowcost; furthermore, the chlorinating agent can be recycled, no waste water is discharged, and the method is free from environmental pollution.
Description
Affiliated technical field
The present invention relates to the method for the collection and treatment of nickelous chloride in the high-temp chlorination volatilization of nickel in a kind of red soil nickel ore and the flue gas, genus Non-ferrous Metallurgy field.
Background technology
Red soil nickel ore is the valuable source that extracts the nickel product, and the treatment process of known red soil nickel ore mainly contains pyrometallurgical smelting, wet processing and fiery wet method in conjunction with three classes.
Firing method process mainly contains retailoring ferronickel, melting nickel matte and reducing roasting---the mill choosing, disclosed technological process has: send the dry kiln drying after (1) ore reduction, send calcination rotary kiln again, under 700 ℃ of temperature, drying, preheating and calcining, the output calcining; After calcining adds electric furnace, under the temperature about 1500 ℃, add reductive agent retailoring, output Rhometal then; (2) red soil nickel ore is through fragmentation, and by a certain percentage, adding reductive agent, additive mix with laterite, system ball after drying, in metallurgical furnaces such as rotary kiln or rotary hearth furnace, tunnel furnace 950～1300 ℃ of following reducing roastings, the calcining fragmentation, through magnetic separation, gravity treatment, obtain nickeliferous 7～15% ferronickel powders; (3) add vulcanizing agent after the red soil nickel ore drying at the low nickel matte of melting output under 1500～1600 ℃ of high temperature, further obtain high nickel matte after the refining deironing again.
Wet processing mainly contains pressurized acid leaching, normal pressure stirs acidleach and dump leaching, disclosed technological process adds sulfuric acid after (1) laterite fragmentation is arranged, after the water slurryization at 250～270 ℃, leached under 4～5MPa condition 1～1.5 hour, nickel in the red soil nickel ore, brill waits valuable metal and magnesium, iron, aluminium leaches and enters solution, in the leach liquor and deironing, behind the aluminium, add sulfide precipitation output nickel cobalt sulfide, again by refining output the finished product, or leach liquor precipitation nickel hydroxide---ammonia is molten---extraction of nickel, strip liquor send nickel electrodeposition to produce cathode nickel, or adopt Cyanex272 directly to extract cobalt in the leach liquor and after the removal of impurities, raffinate extraction Ni, strip liquor send nickel electrodeposition to produce cathode nickel; (2) after the red soil nickel ore fragmentation, the red soil nickel ore that iron content is high enters autoclave pressurization leaching after adding sulfuric acid and water slurryization, after the solid-liquid separation, the pressurization leach liquor returns and adds high magnesium laterite nickel mine pulp normal pressure and leach, the normal pressure leach liquor enter molten in and after the removal of impurities, heavy nickel refining obtain the nickel product; (3) normal pressure agitation leach: after the red soil nickel ore fragmentation, add mineral acid normal pressure agitation leachs such as sulfuric acid, hydrochloric acid, leach liquor can adopt the whole bag of tricks to handle and obtain the nickel product, is that leaching agent also comprises chloride waste liquid regeneration hydrochloric acid with hydrochloric acid, with recycle hydrochloric acid, reduce acid consumption cost; (4) dump leaching: go into heap after the ore reduction, by spray liquid acidity is 5～18%, and spraying intensity is that the amount of 15～30L/m2.h sprays, and the leach liquor after collecting spray and dripping pouring is allocated, make the nickel ion concentration in the leach liquor reach 2～4g/L, get the leach liquor of nickel and cobalt containing.
The combination of fire wet method is reducing roasting mainly---ammonia soaks flow process, its technological process is the laterite drying, grinds, add reductive agent reducing roasting under 700～1000 ℃ of temperature, nickel, brill and part iron are reduced into alloy, adding ammoniacal liquor then---sal volatile leaches, ammonia still process obtains basic nickel carbonate after the leach liquor deironing, calcining obtains NiO or refining obtains metallic nickel, nickel salt, or leach liquor directly extracts Ni with LIX84-I from ammonia solution, and the sulfuric acid back extraction obtains the nickel sulfate solution electrodeposition and produces cathode nickel.Raffinate H
2The heavy cobalt of S obtains cobaltous sulfide.
