CN103509955B - The technique of two ore deposit integrated process process red soil nickel ores and pyrolusite - Google Patents
The technique of two ore deposit integrated process process red soil nickel ores and pyrolusite Download PDFInfo
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Abstract
The present invention relates to the technique of a kind of two ore deposit integrated process process red soil nickel ores and pyrolusite, comprise the following steps: after being mixed with coal by red soil nickel ore, roasting obtains nickeliferous, the ferrous powder of cobalt oxidation; Nickeliferous, the ferrous powder of cobalt oxidation is leached with the vitriol oil; After filtration, add ammonium sulfate to solution, control H
2sO
4concentration, adds pyrolusite, by Fe
2+be oxidized to Fe
3+, Mn
4+be reduced into Mn
2+, after filtration, obtain containing MnSO
4solution and ammonium jarosite precipitation; Vulcanizing agent is added containing MnSO
4solution in, produce nickelous sulfide and cobaltous sulfide precipitation, will obtain after precipitation drying mixing nickelous sulfide, cobaltous sulfide powder; By the ammonium jarosite precipitation roasting obtained, dry after washing, obtain crude iron red.This technique can extract the valuable metal elements such as nickel, cobalt, iron, manganese from two ore deposits, and compared to processing red soil nickel ore and pyrolusite respectively, this technique has saved production cost, improves production efficiency.
Description
Technical field
The present invention relates to metalliferous mineral field of smelting, especially relate to a kind of method of Footwall drift mineral from red soil nickel ore and pyrolusite.
Background technology
At present, verify in land nickel minerals data, the industrial reserves of nickel metal is 80,000,000 tons, nickel mineral mainly exists with nickelous sulfide and red soil nickel ore two kinds of forms, wherein nickel sulfide ore accounts for 20%, red soil nickel ore is about 75%, silicic acid nickel minerals accounts for 5%, the exploitation of nickel minerals are based on nickel sulfide ore and red soil nickel ore, and main Chan Nie state is Canada, Russia, Australia, Philippines, Cuba, China.In nickel oxide ore, red soil nickel ore iron content is high, and siliceous magnesium is low, and nickeliferous is 1% ~ 2%.At present, the exploitation of nickel oxide ore are based on red soil nickel ore, and it is formed by ultrabasic rocks weathering development, and nickel mainly exists with nickel limonite (little crystallization is to non crystallized ferric oxide) form.
Because the continuous increase of nickel consumption in recent years and nickel sulfide ore reserves constantly reduce, the exploitation of red soil nickel ore comes into one's own day by day, current red soil nickel ore all adopts the mode of directly smelting raw ore, smelting process can be divided into pyrogenic process and the large class of wet method two substantially: pyrogenic process 1: primary red soil nickel ore (rotary kiln drying, electrosmelting) → ferronickel; Pyrogenic process 2: primary red soil nickel ore (sinter machine sinters, blast-furnace smelting) → Rhometal; Wet method 1: primary red soil nickel ore (adding sulfuric acid high pressure to leach) → single nickel salt (adding precipitation agent hydrogen sulfide) → nickelous sulfide (NiS); Wet method 2: the nickel in primary red soil nickel ore (also first wife burns) → ore exists (adding carbonic acid ammonia solution) → nickel hexmmine (rotary kiln drying calcining) → nickel oxide powder (reduction reaction) → metallic nickel with Rhometal structure.
Pyrogenic attack red soil nickel ore has that flow process is short, efficiency advantages of higher, but it is high to consume energy.Such as adopt electrosmelting, only power consumption just accounts for 50% of production cost, and the burning consumption of the drying before adding red soil nickel ore melting, roasting pretreatment technique, the energy consumption in running cost more accounts for more than 65%.In addition, the red soil nickel ore grade of thermal process to process has certain requirement, and ore is nickeliferous often reduces by 1%, and production cost approximately improves 30% ~ 40%, and current thermal process mainly processes high-grade red soil nickel ore.
The main technique of hydrometallurgy leaches, at present primarily of reduction-ammonia leaching process, high pressure pickling process, normal pressure pickling process and Microorganism Leaching method.Normal pressure pickling process processes red soil nickel ore at present to adopt more technique, this technique have simple to operate, consume energy low, the advantage such as do not use high-tension apparatus, investment cost few, but nickel recovery is low, seriously polluted.
