CN104278151A - High-concentration-alkali-leaching comprehensive utilization process for laterite-nickel ore - Google Patents
High-concentration-alkali-leaching comprehensive utilization process for laterite-nickel ore Download PDFInfo
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Abstract
The invention relates to a high-concentration-alkali-leaching comprehensive utilization process for laterite-nickel ore. According to the process, processes for high-added-value environment-friendly comprehensive utilization of the laterite-nickel ore are researched. Through analyzing the composition and material phase of the laterite-nickel ore raw material, process flows of preparing a silicon dioxide product by laterite-nickel ore alkali-method treated silicon leaching, preparing magnesium carbonate and magnesium oxide products by desilication residue carbonized magnesium leaching and preparing a nickel oxide product by carbonized residue ammonia nickel leaching are designed. According to the process, no waste gas, waste water or waste residue is discharged, and the cyclic utilization of chemical raw materials is realized, so that the process is a green and environment-friendly novel process for comprehensive resource utilization and meets the requirements of national development on circular economy.
Description
Technical field
The present invention relates to red soil nickel ore field, a kind of red soil nickel ore high concentration alkali leaching comprehensive utilization process.
Background technology
Along with society is to the requirement of protection of the environment, industrial production more and more payes attention to the pollution that its production process causes, thus seeks environment amenable technical process by every means, develops a circular economy just to the preferably response of this problem.And how to make the Mineral resources day by day reduced be utilized, be also an importance of Sustainable development.
Nickel is the metal of most worthy in red soil nickel ore, is the target product in traditional technology.But because in red soil nickel ore, the content of nickel is low, thus can produce a large amount of slag dump and abandon in nickel fibers process, land occupation, contaminate environment.On the other hand, containing a large amount of britesorb mineral, rhombohedral iron ore etc. in red soil nickel ore, products such as can preparing silicon, magnesium, iron is made full use of to it, both red soil nickel ore high value added utilization had been improved, the discharge of waste can be reduced again, the requirement meeting recycling economy, cleaner production and improve mineral resources comprehensive utilization rate.
The present invention is directed to the present situation that red soil nickel ore fails rationally to process, carry out the research of red soil nickel ore high value-added greening comprehensive utilization process, the silicon adopting alkaline leaching to extract in red soil nickel ore prepares silica product; The desiliconization slag employing carborization obtained is carried magnesium and is prepared magnesium oxide product; Finally carbide slag ammonia leaching nickel is prepared nickel oxide product; Residue slag is directly used as iron-smelting raw material or deep processing becomes iron oxide red product.This technique is applicable to the various red soil nickel ore of process, the material accounting for red soil nickel ore total content 99% is made to obtain utilization, and prepared various Chemicals, reach the utilization that becomes more meticulous, in technological process, industrial chemicals all realizes circulation, without waste residue, waste water, exhaust gas emission, realizes full-range greenization, meet and develop a circular economy, the requirement of Resources for construction saving type and friendly environment society.
Summary of the invention
For the deficiencies in the prior art, an object of the present invention is to provide a kind of red soil nickel ore high concentration alkali to soak comprehensive utilization process.Described technique is studied the technique that red soil nickel ore high value-added greening fully utilizes.By to the composition of red soil nickel ore raw material and the analysis of thing phase, devise the process of red soil nickel ore alkaline process and carry silicon and prepare silica product, desiliconization slag carbonization is carried magnesium and is prepared magnesiumcarbonate and magnesium oxide product, and carbide slag ammonia leaching nickel prepares the technical process of nickel oxide product.Without the discharge of waste gas, waste water, waste residue in this technological process, and achieve the recycle of industrial chemicals, be the comprehensive utilization of resources novel process of an environmental protection, meet the requirement of national development recycling economy.
Present invention employs following technical scheme:
A kind of red soil nickel ore high concentration alkali leaching comprehensive utilization process, comprises the following steps:
(1) red soil nickel ore alkalinity extraction silicon-dioxide technique
A high concentration alkali leaching red soil nickel ore
Take solid sodium hydroxide by certain liquid-solid mass ratio (mass ratio of NaOH solution and red soil nickel ore) and put into reactor, add the concentration of deionized water to setting, red soil nickel ore is added after sodium hydroxide dissolves completely, build kettle cover, open water of condensation, stir, be heated to the temperature of setting.Leaching reaction arrived after the fixed time, added the dilution of 500mI water, when system temperature is down to 100 DEG C, opened still feeding, centrifugation, filter residue be desiliconization slag for extracting other element, filtrate is sodium silicate solution.