There is the segregation roasting high-temp chlorination processing aspect of red soil nickel ore---and mill choosing or ammonia soak.Its process is: add a certain amount of carbonaceous reducing agent (coal or coke) and chlorizating agent (sodium-chlor or calcium chloride) in ore, in the atmosphere of neutrality or week reduction, heat, make valuable metal chlorination and become metallic particles from ore at the carbon granule surface reduction, use the method enrichment of ore dressing then, or, leach with ammoniacal liquor and sal volatile with after nickel, cobalt and part iron segregation are reduced to metal in the red soil nickel ore.Chen Xiaomin has reported that in " non-ferrous metal " (ore dressing part) the 3rd phase in 2007 with the red soil nickel ore that contains Ni1.24%, Co 0.026% be the segregation that raw material carries out---the magnetic separation test, under best integrated condition, obtained the nickel grade and be 10.33%, the rate of recovery is 87.22%, the nickel cobalt collective concentrate of cobalt grade 0.46%, the rate of recovery 80.21%.Wang Chengyan has reported employing chlorination segregation in " mining and metallurgy " 1997 the 3rd phases---ammonia soaks the red soil nickel ore of handling nickeliferous 1.24%, cobalt 0.08%, iron 24.60%, and the nickel leaching yield is 81.54% under the optimum control condition, cobalt leaching yield 55.63%.
Summary of the invention
Technical problem to be solved by this invention provides the method for the collection and treatment of nickelous chloride in the high-temp chlorination volatilization of nickel in a kind of red soil nickel ore and the flue gas.Have that technical process is short, nickel recovery is high, chlorizating agent can be recycled, with low cost, non-wastewater discharge, the characteristics of environmentally safe.
Solving the technical scheme that technical problem of the present invention adopts is: with the red soil nickel ore fragmentation, add carbonaceous reducing agent, add the chlorizating agent aqueous solution again, mix, make pelletizing; Heat up in the dry pelletizing, High Temperature Furnaces Heating Apparatus and be heated to the volatilization temperature of nickelous chloride, make nickelous chloride enter flue gas, wash with water, absorb and dissolve muriate in the flue gas, obtain containing the solution of nickelous chloride; Add in the alkali and nickel chloride solution, obtain nickel hydroxide solid and chloride waste liquid, solid nickel hydroxide is as the raw material of producing the nickel product, and chloride waste liquid returns use as chlorizating agent after replenishing muriate.
Concrete processing parameter of the present invention and method are as follows:
(1) red soil nickel ore is crushed to 40 orders, 1～10% the carbonaceous reducing agent that adds red soil nickel ore weight mixes, 20～40% the chlorizating agent aqueous solution that adds red soil nickel ore weight then, the weight of chlorizating agent is 5～20% of red soil nickel ore weight in the aqueous solution, mix, make the pelletizing of diameter 10～20mm;
(2) with pelletizing 200～300 ℃ of dryings 1～2 hour, put into High Temperature Furnaces Heating Apparatus then, be heated to 800～1200 ℃ of volatilizations 1～3 hour;
(3) solution that contains nickelous chloride adds alkali and is neutralized to PH7～8.
Described carbonaceous reducing agent is one or more of granularity 40 purpose coal dusts, coke powder, wood charcoal powder;
Described chlorizating agent is one or more in calcium chloride, sodium-chlor, hydrogenchloride, magnesium chloride, iron(ic) chloride, the ammonium chloride.
The High Temperature Furnaces Heating Apparatus that described roasting is used adopts arbitrary metallurgical furnace in rotary kiln, rotary hearth furnace, blast furnace, the blast furnace.
Described adding, adopted in lime, yellow soda ash, sodium hydroxide, ammoniacal liquor, the magnesium oxide one or more when alkali neutralization contains the aqueous solution of nickelous chloride.
The invention has the beneficial effects as follows: adopt under the high temperature nickel in the red soil nickel ore is entered flue gas with the form volatilization of nickelous chloride, again by the water washing of flue gas, the solution that dissolving is directly contained nickelous chloride, the evaporation rate of the nickel in the red soil nickel ore can reach more than 85%, iron, magnesium evaporation rate are lower than 10%, nickel recovery reaches more than 80%, the nickel recovery height, gangue good separating effects such as nickel in the laterite and iron, magnesium; Chloride waste liquid behind the heavy nickel recycles as chlorizating agent, and reagent consumption is few, and is with low cost, non-wastewater discharge, environmentally safe; Directly obtain nickel chloride solution from the volatilization flue gas, avoided processes such as mill choosing, leaching, technical process is short, and therefore the efficient height is a kind of red soil nickel ore treatment process of novelty.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Specific embodiments
Embodiment 1
Red soil nickel ore main component: Ni1.06%, Fe9.75%, MgO27.57%, granularity 40 orders.