Manganse Dioxide in pyrolusite is insoluble to sulfuric acid, by reduction reaction, it must be reduced into manganese monoxide (MnO), could become manganous sulfate with sulfuric acid reaction.Manganese sulfate solution is the main raw material preparing the manganese products such as industrial manganic sulfate, manganous carbonate, Manganse Dioxide, trimanganese tetroxide and electrolytic manganese.The method that manganous sulfate is prepared in present pyrolusite reduction mainly contains three kinds: coal reducing roasting---sulfuric acid leaching, two ore deposit roasting methods and wet reducing extract technology, coal reducing roasting---sulfuric acid leaching is traditional processing technology, this method has semicentennial history, it is traditional processing technology, technology maturation, the quality of manganous sulfate is good.But the SO that it is produced
2, serious dust pollution of the environment, coal consumption amount is large; Pyrolusite and manganous sulfate are pulverized by two ore deposit roasting methods respectively, mix, and 500 DEG C ~ 600 DEG C roasting temperatures 0.5 ~ 1 hour, then with clear water leaching, after being separated slag, condensing crystal obtained manganous sulfate, and the method equally also can produce SO
2and dust, contaminate environment; Wet reducing extract technology, by pyrolusite, sulfuric acid and a certain amount of reductive agent hybrid reaction, can obtain manganese sulfate solution with the water extraction regular hour at a certain temperature, and the method is the developing direction that pyrolusite leaches, and is not also applied to suitability for industrialized production.
Red soil nickel ore and pyrolusite are all the Mineral resources being difficult to utilize, and process, therefrom propose useful metalliferous mineral, then greatly can save production cost, enhance productivity if these two kinds of ore deposits can be combined.
Summary of the invention
A kind of method that the technical problem to be solved in the present invention is to avoid above-mentioned the deficiencies in the prior art part and provides combination treatment red soil nickel ore and pyrolusite, i.e. two ore deposit integrated processs, the operational path that this technique adopts fire-wet method to combine, combination treatment is carried out to red soil nickel ore and pyrolusite, therefrom extracts the valuable metal elements such as nickel, cobalt, iron, manganese.
The object of the invention is realized by following technical proposals:
A technique for two ore deposit integrated process process red soil nickel ores and pyrolusite, is characterized in that comprising the following steps:
1. mixed by a certain percentage with coal by red soil nickel ore, be ground into powder after oven dry, then carry out roasting, maturing temperature is 750 DEG C ~ 950 DEG C, and roasting time is 1 ~ 3 hour;
2. the material after roasting is ground again, obtain ferrous oxide powder that is nickeliferous, cobalt;
3. under normal temperature condition, adopt electrolytic manganese anolyte and the vitriol oil to leach nickeliferous, the ferrous powder of cobalt oxidation, sour ore deposit ratio is 0.8 ~ 1.2:1, extraction time 1.5 ~ 3 hours, controls to leach terminal H
2sO
4concentration, at 10g/L ~ 30g/L, after filtration, obtains containing FeSO
4, NiSO
4and CoSO
4solution and filter residue;
4. add ammonium sulfate to solution, add the pyrolusite grinding to form powdery, redox reaction occurs, by Fe
2+be oxidized to Fe
3+, Mn
4+be reduced into Mn
2+, after solution is filtered, obtain containing MnSO
4solution and ammonium jarosite precipitation;
5. vulcanizing agent is added containing MnSO
4solution in, produce nickelous sulfide and cobaltous sulfide precipitation, will obtain after precipitation drying mixing nickelous sulfide, cobaltous sulfide powder;
6. the ammonium jarosite precipitation roasting will obtained, maturing temperature is 950 DEG C, and the time is 2 hours, dry after washing, obtains crude iron red.
Described step 1. in the ratio of red soil nickel ore and coal be 100:16.
Described step 1. in maturing temperature be 950 DEG C, roasting time is 2 hours.
Described step 3. in ore deposit liquor ratio be 1:6 ~ 10, extraction time is 1.5 hours.
3. described step leaches terminal H
2sO
4concentration be 25g/L.
Described step 5. vulcanizing agent to be massfraction be 15% sodium sulfide solution.
