CN103074493A - Application of brucite to recovery of nickel cobalt - Google Patents
Application of brucite to recovery of nickel cobalt Download PDFInfo
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- CN103074493A CN103074493A CN2013100541686A CN201310054168A CN103074493A CN 103074493 A CN103074493 A CN 103074493A CN 2013100541686 A CN2013100541686 A CN 2013100541686A CN 201310054168 A CN201310054168 A CN 201310054168A CN 103074493 A CN103074493 A CN 103074493A
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Abstract
The invention relates to application of brucite to the recovery of nickel cobalt in nickel laterite ore wet method smelting. The brucite directly serves as a neutralizer to replace lime and is applied to a purification impurity-removing process of laterite-nickel ore leaching liquid or leaching pulp. The calcinated brucite serves as the neutralizer to replace sodium hydroxide or the lime and is applied to a nickel precipitation process of a nickel-containing solution. The application of brucite powder which replaces the lime to the purification impurity-removing process of nickel cobalt recovery in the laterite-nickel ore wet metallurgy has the advantages of small residue quantity and environmental friendliness, calcination is not required, and greenhouse gas such as carbon dioxide cannot be emitted. The application of the calcinated brucite to the nickel precipitation process of the nickel cobalt recovery in laterite-nickel ore wet metallurgy has the same effect as sodium hydroxide and lime milk. Compared with the sodium hydroxide, the calcinated brucite is low in cost. Compared with the lime milk, the calcinated brucite has the advantages that gypsum waste residues can be avoided; a process of separating nickel hydroxide from gypsum in a subsequent process is eliminated; and the defects of lime using, such as large residue quantity, large water consumption, and blocking of a process pipe network caused by scaling of calcium sulphate, are solved.
Description
Technical field
The present invention relates to the technology that brucite is used for reclaiming from red soil nickel ore acidleach system the nickel cobalt.
Background technology
Existing red soil nickel ore wet method is carried in the nickel technology the main acid leaching process that adopts and is leached nickel cobalt metal in the ore, no matter be to adopt pressure leaching, normal pressure to leach or dump leaching, usually use sulfuric acid as soaking the ore deposit agent, soak nickel in the process ore of ore deposit, when cobalt is leached, the impurity such as iron, copper, zinc, chromium, manganese also are dissolved, and follow-uply need to carry out to remove impurity by means of precipitation to nickeliferous leach liquor.In the prior art, leach liquor or leaching ore pulp are to come the impurity such as precipitated iron, copper, zinc, chromium, manganese by adding the pH value of adding limestone slurry or lime slurry neutralization and the solution that raises.Make the neutralizing agent cleaner with lime and have cheapness, easily obtain, advantage easily.But also have obvious shortcoming, precipitation process lime and sulfuric acid reaction generate insoluble gypsum product, and it is excessive to cause producing the quantity of slag, and water loss is large, and main metallic nickel recovery of Co rate is low.
Ca(OH)
2+H
2SO
4＝CaSO
4·2H
2O↓
CaCO
3+ H
2SO
4+ H
2O=CaSO
42H
2O ↓+CO
2↑ process produces a large amount of sediments
Resultant also is wrapped in the surface of lime, causes the utilization ratio of neutralizing agent lime low, produces that the quantity of slag is large, the difficult washing of slag, nickel and cobalt recovery rate are low etc.In addition, calcium sulfate also has disadvantageous effect to production operation, and calcium sulfate easily produces fouling, causes obstruction etc. that at processing pipe network, pump valve and even equipment (such as thickener etc.) trouble that causes also is well-known.
Along with the development of environmental protection cause, the cry of economizing on water, subtract slag grows to even greater heights since 21 century, and the requirement that enterprise reduces production costs and pressure increase! Therefore, the knowledgeable people has proposed to replace in the calcium work and cleaner with magnesium both at home and abroad, to reach the purpose that subtracts the slag water saving.In doing with magnesium and the reaction of cleaner have:
MgO+H
2SO
4=MgSO
4+ H
2O does not produce sediment, and utilization ratio is high!
The slag effect that subtracts with cleaner in clearly doing with magnesium oxide is obvious.
And magnesian alkalescence is not strong, and its concentration can be much higher than lime milk concentration during use, can reduce water consumption and wastewater treatment capacity, the nickel concentration before the heavy nickel of raising in the liquid etc.