The condition of high concentration alkali leaching red soil nickel ore is: extraction temperature 210-230 DEG C, NaOH concentration 80-90%, extraction time 80-100min, liquid-solid mass ratio 4-6:1.
B sodium silicate solution carbonation decomposition prepares precipitated silica
Sodium silicate solution is formulated into finite concentration and modulus, be heated to temperature required, under constant temperature, pass into CO2 gas with certain flow velocity, detect solution ph at regular intervals, when pH value reaches a certain value, filtering separation, then carries out secondary carbonation decomposition to filtrate, terminates reaction when pH value is 9, vacuum filtration, obtains silicon-dioxide and sodium carbonate solution.Sodium carbonate solution realizes recycle through causticization
The processing condition that sodium silicate solution carbonation decomposition prepares precipitated silica are: carbonation decomposition temperature 60-80 DEG C, sodium silicate silicate 20-90g/L, and sodium silicate solution modulus is less than 0.6-1.
C sodium carbonate solution causticization
Get a certain amount of activated CaO, add deionized water, form milk of lime, by a certain percentage milk of lime is joined in certain density Na2CO3 solution, heating, stir, milk of lime and the severe rapid reaction of Na2CO3.
The condition of sodium carbonate solution causticization is: temperature 80-90 DEG C, time 7-9min, and nCaO:nNa2CO3=1.1-1.3, Na2CO3 concentration is 90-110g/L.
The evaporation concentration of the calcination of d calcium carbonate and sodium hydroxide
CaCO3 precipitation and NaOH strong solution is obtained after sodium carbonate solution causticization.The alkaline process that sodium hydroxide solution returns red soil nickel ore after evaporation concentration carries silicon technology; CaCO3 precipitation can directly as light calcium carbonate product after washing, drying, and also can be prepared into CaO and CO2 gas 1000-1300 DEG C of calcination, the carbon of the causticization and sodium silicate solution that are respectively used to sodium carbonate solution divides.
(2) magnesium oxide is prepared in the carbonization of red soil nickel ore desiliconization slag
Red soil nickel ore desiliconization slag is mixed by certain liquid-solid ratio (ml:g) with water, passes into carbon dioxide while stirring at a certain temperature.After reaction arrives the fixed time, vacuum filtration, filter cake is carbide slag, repetitive scrubbing, and gained filtrate is magnesium bicarbonate solution, is crossing thermal degradation precipitated magnesium carbonate through magnesium bicarbonate solution, and magnesiumcarbonate calcining obtains magnesium oxide.
The carbonization of red soil nickel ore desiliconization slag normal pressure is prepared magnesian condition and is: temperature of reaction 10-20 DEG C, reaction times 30-42h, liquid-solid ratio 48-52:1.
(3) red soil nickel ore carbide slag ammonia infuse is for nickel oxide
Get the carbide slag of certain mass, pour certain density leaching agent solution into flask, and heat, pass into oxygen, rapid stirring.Leach for some time, filter, filter cake is the ammonia leaching residue containing ferro element, is used as iron-smelting raw material or carries out high value added utilization after washing.Filtrate is nickel amine complex solution.The ammonia still process of nickel amine complex solution is obtained basic nickel carbonate, obtains nickel oxide product through calcination.
Red soil nickel ore carbide slag ammonia infuse for nickel oxide condition is: extraction temperature 55-65 DEG C, and leaching agent is volatile salt, concentration 5.5-6.5mo1/L, and extraction time is 120-180min, liquid-solid ratio 4.5-5.5:1.
Wherein preferred technique is:
The top condition of high concentration alkali leaching red soil nickel ore is: extraction temperature 220 DEG C, NaOH concentration 85%, extraction time 90min, liquid-solid mass ratio 5:1.The leaching yield of silicon-dioxide can reach more than 85%.