To described step 5. in the filtrate that obtains add liquid SDD and carry out post cure, control temperature is at 50 DEG C.
By the crude iron that 6. arrives of step is red carries out roasting again, maturing temperature is 900 DEG C, obtains smart iron oxide red after washing and drying.
Roasting after the filter residue washing obtained after step 3. being filtered, is then separated by magnetic separation, obtains fine chrome mine.
The further deironing of the solution obtained after step 4. being filtered, adds hydrogen peroxide in solution, by remaining Fe
2+be oxidized to Fe
3+, then add ammoniacal liquor, regulate pH value between 3.5 ~ 4, controlling solution terminal pH value is 4.5, by Fe
3+become goethite precipitation and be separated.
Experimental principle of the present invention:
Prepare nickel and cobalt containing ferrous oxide powder.Take red soil nickel ore as raw material, coal dust is reductive agent, at a certain temperature Fe3+ reduction is become FeO, and nickel, cobalt are reduced into metal, thus obtained nickeliferous ferrous oxide powder (main component is FeO).Main chemical reactions equation is as follows:
2C+O
2→2CO↑(1)
Fe
2O
3+CO→2FeO+2CO
2↑(2)
NiO+CO→Ni+CO
2↑(3)
CoO+CO→Co+CO
2↑(4)
Sulfuric acid leaching.At normal temperatures, leach the nickeliferous ferrous oxide powder of pressed powder with a certain amount of vitriol oil, the heat of dilution maintenance leaching process utilizing the vitriol oil in reaction process to release completes at relatively high temperatures, thus obtains nickeliferous, cobalt, iron solution.Main chemical reactions equation is as follows:
FeO+H
2SO
4→FeSO
4+H
2O(5)
Ni+H
2SO
4→NiSO
4+H
2↑(6)
Co+H
2SO
4→CoSO
4+H
2↑(7)
Preliminary deironing.Pyrolusite main component is MnO
2, there is stronger oxidisability in acid condition, and ferrous ion has stronger reductibility.First utilize redox reaction between the two by Fe
2+be oxidized to Fe
3+, Mn
4+be reduced into Mn
2+, then under ammoniumsulphate soln system, the pH value of regulation system, adopts the Fe that ferriammonium sulfate method will be oxidized to
3+become ammonium jarosite precipitation and separate, main chemical reactions equation is as follows:
MnO
2+2FeSO
4+2H
2SO
4→MnSO
4+Fe
2(SO
4)
3+2H
2O（8）
3Fe
2(SO
4)
3+12H
2O+(NH
4)
2SO
4→(NH
4)
2Fe
6(SO
4)
4(OH)
12↓+6H
2SO
4（9）
Deep iron removal.Deep iron removal is first with the Fe of hydrogen peroxide by remnants
2+be oxidized to Fe
3+, then adopt goethite process, the pH value of the hierarchy of control, by Fe
3+become goethite precipitation and be separated, main chemical reactions equation is as follows:
2Fe
2++H
2O
2→2Fe
3++2OH
-（10）
Fe
3++3OH
-→FeOOH↓+H
2O（11）
Sulfuration separating nickel, cobalt and manganese.At normal temperatures, make nickel cobalt form precipitation by adding vulcanizing agent, thus reach the object be separated with manganese sulfate solution, main chemical reactions equation is as follows:
NiSO
4+Na
2S→NiS↓+Na
2SO
4（12）
CoSO
4+Na
2S→CoS↓+Na
2SO
4（13）
Beneficial effect of the present invention: the present invention adopts two ore deposit integrated processs to process red soil nickel ore and pyrolusite, therefrom extract the valuable metal elements such as nickel, cobalt, iron, manganese, compared to processing red soil nickel ore and pyrolusite respectively, this technique has saved production cost, improves production efficiency.The spent acid obtained after this technology utilization acidleach red soil nickel ore directly carries out leaching pyrolusite and heavy iron, substantially increases the effective rate of utilization of sulfuric acid.By this technique, red soil nickel ore and pyrolusite are processed, obtain crude iron red (can process further and obtain smart iron oxide red), mixing nickelous sulfide cobalt and manganese sulfate solution, as required manganese sulfate solution is prepared into the manganese products such as industrial manganic sulfate, manganous carbonate, Manganse Dioxide, trimanganese tetroxide and electrolytic manganese.The rate of recovery of this technique whole process nickel, cobalt, manganese, iron is respectively 90%, 73%, 91%, 90%, thus achieves the comprehensive reutilization of cobalt, nickel, manganese, each valuable metal element of iron.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of the present invention two ore deposit integrated process process red soil nickel ore and pyrolusite.