Magnesium is that neutralizing agent is used for the case that red soil nickel ore reclaims the patent application of nickel cobalt and has much.
Just use in the magnesium oxide slurries and raffinate the WO2006/069416CN101094926A " extracting nickel and cobalt from resin eluate " by name.
MgO, Mg (OH) have just been used among the WO2007/035978CN101273146A " method of normal pressure acidleach laterite ore " by name
2And MgCO
3Use neutralizing agent, in this patent, described MgO, Mg (OH)
2, MgCO
3MgO, the Mg (OH) that is generated by sal epsom reduction calcining
2And MgCO
3
The described magnesium oxide neutralizing agent of patent of WO2009/146518A1 " reclaiming magnesium and sulphur in leaching red soil nickel ore " by name is the same with WO2007/035978, is the magnesium oxide that is made by the sal epsom thermolysis.
But be that the magnesium oxide product of purchase or the magnesium oxide cost that the recovery of scheme process makes are all higher.
Disclosing this patent of CN200910113991.3 " from the method for red soil nickel ore recovery nickel cobalt, magnesium, iron and silicon " by name uses magnesite powder to make the technical scheme of neutralizing agent, described magnesite powder is a kind of undressed natural magnesium magnesium mineral, in fact, magnesite powder as neutralizing agent use with the process of acid-respons in can produce great amount of carbon dioxide gas and foam, affect the carrying out of actually operating.
Summary of the invention
Be directed to the defective that exists in the prior art, the invention provides a kind of in the laterite nickel ore by sulfuric acid leaching system not the extra waste residue of output, do not produce carbon dioxide greenhouse gas, do not stop up processing pipe network, cheap, environment amenable neutralizing agent.
Brucite of the present invention, mean by natural water magnesium ore, industrial, brucite is mainly for the production of purposes such as magnesite refractory, fire retardant, papermaking, chemical industry, building materials, rubber, potteries, and the present invention uses it for a kind of new purposes---from the laterite nickel ore by sulfuric acid leaching system, reclaim the nickel cobalt.With the magnesium oxide that the sal epsom processing treatment is obtained, and be different by industrial magnesium oxide, the magnesium hydroxide that sell in the chemical plant, indication brucite of the present invention is a kind of cheap mineral substance that contains the magnesium hydroxide composition that is easy to get.
The objective of the invention is to realize according to following scheme:
Brucite is used for the purposes that the red soil nickel ore hydrometallurgy reclaims the nickel cobalt, and described brucite is the natural brucite mineral, and its major ingredient is magnesium hydroxide.
According to above-mentioned purposes, concrete usage is: with the brucite mineral of exploitation through broken, replace Wingdale or milk of lime as neutralizing agent after being finely ground to powder, be used for red soil nickel ore after acidleach leach liquor or leach the purification and impurity removal process of ore pulp.
Described red soil nickel ore acidleach method comprises normal pressure acidleach, pressurized acid leaching and dump leaching, and described purification and impurity removal process comprises the used neutralizing agent of removal of impurities process for yellow modumite method, jarosite process, ammonium jarosite method, goethite process, hydronium(ion) oxidation iron processes.
Brucite also can be used as the heavy nickel agent of solution containing nickel, but the alkalescence of brucite a little less than, can not directly be used as the heavy nickel agent of solution containing nickel, need to become magnesium oxide to improve activity through calcination processing, thermogravimetric analysis figure (seeing Figure of description 2) according to brucite, the loss of weight of brucite begins under 330 ℃ greatly, slows down to 750 ℃ of weightlessness.Therefore, the decomposition temperature of brucite is 450 ℃～800 ℃, the too high or too low chemically reactive that will lower the calcining after product of calcining temperature.Concrete way is: brucite mineral is broken, be milled down to granularity less than 0.14mm, and be 450 ℃～800 ℃ through excess temperature, after processing in 1～10 hour, calcination as neutralizing agent, replace sodium hydroxide or milk of lime as the heavy nickel agent of solution containing nickel.The process reaction formula is:
MgO+Ni
2++H
2O＝Mg
2++Ni(OH)
2↓
Beneficial effect of the present invention: the present invention use brucite powder replace traditional limestone powder or milk of lime be used for purification and impurity removal process that the red soil nickel ore hydrometallurgy reclaims the nickel cobalt have the quantity of slag of producing little, need not calcining, without carbon dioxide greenhouse gas emit, environment amenable advantage; Brucite is used for the heavy nickel precipitate and separate enrichment process that the red soil nickel ore hydrometallurgy reclaims the nickel cobalt after using calcining, effect and sodium hydroxide and milk of lime are suitable, have cheap advantage but compare with sodium hydroxide, compare with milk of lime and have the process that produces and avoided nickel hydroxide and Separation of gypsum in the subsequent handling without gypsum offscum.In addition, in and in removal of impurities and the heavy nickel process brucite or burnt brucite all can directly add powder and not need the pulp process, simple to operate, and can avoid in the pulp process water yield in system, introduced.