Red soil nickel ore 100Kg, it is even that adding 5Kg is crushed to 40 purpose coal dust thorough mixing.The 6Kg chlorizating agent is dissolved in the 15Kg water, adds in the mixture of red soil nickel ore and coal dust, thorough mixing was even, makes the pelletizing of diameter 10～20mm, 200 ℃ of dryings 2 hours.
Pelletizing is put into High Temperature Furnaces Heating Apparatus, be heated to 800～850 ℃ of chloridizing volatilizations 3 hours, the slag 3.5Kg that must volatilize, main component: Ni0.20%, Fe9.68%, MgO28.15%, evaporation rate: Ni82.11%, Fe7.16%, MgO4.52%.
Flue gas washes with water, dissolves and absorbs, and adds milk of lime and sodium hydroxide and is neutralized to PH7～8, filters, obtains nickel hydroxide solid 3.1Kg after the drying, and is nickeliferous 27.54%, nickel recovery 80.32%.Heavy nickel waste liquid 15L returns use as chlorizating agent.
Embodiment 2
Red soil nickel ore main component: Ni1.06%, Fe9.75%, MgO27.57%, granularity 40 orders.
Red soil nickel ore 100Kg, it is even that adding 9Kg is crushed to 40 purpose coal dust thorough mixing.The 18Kg chlorizating agent is dissolved in the 22Kg water, adds in the mixture of red soil nickel ore and coal dust, thorough mixing was even, makes the pelletizing of diameter 10～20mm, 300 ℃ of dryings 2 hours.
Pelletizing is put into High Temperature Furnaces Heating Apparatus, be heated to 1150～1200 ℃ of chloridizing volatilizations 1 hour, the slag 3.5Kg that must volatilize, main component: Ni0.17%, Fe9.64%, MgO27.72%, evaporation rate: Ni85.27%, Fe9.84%, MgO8.32%.
Flue gas washes with water, dissolves and absorbs, and adds milk of lime and sodium hydroxide and is neutralized to PH7～8, filters, obtains nickel hydroxide solid 3.65Kg after the drying, and is nickeliferous 24.39%, nickel recovery 83.98%.Heavy nickel waste liquid 20L returns use as chlorizating agent.
Embodiment 3
Red soil nickel ore main component: Ni1.06%, Fe9.75%, MgO27.57%, granularity 40 orders.
Red soil nickel ore 100Kg, it is even that adding 1Kg is crushed to 40 purpose coal dust thorough mixing.The 12Kg chlorizating agent is dissolved in the 20Kg water, adds in the mixture of red soil nickel ore and coal dust, thorough mixing was even, makes the pelletizing of diameter 10～20mm, 250 ℃ of dryings 2 hours.
Pelletizing is put into rotary kiln, be heated to 950～1000 ℃ of chloridizing volatilizations 2 hours, must volatilize slag and 94.8Kg, main component: Ni0.14%, Fe9.90%, MgO27.13%, evaporation rate: Ni87.46%, Fe3.74%, MgO6.73%.
Flue gas washes with water, dissolves and absorbs, and adds milk of lime and sodium hydroxide and is neutralized to PH7～8, filters, obtains nickel hydroxide solid 2.9Kg after the drying, and is nickeliferous 31.52%, nickel recovery 86.23%.Heavy nickel waste liquid 21L returns use as chlorizating agent.
Embodiment 4
Red soil nickel ore main component: Ni1.06%, Fe9.75%, MgO27.57%, granularity 40 orders.
Red soil nickel ore 100Kg, it is even that adding 5Kg is crushed to 40 purpose coal dust thorough mixing.The 13Kg chlorizating agent is dissolved in the 25Kg water, adds in the mixture of red soil nickel ore and coal dust, thorough mixing was even, makes the pelletizing of diameter 10～20mm, 300 ℃ of dryings 2 hours.
Pelletizing is put into rotary kiln, be heated to 850～900 ℃ of chloridizing volatilizations 2 hours, must volatilize slag and 92.7Kg, main component: Ni0.16%, Fe9.84%, MgO27.41%, evaporation rate: Ni85.73%, Fe6.42%, MgO7.85%.
Flue gas washes with water, dissolves and absorbs, and adds milk of lime and sodium hydroxide and is neutralized to PH7～8, filters, obtains nickel hydroxide solid 3.3Kg after the drying, and is nickeliferous 26.89%, nickel recovery 83.71%.Heavy nickel waste liquid 20L returns use as chlorizating agent.