Embodiment
Adopt Philippines's red soil nickel ore and Gabon's pyrolusite to be raw material, main chemical compositions content (massfraction) as shown in Table 1.
Table one Philippines red soil nickel ore and Gabon's pyrolusite main chemical compositions content (%)
1, pyrogenic process prepares nickeliferous, the ferrous powder of cobalt oxidation
Raw material (comprising red soil nickel ore and reduction coal) is placed in electric heating constant-temperature blowing drying box, dries at 105 DEG C of temperature.Wherein red soil nickel ore requires H
2o≤10%, reduction coal dries to constant weight.(red soil nickel ore: coal=100:16) will be baked raw material and fully mix rear for subsequent use according to a certain ratio.Adopt micromill that compound is milled to certain particle size, require percent of pass >=95% under 100 mesh sieves.
Raw material after grinding is put into chamber type electric resistance furnace reducing roasting 2h, and reduction temperature is set as 750 DEG C, 850 DEG C, 950 DEG C respectively, according to Fe
3+reduction degree select best temperature condition, roasting sample analytical results is in table two.
Table two temperature condition test-results
As can be seen from table two data, along with the rising of reduction temperature, burn out rate, Fe
3+reduction degree increases successively, illustrates that high temperature is more conducive to the carrying out of reduction reaction.Known by contrasting, 750 DEG C differ nearly 70% with the reduction degree of 950 DEG C, illustrate that temperature on reduction effect impact significantly, therefore for making Fe
3+as much as possiblely be converted into Fe
2+, this process choice 950 DEG C is as optimum calcination temperature.
By red soil nickel ore and reduction coal in mass ratio 100:16 mix, at 950 DEG C of temperature, carry out reducing roasting, the time is respectively 1 hour, 2 hours, 3 hours, according to Fe
3+reduction degree select best roasting time, test-results is in table three.
Table three roasting time condition test result
Data as can be seen from table three, Fe
3+reduction degree reached maximum value at 2 hours, along with the prolongation of roasting time, Fe
3+reduction degree not only do not improve and decline to some extent on the contrary, mainly because weakening along with reducing atmosphere, this has been reduced the Fe of generation
2+oxidized generation Fe gradually again
3+, therefore this process choice conduct in 2 hours best recovery time.
Top condition according to above-mentioned test: proportioning (red soil nickel ore: reduction coal) is 100:16, maturing temperature 950 DEG C, carries out circulation ratio proof test, the results are shown in Table four at 2 hours recovery times.
Table four circulation ratio proof test result
As can be seen from Table IV, roasting test is carried out at optimum conditions, Fe
3+reduction degree about 99%, burn out rate 23.68%, nickeliferous, the ferrous powder of cobalt oxidation that obtain after roasting can meet subsequent handling requirement.
2, wet-leaching extracts each valuable metal element
The electrolytic manganese anolyte obtained after adding manganese sulfate solution electrolysis to nickeliferous, the ferrous powder of cobalt oxidation and concentration are 98% vitriol oil (analytical pure), ore deposit liquor ratio is 1:6 ~ 10, test respectively than for 1:1,1.1:1,1.2:1 by sour ore deposit, extraction time is all 1.5 hours, and table five is that test-results is compared in sour ore deposit.
Test-results is compared in the sour ore deposit of table five
Test-results shows, along with the increase of acid amount, each metal leaching rate is all in rising trend, complete under subsequent processing (deironing of leaching manganese) needs to remain on certain acidity condition in addition, spent acid very few being difficult to meets acidity needed for leaching manganese, spent acid too much can increase the consumption of neutralizing agent, to sum up considers to select best sour ore deposit than being 1.1:1.