Description of drawings
Fig. 1 is that brucite is used for the process flow sheet that red soil nickel ore reclaims the nickel cobalt.
Fig. 2 is brucite thermogravimetric analysis figure.
Embodiment
Hydrometallurgic recovery nickel cobalt generally is to adopt acid leaching process from red soil nickel ore, described acid leaching process comprises that normal pressure stirs acidleach, pressurized acid leaching and dump leaching, use is cheap, the ore deposit agent is soaked in less demanding sulfuric acid conduct to equipment anticorrosion, ore pulp after red soil nickel ore leaches or the solution that contains the nickel cobalt need to carry out preliminary removal of impurities to be processed, remove those undesired metallic impurity such as iron etc. in the solution, the method of deironing has yellow modumite method, jarosite process, ammonium jarosite method, goethite process, hydronium(ion) oxidation iron processes etc., in the hydrometallurgy field, these all are known technology.Yet in iron removal, reaction can discharge sulfuric acid, can proceed in order to make the deironing reaction, need to neutralize the unnecessary sulfuric acid that this discharges, usually use lime as the spent acid neutralizing agent in the prior art, and lime and sulfuric acid reaction are understood the extra gypsum tailings of output, have namely increased the treatment capacity of technological process ore pulp, can cause again the loss of nickel cobalt in slag to increase.And use brucite powder of the present invention just can avoid these problems, at this, brucite powder is the sulfuric acid as it is unnecessary that alkaline matter neutralizes, brucite powder is adjustable, and one-tenth slurry mode adds, also can the dry powder mode add, magnesium hydroxide alkalescence in the brucite a little less than, can not cause partial over-alkali and precipitate the nickel cobalt ion of loss in the solution, compare with milk of lime and have obvious advantage.In addition, the reaction process of brucite powder and sulfuric acid can the extra waste residue of output, thereby utilization ratio is high, and the sal epsom that forms after the dissolving can be by follow-up operation recovery, and the add-on of brucite powder is decided on the regulation of processing requirement in the concrete method for removing iron.
Embodiment 1
The solution containing nickel of a kind of red soil nickel ore after the sulfuric acid dump leaching, composition sees Table 1.
Table 1. heap leaching solution component list (g/L)
| Element | Ni | Fe | Al | SiO 2 | Cr | pH |
| Content | 6.49 | 5.87 | 1.56 | 0.23 | 0.19 | 1.1 |
Employed brucite mineral major ingredient is: Mg (OH)
297.2%, SiO
20.8%, Fe0.15%.Furnishing slurry behind the brucite mineral mill is processed for the purification and impurity removal of solution containing nickel after the dump leaching as neutralizing agent, and removal of impurities adopts goethite process to carry out, and temperature of reaction is 90 ℃, time 2 h filters after the reaction, and slag liquid separates, under equal conditions do simultaneous test with lime simultaneously, impurity-eliminating effect sees Table 2.
Material component table behind table 2. purification and impurity removal
The calculation result of purification and impurity removal process water magnesite consumption and nickel recovery sees Table 3.
The consumption of table 3. brucite and the rate of recovery
From top data as seen, brucite obviously is better than using lime for the purification and impurity removal process of red soil nickel ore acid dip solution.
Embodiment 2
Ore pulp behind a kind of red soil nickel ore process normal pressure sulfuric acid leaching, composition sees Table 4.