The top condition that sodium silicate solution carbonation decomposition prepares precipitated silica is: carbonation decomposition temperature 70 C, sodium silicate silicate 50g/L, and sodium silicate solution modulus is less than 0.8.Prepared purity be 99.93% silica product.
The top condition of sodium carbonate solution causticization is: temperature 85 DEG C, time 8min, and nCaO:nNa2CO3=1.2, Na2CO3 concentration is 100g/L.The causticizing efficiency of sodium carbonate solution can reach more than 92%.
The carbonization of red soil nickel ore desiliconization slag normal pressure is prepared magnesian top condition and is: temperature of reaction 15 DEG C, reaction times 36h, liquid-solid ratio 50:1.Magnesian extraction yield can reach more than 92%.
Red soil nickel ore carbide slag ammonia infuse for nickel oxide top condition is: extraction temperature 60 DEG C, and leaching agent is volatile salt, concentration 6mo1/L, and extraction time is 150min, liquid-solid ratio 5:1.The NiO rate of recovery can reach more than 92%.
The present invention is described in detail below:
Chemical analysis show in red soil nickel ore containing have an appointment 50% silicon-dioxide, be realize comprehensive utilization, the extraction and isolation of silicon-dioxide must be studied.According to the character of silicon-dioxide, easily and alkali reaction, and alkali does not react with ferric oxide, nickel oxide known silicon-dioxide, although Magnesium Silicate q-agent meeting in serpentine and alkali reaction, but generate magnesium hydroxide and be deposited in slag, thus considering to adopt alkali lye or molten caustic soda process red soil nickel ore.Carry in the red soil nickel ore after silicon and contain a large amount of magnesium hydroxides, the utilization of magnesium elements be realized, the extraction and isolation of magnesium hydroxide must be considered.And magnesium hydroxide is easy and acid-respons, conventional acid has sulfuric acid, hydrochloric acid, carbonic acid etc.Sulfuric acid, hydrochloric acid acidity are comparatively strong, can not only react, and can react with the ferric oxide in ore and nickel oxide, do not consider with magnesium hydroxide.Carbonic acid acidity is more weak, can react with magnesium hydroxide, and does not react with the ferric oxide in ore and nickel oxide, thus can consider that in ore pulp, pass into carbon dioxide at ambient pressure extracts magnesium hydroxide, realizes being separated.Containing a large amount of ferric oxide and a small amount of nickel oxide in red soil nickel ore after carrying silicon, magnesium, the nickel oxide now in ore comes out, can consider ammonia leaching process, and ferric oxide does not participate in reaction.Recrement after ammonia leaching, mainly containing ferric oxide, can be used as iron-smelting raw material or deep processing becomes iron oxide red product.
(1) red soil nickel ore alkalinity extraction silicon-dioxide technical process
First red soil nickel ore is adopted the silicon-dioxide in high concentration alkali solution process extraction ore, siliceous mineral in ore and sodium hydroxide react the water glass generating solubility, after stripping, centrifugation, the filter cake obtained is the desiliconization slag of the elements such as enrichment magnesium, nickel, iron, and filtrate is sodium silicate solution.
Pass into carbonic acid gas to sodium silicate solution and carry out carbonation decomposition, reaction generates sodium carbonate and precipitation of silica, filtering separation, filter cake obtains silica product through washing, drying, filtrate is sodium carbonate solution, adds calcium oxide and carries out causticization, can generate sodium hydroxide solution and light calcium carbonate.
Sodium hydroxide solution is used as the raw material of alkaline process process red soil nickel ore after evaporation concentration, light calcium carbonate can directly as product, also malleablely fire standby carbon dioxide and calcium oxide, be used separately as the raw material of sodium silicate solution carbonation decomposition and sodium carbonate solution causticization.
(2) magnesium oxide technical process is prepared in the carbonization of red soil nickel ore desiliconization slag
First with red soil nickel ore desiliconization slag for raw material, adopt the magnesium oxide in normal pressure carbon method extraction slag, the Magnesium hydrogen carbonate that magnesium hydroxide in slag and carbon dioxide reaction generate solubility enters solution, filtering separation, filter cake is the carbide slag of the elements such as further enriching nickel, iron, and filtrate is magnesium bicarbonate solution.Heated by magnesium bicarbonate solution, decompose and generate magnesiumcarbonate and release carbonic acid gas, filter, filtrate is the aqueous solution containing a small amount of magnesium ion, returns carbonation process, and filter cake through washing, dry obtained magnesiumcarbonate product, then can obtain magnesium oxide product through calcination.The carbon dioxide that pyrolytic process and calcination produce is all as the raw material of desiliconization slag carbonization.