Extraction time is tested.At temperature of reaction 55 DEG C, ore deposit liquor ratio is 1:10, and sour ore deposit is than being 1.2:1, after adding ore deposit, every 30min gets a sample, extraction time is 3 hours, investigates the changing conditions of Fe, Co, Ni and spent acid in leach liquor, (nickeliferous, the ferrous grade powder of cobalt oxidation: the Fe of this condition that the results are shown in Table six
2+: 48.21%, Co:0.14%, Ni:1.12%).
Table six extraction time test-results
As can be seen from table 3.6: after adding ore deposit, reaction reaches 1.5 hours, except Co, the leaching yield of Fe, Ni has all exceeded 93%, when extraction time reaches 2 constantly little, only have the leaching yield of cobalt to change greatly, the leaching yield of Fe, Ni is substantially unchanged, due to Co denier, from the viewpoint of the reduction energy and raising product economy benefit two, best extraction time is selected to be 1.5 hours; Control to leach terminal H
2sO
4concentration is at 10g/L ~ 30g/L.
Preliminary deironing.Adding ammonium sulfate to leaching the solution after filtering, adding the pyrolusite grinding to form powdery, redox reaction occurring, by Fe
2+be oxidized to Fe
3+, Mn
4+be reduced into Mn
2+, after solution is filtered, obtain containing MnSO
4solution and ammonium jarosite precipitation.Table seven is H
2sO
4concentration is to Mn
4+the impact of leaching yield.
Table seven H
2sO
4concentration is to Mn
4+the impact of leaching yield
As can be seen from Table VII, when initial acid is 25g/l, Mn
4+leaching yield reach 97.86%, the Fe in solution system
2+≤ 2g/L, has met successive depths deironing requirement, if by Fe in system
2+concentration is down to lower, not only can increase acid consumption, and lower concentration is unfavorable for the formation of deep iron removal crystal grain excessively, therefore selects best initial acid to be 25g/L.
To the ammonium jarosite precipitation roasting that will obtain, maturing temperature is 950 DEG C, and the time is 2 hours, dry after washing, obtains crude iron red.
Deep iron removal.The solution obtained after preliminary deironing filtration adds hydrogen peroxide, the Fe of oxidizes residual
2+, then under 85 DEG C of temperature condition, adopt goethite process to carry out deep iron removal, regulate acidity to make pH between 3.5 ~ 4.0 with ammoniacal liquor in experimentation, control solution terminal about pH=4.5, experimental result is in shown in table eight.
Table eight deep iron removal liquid analytical results
As can be seen from Table VIII, after deep iron removal, in solution, residual iron reaches trace, meets deironing requirement.
Sulfuration separating nickel, cobalt.A sulfuration: under normal temperature condition, adopt the vulcanizing agent of theoretical amount to carry out sulfuration to the solution after deep iron removal, wherein vulcanizing agent adopts concentration to be the sodium sulfide solution of 15%, filters and obtains vulcanized slag and manganese sulfate solution.Post cure: under normal temperature condition, adds SDD(Sodium dimethyldithiocarbamate 40min to the solution after a sulfuration) carry out deep impurity-removing.With qualitative without nickel for reaction end, filter and obtain qualified manganese sulfate solution.Table nine is liquid analytical results after sulfuration, and table ten is slag analytical results after sulfuration.
Liquid analytical results after table nine sulfuration
Slag analytical results after table ten sulfuration
As can be seen from manganese sulfate solution and the vulcanized slag composition analysis result of above-mentioned two table gained, nickel, cobalt, manganese separating effect are more satisfactory, both the qualified manganese sulfate solution that can meet needed for electrolytic metal Mn production had been obtained, Co, Ni in solution is made again to obtain effective enrichment, obtain the high-quality vulcanized slag of high cobalt, nickelic, low manganese, in two kinds of dissimilar vulcanized slags, Co, Ni content reaches 4.5% respectively, 29.5%(sodium sulphite sinks nickel cobalt) and 0.15%, 14%(SDD sinks nickel cobalt).
The filter residue that nickeliferous, the acid of cobalt oxidation ferrous powder obtain after entering rear filtration can also be washed by this technique, carries out magnetic separation separation again, finally can obtain fine chrome mine after roasting.Obtain manganese metal and electrolytic manganese anolyte by electrolyzing manganese sulfate solution, electrolytic manganese anolyte can be used for again leaching nickeliferous, the ferrous powder of cobalt oxidation; Manganese sulfate solution also can prepare the manganese products such as industrial manganic sulfate, manganous carbonate, Manganse Dioxide, trimanganese tetroxide as required.