Table 4. ore pulp compositional data table
Brucite mineral is levigate rear as neutralizing agent, directly carrying out iron purification for the ore pulp behind the normal pressure sulfuric acid leaching processes, deironing adopts yellow modumite method to carry out, brucite mineral directly adds ore pulp in the dry powder mode, and temperature of reaction is 95 ℃, 3 hours time, filter after the reaction, slag liquid separates, and under equal conditions does simultaneous test with lime simultaneously, and impurity-eliminating effect sees Table 5
Material component table behind table 5 purification and impurity removal
Data from table as seen, the ore pulp purification and impurity removal process that brucite is used for after the red soil nickel ore acidleach obviously is better than using lime.
Brucite can also be as the heavy nickel agent of solution containing nickel, but the alkalescence of brucite a little less than, can not directly be used as the heavy nickel agent of solution containing nickel, need to become magnesium oxide to improve chemically reactive through calcination processing, concrete way is: brucite mineral is broken, be milled down to granularity less than 0.14mm, be 450～800 ℃ through excess temperature, as neutralizing agent, replace sodium hydroxide or milk of lime as the heavy nickel agent of solution containing nickel after calcination was processed in 1～10 hour.
Embodiment 3～5 (one section heavy nickel)
With composition be: Mg (OH)
297.2%, SiO
2The brucite concentrate of 0.8%, Fe0.15% is worn into the powder of 0.043mm granularity, then brucite powder is done calcination processing, and calcination condition and result data see Table 6.
Table 6. brucite breeze calcination processing data sheet
Table 7. solution containing nickel compositional data table (g/L of unit)
| Ni | Mg | Mn | Ca | The pH value |
| 3.38 | 23.53 | 0.73 | 0.23 | 4.68 |
Respectively 1 liter of composition solution containing nickel as shown in table 7 is packed in the glass beaker, solution temperature is 50 ℃ in heating and the maintenance glass beaker, brucite powder after under agitation condition powder being forged slowly adds separately, nickel ion in the neutralization precipitation solution, until the pH of solution stabilizes to 7.8, draw the gross weight that consumes powder, with the nickel hydroxide precipitate thing analysis total nickel amount wherein that obtains, the gross weight that consumes powder is namely drawn the consumption (precipitating the powder weight that every gram nickel consumes) of powder in the table 1 divided by total nickel amount, will also list in the table 8 with the heavy nickel Experimental Comparison example data that sodium hydroxide is done by the same terms simultaneously.
One section heavy nickel test-results data sheet of table 8.
Brucite powder consumption during one section heavy nickel is tested after the calcining and the result data of the rate of recovery see Table 9
Brucite powder consumption and rate of recovery data sheet after table 9. calcining
From top data as seen, the brucite powder after the calcining is used for the heavy nickel process of solution containing nickel and compare the effect difference with sodium hydroxide little, but consumption lacks than sodium hydroxide.
Embodiment 6 (two sections heavy nickel)
Brucite powder after the calcining also can be used for two sections heavy nickel processes, filtrate (composition sees Table 10) behind one section heavy nickel is being kept 45 ℃, when constantly stirring, brucite powder after slowly low adding is calcined, the pH value of solution rises to about pH8.8 from about 7.8, and about half an hour of steady time, filter, to be 5% NaOH as precipitation agent contrast sees Table 11 and table 12 for the composition of filtrate and filter residue and massfraction.
Filtrate constituent data (g/L) behind one section heavy nickel of table 10
| Element | pH | Ni | Mg | Mn | Ca |
| Content | 7.8 | 0.18 | 18.07 | 0.045 | 0.23 |
Two sections heavy nickel rear filtrate compositional datas of table 11 (g/L)
| Element | pH | Ni | Mg | Mn | Ca |
| Brucite calcining powder | 8.73 | 0.0015 | 18.75 | 0.005 | 0.30 |
| NaOH | 8.79 | 0.0020 | 18.50 | 0.0005 | 0.26 |
Two sections heavy nickel slag ingredient data of table 12 (%)
| Element | Ni | Mg | Mn | Ca |
| Brucite calcining powder | 20.36 | 15.35 | 8.08 | 0.32 |
| NaOH | 20.17 | 15.10 | 8.99 | 0.10 |
Adopt brucite calcining powder and sodium hydroxide gained nickel hydroxide dry weight basically identical, from above data as can be known, the suitable deposition rate with the sodium hydroxide sedimentation effect of brucite calcining powder is about 98.5%, low because of Ni, contain the magnesium height can directly return in and removal step as neutralizing agent and again dissolve wherein nickel.