(3) red soil nickel ore carbide slag ammonia infuse is for nickel oxide technical process
First with red soil nickel ore carbide slag for raw material, adopt volatile salt to leach the nickel extracted in carbide slag, the nickel in slag enters solution with the form of nickel amine complex, filtering separation, and filter cake is the ammonia leaching residue mainly containing ferro element, and filtrate is nickel amine complex solution.By the ammonia still process under certain condition of nickel amine complex solution, produce ammonia and carbon dioxide, after weak ammonia absorbs, prepare volatile salt return Ammonia leaching.Obtain basic nickel carbonate after the ammonia still process of nickel amine complex solution, nickel oxide product can be obtained through calcination.The carbon dioxide that calcination produces returns ammonia leaching preparation section.
The present invention has the following advantages: the technique fully utilize red soil nickel ore high value-added greening and theory are studied.By to the composition of red soil nickel ore raw material and the analysis of thing phase, devise the process of red soil nickel ore alkaline process and carry silicon and prepare silica product, desiliconization slag carbonization is carried magnesium and is prepared magnesiumcarbonate and magnesium oxide product, and carbide slag ammonia leaching nickel prepares the technical process of nickel oxide product.Without the discharge of waste gas, waste water, waste residue in this technological process, and achieve the recycle of industrial chemicals, be the comprehensive utilization of resources novel process of an environmental protection, meet the requirement of national development recycling economy.
Embodiment
For ease of understanding the present invention, it is as follows that the present invention enumerates embodiment.Those skilled in the art should understand, described embodiment is only help to understand the present invention, should not be considered as concrete restriction of the present invention.
Embodiment one
A kind of red soil nickel ore high concentration alkali leaching comprehensive utilization process, comprises the following steps:
(1) red soil nickel ore alkalinity extraction silicon-dioxide technique
A high concentration alkali leaching red soil nickel ore
Take solid sodium hydroxide by certain liquid-solid mass ratio (mass ratio of NaOH solution and red soil nickel ore) and put into reactor, add the concentration of deionized water to setting, red soil nickel ore is added after sodium hydroxide dissolves completely, build kettle cover, open water of condensation, stir, be heated to the temperature of setting.Leaching reaction arrived after the fixed time, added the dilution of 500mI water, when system temperature is down to 100 DEG C, opened still feeding, centrifugation, filter residue be desiliconization slag for extracting other element, filtrate is sodium silicate solution.
The condition of high concentration alkali leaching red soil nickel ore is: extraction temperature 210 DEG C, NaOH concentration 80%, extraction time 80min, liquid-solid mass ratio 4:1.
B sodium silicate solution carbonation decomposition prepares precipitated silica
Sodium silicate solution is formulated into finite concentration and modulus, be heated to temperature required, under constant temperature, pass into CO2 gas with certain flow velocity, detect solution ph at regular intervals, when pH value reaches a certain value, filtering separation, then carries out secondary carbonation decomposition to filtrate, terminates reaction when pH value is 9, vacuum filtration, obtains silicon-dioxide and sodium carbonate solution.Sodium carbonate solution realizes recycle through causticization
The processing condition that sodium silicate solution carbonation decomposition prepares precipitated silica are: carbonation decomposition temperature 60 C, sodium silicate silicate 20g/L, and sodium silicate solution modulus is less than 0.6.
C sodium carbonate solution causticization
Get a certain amount of activated CaO, add deionized water, form milk of lime, by a certain percentage milk of lime is joined in certain density Na2CO3 solution, heating, stir, milk of lime and the severe rapid reaction of Na2CO3.
The condition of sodium carbonate solution causticization is: temperature 80 DEG C, time 7min, and nCaO:nNa2CO3=1.1, Na2CO3 concentration is 90g/L.