Although be described in detail the present invention above in conjunction with the embodiments; but described those skilled in the art can understand, under the prerequisite not departing from present inventive concept; in claims, more can also become above-described embodiment or change etc.
Claims (8)
1. a technique for two ore deposit integrated process process red soil nickel ores and pyrolusite, is characterized in that comprising the following steps:
1. mixed by a certain percentage with coal by red soil nickel ore, be ground into powder after oven dry, then carry out roasting, maturing temperature is 750 DEG C ~ 950 DEG C, and roasting time is 1 ~ 3 hour, and the ratio of red soil nickel ore and coal is 100:16;
2. the material after roasting is ground again, obtain ferrous oxide powder that is nickeliferous, cobalt;
3. under normal temperature condition, adopt electrolytic manganese anolyte and the vitriol oil to leach nickeliferous, the ferrous powder of cobalt oxidation, sour ore deposit ratio is 0.8 ~ 1.2:1, extraction time 1.5 ~ 3 hours, controls to leach terminal H
2sO
4concentration, at 10g/L ~ 30g/L, after filtration, obtains containing FeSO
4, NiSO
4and CoSO
4solution and filter residue;
4. in solution, add ammonium sulfate, add the pyrolusite grinding to form powdery, redox reaction occurs, by Fe
2+be oxidized to Fe
3+, Mn
4+be reduced into Mn
2+, after solution is filtered, obtain containing MnSO
4solution and ammonium jarosite precipitation;
5. vulcanizing agent is added containing MnSO
4solution in, produce nickelous sulfide and cobaltous sulfide precipitation, filter, will obtain after precipitation drying mixing nickelous sulfide, cobaltous sulfide powder; Add liquid SDD to obtained filtrate and carry out post cure, control temperature is at 50 DEG C;
6. the ammonium jarosite precipitation roasting will obtained, maturing temperature is 950 DEG C, and the time is 2 hours, dry after washing, obtains crude iron red.
2. the technique of a kind of two ore deposit integrated process process red soil nickel ores according to claim 1 and pyrolusite, is characterized in that: described step 1. in maturing temperature be 950 DEG C, roasting time is 2 hours.
3. the technique of a kind of two ore deposit integrated process process red soil nickel ores according to claim 2 and pyrolusite, is characterized in that: described step 3. in ore deposit liquor ratio be 1:6 ~ 10, extraction time is 1.5 hours.
4. the technique of a kind of two ore deposit integrated process process red soil nickel ores according to claim 3 and pyrolusite, is characterized in that: 3. described step leaches terminal H
2sO
4concentration be 25g/L.
5. the technique of a kind of two ore deposit integrated process process red soil nickel ores according to claim 4 and pyrolusite, is characterized in that: described step 5. vulcanizing agent to be massfraction be 15% sodium sulfide solution.
6. the technique of a kind of two ore deposit integrated process process red soil nickel ores according to claim 5 and pyrolusite, is characterized in that: by the crude iron that 6. arrives of step is red carries out roasting again, maturing temperature is 900 DEG C, obtains smart iron oxide red after washing and drying.
7. the technique of a kind of two ore deposit integrated process process red soil nickel ores according to claim 1 and pyrolusite, is characterized in that: roasting after the filter residue washing obtained after step 3. being filtered, is then separated by magnetic separation, obtains fine chrome mine.
8. the technique of a kind of two ore deposit integrated process process red soil nickel ores according to claim 1 and pyrolusite, is characterized in that: the further deironing of the solution obtained after step 4. being filtered, adds hydrogen peroxide in solution, by remaining Fe
2+be oxidized to Fe
3+, then add ammoniacal liquor, regulate pH value between 3.5 ~ 4, controlling solution terminal pH value is 4.5, by Fe
3+become goethite precipitation and be separated.
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| CN101509072A (en) * | 2009-02-18 | 2009-08-19 | 中南大学 | Method for extracting valuable metals from laterite nickel mine with hydrochloric acid full-closed circulation method |
| CN102115816A (en) * | 2011-01-07 | 2011-07-06 | 东北大学 | Comprehensive utilization method for laterite-nickel ore |
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