The molar weight that nickel per ton consumes brucite is about 1/2 of sodium hydroxide, and namely the heavy nickel process of secondary precipitates 2.52 tons of natural brucites of nickel consumption per ton, 5.05 tons of solid sodium hydroxides.
Claims (5)
1. brucite is used for the purposes that the red soil nickel ore hydrometallurgy reclaims the nickel cobalt, and described brucite is the natural brucite mineral, and its major ingredient is magnesium hydroxide.
2. purposes according to claim 1, described brucite as neutralizing agent, are used for the leach liquor after the red soil nickel ore acidleach or leach the purification and impurity removal process of ore pulp after broken, levigate.
3. purposes according to claim 2, described red soil nickel ore acidleach method includes normal pressure acidleach, pressurized acid leaching and dump leaching, and described purifying and impurity-removing method includes the removal of impurities process of yellow modumite method, jarosite process, ammonium jarosite method, goethite process, hydronium(ion) oxidation iron processes.
4. purposes according to claim 1, described brucite as neutralizing agent, is used for the heavy nickel process of solution containing nickel after purifying after broken, levigate, calcination are processed.
5. method according to claim 4, described brucite is milled down to granularity less than 0.14mm, and the calcination treatment temp is 450～800 ℃, and the calcination time is 1～10 hour.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103993175A (en) * | 2014-05-23 | 2014-08-20 | 中国恩菲工程技术有限公司 | Method for treating cobalt nickel sulfate solution |
| CN106086409A (en) * | 2016-08-03 | 2016-11-09 | 中国恩菲工程技术有限公司 | The method of liquid after the heavy nickel cobalt of process |
| CN103993175B (en) * | 2014-05-23 | 2016-11-30 | 中国恩菲工程技术有限公司 | The processing method of nickel sulfate cobalt liquor |
| CN107400788A (en) * | 2017-07-18 | 2017-11-28 | 中国恩菲工程技术有限公司 | The method that nickel cobalt is precipitated in laterite nickel ore hydrometallurgical |
| CN109234526A (en) * | 2018-11-26 | 2019-01-18 | 中国恩菲工程技术有限公司 | The processing method of lateritic nickel ore |
| CN111422928A (en) * | 2020-04-13 | 2020-07-17 | 广西赛可昱新材料科技有限公司 | Nickel deposition method without impurity brought in laterite-nickel ore leaching solution |
| GR1010450B (en) * | 2022-06-04 | 2023-04-28 | Ηλιας Θεολογου Σταμπολιαδης | Method of recovery of nickel-cobalt condensate from poor ferronickel lateric ores |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103993175A (en) * | 2014-05-23 | 2014-08-20 | 中国恩菲工程技术有限公司 | Method for treating cobalt nickel sulfate solution |
| CN103993175B (en) * | 2014-05-23 | 2016-11-30 | 中国恩菲工程技术有限公司 | The processing method of nickel sulfate cobalt liquor |
| CN106086409A (en) * | 2016-08-03 | 2016-11-09 | 中国恩菲工程技术有限公司 | The method of liquid after the heavy nickel cobalt of process |
| CN106086409B (en) * | 2016-08-03 | 2018-05-11 | 中国恩菲工程技术有限公司 | The method of liquid after the heavy nickel cobalt of processing |
| CN107400788A (en) * | 2017-07-18 | 2017-11-28 | 中国恩菲工程技术有限公司 | The method that nickel cobalt is precipitated in laterite nickel ore hydrometallurgical |
| CN109234526A (en) * | 2018-11-26 | 2019-01-18 | 中国恩菲工程技术有限公司 | The processing method of lateritic nickel ore |
| CN111422928A (en) * | 2020-04-13 | 2020-07-17 | 广西赛可昱新材料科技有限公司 | Nickel deposition method without impurity brought in laterite-nickel ore leaching solution |
| GR1010450B (en) * | 2022-06-04 | 2023-04-28 | Ηλιας Θεολογου Σταμπολιαδης | Method of recovery of nickel-cobalt condensate from poor ferronickel lateric ores |
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Application publication date: 20130501 |