The evaporation concentration of the calcination of d calcium carbonate and sodium hydroxide
CaCO3 precipitation and NaOH strong solution is obtained after sodium carbonate solution causticization.The alkaline process that sodium hydroxide solution returns red soil nickel ore after evaporation concentration carries silicon technology; CaCO3 precipitation can directly as light calcium carbonate product after washing, drying, and also can be prepared into CaO and CO2 gas 1000-1300 DEG C of calcination, the carbon of the causticization and sodium silicate solution that are respectively used to sodium carbonate solution divides.
(2) magnesium oxide is prepared in the carbonization of red soil nickel ore desiliconization slag
Red soil nickel ore desiliconization slag is mixed by certain liquid-solid ratio (ml:g) with water, passes into carbon dioxide while stirring at a certain temperature.After reaction arrives the fixed time, vacuum filtration, filter cake is carbide slag, repetitive scrubbing, and gained filtrate is magnesium bicarbonate solution, is crossing thermal degradation precipitated magnesium carbonate through magnesium bicarbonate solution, and magnesiumcarbonate calcining obtains magnesium oxide.
The carbonization of red soil nickel ore desiliconization slag normal pressure is prepared magnesian condition and is: temperature of reaction 10 DEG C, reaction times 30h, liquid-solid ratio 48:1.
(3) red soil nickel ore carbide slag ammonia infuse is for nickel oxide
Get the carbide slag of certain mass, pour certain density leaching agent solution into flask, and heat, pass into oxygen, rapid stirring.Leach for some time, filter, filter cake is the ammonia leaching residue containing ferro element, is used as iron-smelting raw material or carries out high value added utilization after washing.Filtrate is nickel amine complex solution.The ammonia still process of nickel amine complex solution is obtained basic nickel carbonate, obtains nickel oxide product through calcination.
Red soil nickel ore carbide slag ammonia infuse for nickel oxide condition is: extraction temperature 55 DEG C, and leaching agent is volatile salt, concentration 5.5mo1/L, and extraction time is 120min, liquid-solid ratio 4.5:1.
The composition of described red soil nickel ore comprises (wt%): 49.3SiO2,15.8Fe2O3,5.05Al2O3,1.08NiO, 0.82CaO, 0.63Cr2O3.
Embodiment two
A kind of red soil nickel ore high concentration alkali leaching comprehensive utilization process, comprises the following steps:
(1) red soil nickel ore alkalinity extraction silicon-dioxide technique
A high concentration alkali leaching red soil nickel ore
Take solid sodium hydroxide by certain liquid-solid mass ratio (mass ratio of NaOH solution and red soil nickel ore) and put into reactor, add the concentration of deionized water to setting, red soil nickel ore is added after sodium hydroxide dissolves completely, build kettle cover, open water of condensation, stir, be heated to the temperature of setting.Leaching reaction arrived after the fixed time, added the dilution of 500mI water, when system temperature is down to 100 DEG C, opened still feeding, centrifugation, filter residue be desiliconization slag for extracting other element, filtrate is sodium silicate solution.
The condition of high concentration alkali leaching red soil nickel ore is: extraction temperature 230 DEG C, NaOH concentration 90%, extraction time 100min, liquid-solid mass ratio 6:1.
B sodium silicate solution carbonation decomposition prepares precipitated silica
Sodium silicate solution is formulated into finite concentration and modulus, be heated to temperature required, under constant temperature, pass into CO2 gas with certain flow velocity, detect solution ph at regular intervals, when pH value reaches a certain value, filtering separation, then carries out secondary carbonation decomposition to filtrate, terminates reaction when pH value is 9, vacuum filtration, obtains silicon-dioxide and sodium carbonate solution.Sodium carbonate solution realizes recycle through causticization
The processing condition that sodium silicate solution carbonation decomposition prepares precipitated silica are: carbonation decomposition temperature 80 DEG C, and sodium silicate silicate 90g/L, sodium silicate solution modulus is less than 1.
C sodium carbonate solution causticization
Get a certain amount of activated CaO, add deionized water, form milk of lime, by a certain percentage milk of lime is joined in certain density Na2CO3 solution, heating, stir, milk of lime and the severe rapid reaction of Na2CO3.
The condition of sodium carbonate solution causticization is: temperature 90 DEG C, time 9min, and nCaO:nNa2CO3=1.3, Na2CO3 concentration is 110g/L.