Claims (6)
1, a kind of high temperature chlorination processing method of red soil nickel ore is characterized in that technological process is: with the red soil nickel ore fragmentation, add carbonaceous reducing agent, add the chlorizating agent aqueous solution again, mix, make pelletizing; Heat up in the dry pelletizing, High Temperature Furnaces Heating Apparatus and be heated to the volatilization temperature of nickelous chloride, make nickelous chloride enter flue gas, wash with water, absorb and dissolve muriate in the flue gas, obtain containing the solution of nickelous chloride; Add in the alkali and nickel chloride solution, obtain nickel hydroxide solid and chloride waste liquid, solid nickel hydroxide is as the raw material of producing the nickel product, and chloride waste liquid returns use as chlorizating agent after replenishing muriate.
2, the high temperature chlorination processing method of red soil nickel ore according to claim 1 is characterized in that:
(1) red soil nickel ore is crushed to 40 orders, 1～10% the carbonaceous reducing agent that adds red soil nickel ore weight mixes, 20～40% the chlorizating agent aqueous solution that adds red soil nickel ore weight then, the weight of chlorizating agent is 5～20% of red soil nickel ore weight in the aqueous solution, mix, make the pelletizing of diameter 10～20mm;
(2) with pelletizing 200～300 ℃ of dryings 1～2 hour, put into High Temperature Furnaces Heating Apparatus then, be heated to 800～1200 ℃ of volatilizations 1～3 hour;
(3) solution that contains nickelous chloride adds alkali and is neutralized to PH7～8.
3, the method handled of the high-temp chlorination of red soil nickel ore according to claim 2 is characterized in that: carbonaceous reducing agent is one or more of granularity 40 purpose coal dusts, coke powder, wood charcoal powder;
4, the method for the high-temp chlorination of red soil nickel ore according to claim 2 processing, it is characterized in that: chlorizating agent is one or more in calcium chloride, sodium-chlor, hydrogenchloride, magnesium chloride, iron(ic) chloride, the ammonium chloride.
5, the method for the high-temp chlorination of red soil nickel ore according to claim 2 processing, it is characterized in that: the High Temperature Furnaces Heating Apparatus that roasting is used adopts arbitrary metallurgical furnace in rotary kiln, rotary hearth furnace, blast furnace, the blast furnace.
6, the method handled of the high-temp chlorination of red soil nickel ore according to claim 2 is characterized in that: add and adopt in lime, yellow soda ash, sodium hydroxide, ammoniacal liquor, the magnesium oxide one or more when the alkali neutralization contains the aqueous solution of nickelous chloride.
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102416288A (en) * | 2011-12-06 | 2012-04-18 | 中南大学 | Method for separating and recovering valuable metal chloride and hydrogen chloride from high-temperature chloridizing metallurgy flue gas |
| CN102936649A (en) * | 2012-11-09 | 2013-02-20 | 连云港市东茂矿业有限公司 | Method for recovering nickel, cobalt, manganese and iron by roasting and leaching nickel oxide ore |
| CN103993174A (en) * | 2014-05-23 | 2014-08-20 | 中国恩菲工程技术有限公司 | Method of precipitating nickel by using mixed base |
| CN104232882A (en) * | 2014-09-28 | 2014-12-24 | 毛黎生 | Technology for recovering nickel, cobalt and iron from nickel oxide ores through high-temperature chlorinating volatilization |
| CN105624430A (en) * | 2016-02-04 | 2016-06-01 | 马守栋 | Method for extracting nickel and cobalt from nickel laterite ore through caustic sludge and waste pickling liquid |
| CN105671305A (en) * | 2016-02-04 | 2016-06-15 | 福安市康齐动力科技有限公司 | Method for chloridizing, roasting and reducing laterite-nickel ore through bittern to prepare ferro-nickel fine powder |
| CN106282582A (en) * | 2015-05-29 | 2017-01-04 | 昆明冶金高等专科学校 | A kind of recovery non-ferrous metal, rare precious metal and method of iron powder from fume from steel making |
| CN108359812A (en) * | 2018-04-10 | 2018-08-03 | 中南大学 | A kind of low-grade complex nickel-molybdenum ore cleaning smelting process |