The evaporation concentration of the calcination of d calcium carbonate and sodium hydroxide
CaCO3 precipitation and NaOH strong solution is obtained after sodium carbonate solution causticization.The alkaline process that sodium hydroxide solution returns red soil nickel ore after evaporation concentration carries silicon technology; CaCO3 precipitation can directly as light calcium carbonate product after washing, drying, and also can be prepared into CaO and CO2 gas 1000-1300 DEG C of calcination, the carbon of the causticization and sodium silicate solution that are respectively used to sodium carbonate solution divides.
(2) magnesium oxide is prepared in the carbonization of red soil nickel ore desiliconization slag
Red soil nickel ore desiliconization slag is mixed by certain liquid-solid ratio (ml:g) with water, passes into carbon dioxide while stirring at a certain temperature.After reaction arrives the fixed time, vacuum filtration, filter cake is carbide slag, repetitive scrubbing, and gained filtrate is magnesium bicarbonate solution, is crossing thermal degradation precipitated magnesium carbonate through magnesium bicarbonate solution, and magnesiumcarbonate calcining obtains magnesium oxide.
The carbonization of red soil nickel ore desiliconization slag normal pressure is prepared magnesian condition and is: temperature of reaction 20 DEG C, reaction times 42h, liquid-solid ratio 52:1.
(3) red soil nickel ore carbide slag ammonia infuse is for nickel oxide
Get the carbide slag of certain mass, pour certain density leaching agent solution into flask, and heat, pass into oxygen, rapid stirring.Leach for some time, filter, filter cake is the ammonia leaching residue containing ferro element, is used as iron-smelting raw material or carries out high value added utilization after washing.Filtrate is nickel amine complex solution.The ammonia still process of nickel amine complex solution is obtained basic nickel carbonate, obtains nickel oxide product through calcination.
Red soil nickel ore carbide slag ammonia infuse for nickel oxide condition is: extraction temperature 65 DEG C, and leaching agent is volatile salt, concentration 6.5mo1/L, and extraction time is 180min, liquid-solid ratio 5.5:1.
The composition of described red soil nickel ore comprises (wt%): 49.3SiO2,15.8Fe2O3,5.05Al2O3,1.08NiO, 0.82CaO, 0.63Cr2O3.
Embodiment three
A kind of red soil nickel ore high concentration alkali leaching comprehensive utilization process, comprises the following steps:
(1) red soil nickel ore alkalinity extraction silicon-dioxide technique
A high concentration alkali leaching red soil nickel ore
Take solid sodium hydroxide by certain liquid-solid mass ratio (mass ratio of NaOH solution and red soil nickel ore) and put into reactor, add the concentration of deionized water to setting, red soil nickel ore is added after sodium hydroxide dissolves completely, build kettle cover, open water of condensation, stir, be heated to the temperature of setting.Leaching reaction arrived after the fixed time, added the dilution of 500mI water, when system temperature is down to 100 DEG C, opened still feeding, centrifugation, filter residue be desiliconization slag for extracting other element, filtrate is sodium silicate solution.
The top condition of high concentration alkali leaching red soil nickel ore is: extraction temperature 220 DEG C, NaOH concentration 85%, extraction time 90min, liquid-solid mass ratio 5:1.The leaching yield of silicon-dioxide can reach more than 85%.
B sodium silicate solution carbonation decomposition prepares precipitated silica
Sodium silicate solution is formulated into finite concentration and modulus, be heated to temperature required, under constant temperature, pass into CO2 gas with certain flow velocity, detect solution ph at regular intervals, when pH value reaches a certain value, filtering separation, then carries out secondary carbonation decomposition to filtrate, terminates reaction when pH value is 9, vacuum filtration, obtains silicon-dioxide and sodium carbonate solution.Sodium carbonate solution realizes recycle through causticization
The top condition that sodium silicate solution carbonation decomposition prepares precipitated silica is: carbonation decomposition temperature 70 C, sodium silicate silicate 50g/L, and sodium silicate solution modulus is less than 0.8.Prepared purity be 99.93% silica product.
C sodium carbonate solution causticization
Get a certain amount of activated CaO, add deionized water, form milk of lime, by a certain percentage milk of lime is joined in certain density Na2CO3 solution, heating, stir, milk of lime and the severe rapid reaction of Na2CO3.
The top condition of sodium carbonate solution causticization is: temperature 85 DEG C, time 8min, and nCaO:nNa2CO3=1.2, Na2CO3 concentration is 100g/L.The causticizing efficiency of sodium carbonate solution can reach more than 92%.
The evaporation concentration of the calcination of d calcium carbonate and sodium hydroxide
CaCO3 precipitation and NaOH strong solution is obtained after sodium carbonate solution causticization.The alkaline process that sodium hydroxide solution returns red soil nickel ore after evaporation concentration carries silicon technology; CaCO3 precipitation can directly as light calcium carbonate product after washing, drying, and also can be prepared into CaO and CO2 gas 1000-1300 DEG C of calcination, the carbon of the causticization and sodium silicate solution that are respectively used to sodium carbonate solution divides.
(2) magnesium oxide is prepared in the carbonization of red soil nickel ore desiliconization slag
Red soil nickel ore desiliconization slag is mixed by certain liquid-solid ratio (ml:g) with water, passes into carbon dioxide while stirring at a certain temperature.After reaction arrives the fixed time, vacuum filtration, filter cake is carbide slag, repetitive scrubbing, and gained filtrate is magnesium bicarbonate solution, is crossing thermal degradation precipitated magnesium carbonate through magnesium bicarbonate solution, and magnesiumcarbonate calcining obtains magnesium oxide.
The carbonization of red soil nickel ore desiliconization slag normal pressure is prepared magnesian top condition and is: temperature of reaction 15 DEG C, reaction times 36h, liquid-solid ratio 50:1.Magnesian extraction yield can reach more than 92%.
(3) red soil nickel ore carbide slag ammonia infuse is for nickel oxide
Get the carbide slag of certain mass, pour certain density leaching agent solution into flask, and heat, pass into oxygen, rapid stirring.Leach for some time, filter, filter cake is the ammonia leaching residue containing ferro element, is used as iron-smelting raw material or carries out high value added utilization after washing.Filtrate is nickel amine complex solution.The ammonia still process of nickel amine complex solution is obtained basic nickel carbonate, obtains nickel oxide product through calcination.
Red soil nickel ore carbide slag ammonia infuse for nickel oxide top condition is: extraction temperature 60 DEG C, and leaching agent is volatile salt, concentration 6mo1/L, and extraction time is 150min, liquid-solid ratio 5:1.The NiO rate of recovery can reach more than 92%.
The composition of described red soil nickel ore comprises (wt%): 49.3SiO2,15.8Fe2O3,5.05Al2O3,1.08NiO, 0.82CaO, 0.63Cr2O3.
Applicant states, the present invention illustrates detailed process equipment and process flow process of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned detailed process equipment and process flow process, namely do not mean that the present invention must rely on above-mentioned detailed process equipment and process flow process and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of ancillary component, the concrete way choice etc. of each raw material of product of the present invention, all drops within protection scope of the present invention and open scope.