| CN108517408A (en) * | 2018-04-10 | 2018-09-11 | 中南大学 | A kind of low-grade complex nickel-molybdenum ore cleaning pretreatment method |
| CN110055405A (en) * | 2019-04-19 | 2019-07-26 | 长沙矿冶研究院有限责任公司 | A kind of preparation method of laterite nickel ore pellets |
| CN110079683A (en) * | 2019-04-19 | 2019-08-02 | 长沙矿冶研究院有限责任公司 | A kind of method of roasting of lateritic nickel ore pelletizing |
| CN110812888A (en) * | 2019-10-23 | 2020-02-21 | 金川集团股份有限公司 | Method for removing silicon by nickel solution adsorption |
| CN111172405A (en) * | 2020-02-27 | 2020-05-19 | 北京矿冶科技集团有限公司 | Microwave rotary hearth furnace chlorination gold extraction device and method |
| CN115821058A (en) * | 2023-02-15 | 2023-03-21 | 矿冶科技集团有限公司 | Method for extracting nickel and cobalt from laterite-nickel ore through chlorination and volatilization |
| CN117721325A (en) * | 2024-02-07 | 2024-03-19 | 矿冶科技集团有限公司 | Method for extracting nickel-cobalt-iron from laterite-nickel ore |
-
2009
- 2009-06-22 CN CN200910094630A patent/CN101643858A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102416288A (en) * | 2011-12-06 | 2012-04-18 | 中南大学 | Method for separating and recovering valuable metal chloride and hydrogen chloride from high-temperature chloridizing metallurgy flue gas |
| CN102416288B (en) * | 2011-12-06 | 2015-01-07 | 中南大学 | Method for separating and recovering valuable metal chloride and hydrogen chloride from high-temperature chloridizing metallurgy flue gas |
| CN102936649A (en) * | 2012-11-09 | 2013-02-20 | 连云港市东茂矿业有限公司 | Method for recovering nickel, cobalt, manganese and iron by roasting and leaching nickel oxide ore |
| CN103993174A (en) * | 2014-05-23 | 2014-08-20 | 中国恩菲工程技术有限公司 | Method of precipitating nickel by using mixed base |
| CN103993174B (en) * | 2014-05-23 | 2016-06-29 | 中国恩菲工程技术有限公司 | The method of mixed base coprecipitated nickel hydroxide |
| CN104232882A (en) * | 2014-09-28 | 2014-12-24 | 毛黎生 | Technology for recovering nickel, cobalt and iron from nickel oxide ores through high-temperature chlorinating volatilization |
| CN106282582A (en) * | 2015-05-29 | 2017-01-04 | 昆明冶金高等专科学校 | A kind of recovery non-ferrous metal, rare precious metal and method of iron powder from fume from steel making |
| CN105624430A (en) * | 2016-02-04 | 2016-06-01 | 马守栋 | Method for extracting nickel and cobalt from nickel laterite ore through caustic sludge and waste pickling liquid |
| CN105671305A (en) * | 2016-02-04 | 2016-06-15 | 福安市康齐动力科技有限公司 | Method for chloridizing, roasting and reducing laterite-nickel ore through bittern to prepare ferro-nickel fine powder |
| CN108517408A (en) * | 2018-04-10 | 2018-09-11 | 中南大学 | A kind of low-grade complex nickel-molybdenum ore cleaning pretreatment method |
| CN108359812A (en) * | 2018-04-10 | 2018-08-03 | 中南大学 | A kind of low-grade complex nickel-molybdenum ore cleaning smelting process |
| CN108517408B (en) * | 2018-04-10 | 2019-07-26 | 中南大学 | A kind of low-grade complex nickel-molybdenum ore cleaning pretreatment method |
| CN108359812B (en) * | 2018-04-10 | 2019-07-26 | 中南大学 | A kind of low-grade complex nickel-molybdenum ore cleaning smelting process |
| CN110055405A (en) * | 2019-04-19 | 2019-07-26 | 长沙矿冶研究院有限责任公司 | A kind of preparation method of laterite nickel ore pellets |
| CN110079683A (en) * | 2019-04-19 | 2019-08-02 | 长沙矿冶研究院有限责任公司 | A kind of method of roasting of lateritic nickel ore pelletizing |
| CN110812888A (en) * | 2019-10-23 | 2020-02-21 | 金川集团股份有限公司 | Method for removing silicon by nickel solution adsorption |
| CN111172405A (en) * | 2020-02-27 | 2020-05-19 | 北京矿冶科技集团有限公司 | Microwave rotary hearth furnace chlorination gold extraction device and method |
| CN115821058A (en) * | 2023-02-15 | 2023-03-21 | 矿冶科技集团有限公司 | Method for extracting nickel and cobalt from laterite-nickel ore through chlorination and volatilization |
| CN117721325A (en) * | 2024-02-07 | 2024-03-19 | 矿冶科技集团有限公司 | Method for extracting nickel-cobalt-iron from laterite-nickel ore |
| CN117721325B (en) * | 2024-02-07 | 2024-05-14 | 矿冶科技集团有限公司 | Method for extracting nickel-cobalt-iron from laterite-nickel ore |
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Application publication date: 20100210 |