Claims (6)
1. a red soil nickel ore high concentration alkali leaching comprehensive utilization process, comprises the following steps:
(1) red soil nickel ore alkalinity extraction silicon-dioxide
A high concentration alkali leaching red soil nickel ore
Take solid sodium hydroxide by certain liquid-solid mass ratio (mass ratio of NaOH solution and red soil nickel ore) and put into reactor, add the concentration of deionized water to setting, red soil nickel ore is added after sodium hydroxide dissolves completely, build kettle cover, open water of condensation, stir, be heated to the temperature of setting; Leaching reaction arrived after the fixed time, added the dilution of 500mI water, when system temperature is down to 100 DEG C, opened still feeding, centrifugation, filter residue be desiliconization slag for extracting other element, filtrate is sodium silicate solution;
The condition of high concentration alkali leaching red soil nickel ore is: extraction temperature 210-230 DEG C, NaOH concentration 80-90%, extraction time 80-100min, liquid-solid mass ratio 4-6:1;
B sodium silicate solution carbonation decomposition prepares precipitated silica
Sodium silicate solution is formulated into finite concentration and modulus, be heated to temperature required, under constant temperature, pass into CO2 gas with certain flow velocity, detect solution ph at regular intervals, when pH value reaches a certain value, filtering separation, then carries out secondary carbonation decomposition to filtrate, terminates reaction when pH value is 9, vacuum filtration, obtains silicon-dioxide and sodium carbonate solution; Sodium carbonate solution realizes recycle through causticization;
The processing condition that sodium silicate solution carbonation decomposition prepares precipitated silica are: carbonation decomposition temperature 60-80 DEG C, sodium silicate silicate 20-90g/L, and sodium silicate solution modulus is less than 0.6-1;
C sodium carbonate solution causticization
Get a certain amount of activated CaO, add deionized water, form milk of lime, by a certain percentage milk of lime is joined in certain density Na2CO3 solution, heating, stir, milk of lime and the severe rapid reaction of Na2CO3;
The condition of sodium carbonate solution causticization is: temperature 80-90 DEG C, time 7-9min, and nCaO:nNa2CO3=1.1-1.3, Na2CO3 concentration is 90-110g/L;
The evaporation concentration of the calcination of d calcium carbonate and sodium hydroxide
CaCO3 precipitation and NaOH strong solution is obtained after sodium carbonate solution causticization; The alkaline process that sodium hydroxide solution returns red soil nickel ore after evaporation concentration carries silicon technology; CaCO3 precipitation can directly as light calcium carbonate product after washing, drying, and also can be prepared into CaO and CO2 gas 1000-1300 DEG C of calcination, the carbon of the causticization and sodium silicate solution that are respectively used to sodium carbonate solution divides;
(2) magnesium oxide is prepared in the carbonization of red soil nickel ore desiliconization slag
Red soil nickel ore desiliconization slag is mixed by certain liquid-solid ratio (ml:g) with water, passes into carbon dioxide while stirring at a certain temperature; After reaction arrives the fixed time, vacuum filtration, filter cake is carbide slag, repetitive scrubbing, and gained filtrate is magnesium bicarbonate solution, is crossing thermal degradation precipitated magnesium carbonate through magnesium bicarbonate solution, and magnesiumcarbonate calcining obtains magnesium oxide;
The carbonization of red soil nickel ore desiliconization slag normal pressure is prepared magnesian condition and is: temperature of reaction 10-20 DEG C, reaction times 30-42h, liquid-solid ratio 48-52:1;
(3) red soil nickel ore carbide slag ammonia infuse is for nickel oxide
Get the carbide slag of certain mass, pour certain density leaching agent solution into flask, and heat, pass into oxygen, rapid stirring; Leach for some time, filter, filter cake is the ammonia leaching residue containing ferro element, is used as iron-smelting raw material or carries out high value added utilization after washing; Filtrate is nickel amine complex solution; The ammonia still process of nickel amine complex solution is obtained basic nickel carbonate, obtains nickel oxide product through calcination;
Red soil nickel ore carbide slag ammonia infuse for nickel oxide condition is: extraction temperature 55-65 DEG C, and leaching agent is volatile salt, concentration 5.5-6.5mo1/L, and extraction time is 120-180min, liquid-solid ratio 4.5-5.5:1.
2. technique according to claim 1, the top condition of high concentration alkali leaching red soil nickel ore is: extraction temperature 220 DEG C, NaOH concentration 85%, extraction time 90min, liquid-solid mass ratio 5:1.
3. technique according to claim 1, the top condition that sodium silicate solution carbonation decomposition prepares precipitated silica is: carbonation decomposition temperature 70 C, sodium silicate silicate 50g/L, and sodium silicate solution modulus is less than 0.8.
4. technique according to claim 1, the top condition of sodium carbonate solution causticization is: temperature 85 DEG C, time 8min, and nCaO:nNa2CO3=1.2, Na2CO3 concentration is 100g/L.
5. technique according to claim 1, the carbonization of red soil nickel ore desiliconization slag normal pressure is prepared magnesian top condition and is: temperature of reaction 15 DEG C, reaction times 36h, liquid-solid ratio 50:1.
6. technique according to claim 1, red soil nickel ore carbide slag ammonia infuse for nickel oxide top condition is: extraction temperature 60 DEG C, and leaching agent is volatile salt, concentration 6mo1/L, and extraction time is 150min, liquid-solid ratio 5:1.
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