CN101058852A - Multistage counter current acid leaching process containing nickel serpentine ore - Google Patents
Multistage counter current acid leaching process containing nickel serpentine ore Download PDFInfo
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Abstract
The invention discloses a nepouite with the multi-stage reverse-current acid-dipping technology, which comprises the following steps : grinding the nepouite; reacting with mixing the primary immersion liquid and water; reacting the leach residues a plurality of times endlessly; getting the K extract after finishing filtering the reaction of the k times; making the K extract liquor and the K extract react cyclically the k+1 times; regarding the k extract liquor as the extract liquor of the k-1 leaching reaction; regarding a corrosive acid as the extract liquor of the last leaching reaction; regarding the last extract liquor as a liquor containing Ni and Mg after n times reaction (k is between 1 and n and n is not less than 2). The invention reduces the cost, which recovers the Ni and Mg highly effectively.
Description
Technical field
The invention belongs to the hydrometallurgy field, relate to a kind of chemical metallurgical method of serpentine ore, particularly a kind of multistage counter current acid leaching process that helps metals such as comprehensive extraction nickel, magnesium from the serpentine ore.
Background technology
Serpentine (Mg
6[Si
4O
10] (OH)
8) be a kind of layer silicate mineral, its structural sheet is the bilayer by one deck silicon-oxy tetrahedron and the octahedra be combined into of one deck brucite.Six coordinate Mg can be by Al in the ore
3+, Ni
2+, Fe
2+, Fe
3+, Mn
2+Deng replace, William stone is a kind of common nickeliferous, magnesium mineral.China's serpentine resource is abundant, fine texture, and explored reserves surpass 500,000,000 t.The development and use of China's serpentine at present still are in the junior stage, research level is lower, most of mines mainly are the thick products of former lump ore of raise money on and simple processing, as make chemical fertilizer (fused(calcium magnesium)phosphate), make the auxiliary material of refractory materials, production cast stone or rock wool etc., added value is low, economic benefit is very poor, serious waste of resources.
Because nickel mainly is present in the silicate minerals with isomorph in the William stone ore deposit, and granularity is very thin, therefore can not give enrichment with the mechanical beneficiation method, can only adopt chemical mineral processing or smelting enriching method to extract nickel.Chemical mineral processing or smelting enriching method to nickel oxide ore have pyrogenic process and wet method two big classes again.The former divides and makes sulphur melting, ferronickel method and nodulizing process, and the latter has alkaline process and acidic process method etc. again.Because the pyrogenic process concentration method needs to adopt the pyroprocessing ore, and needs a large amount of heat energy when refining nickel, ferronickel, so wet method is carried nickel and is obtained the investigator and pay attention to.
Serpentine for low-grade nickel oxide adopts roasting-ammonia soaking technology more, or reducing roasting-pickling process reclaims the nickel metal." non-ferrous extractive metallurgy handbook (copper nickel volume) " disclosed a kind of employing sulfuric acid extract technology, leach liquor employing hydrogen sulfide is heated to pressurize and is reclaimed method (" non-ferrous extractive metallurgy handbook (copper nickel volume) " metallurgical press, 2000,7 of nickel, first version, p
724-p
727).These conventional process flow complexity, facility investment is big, and the energy consumption height causes nickel production cost height, deficiency in economic performance.
Patent US20060002835 (D Neudorf, C A Oakville.Method for leaching laterite ores by reaction withconcentrated acid and water leaching, US20060002835 2006-01-05) has disclosed a kind of sulfuric acid and has leached the method that red soil nickel ore extracts low-grade nickel oxide.Patent CN200310110839.2 heats under normal pressure in the leaching serpentine, and leach liquor is with sulfide precipitation nickel metal, output nickel ore concentrate grade up to 20～50% (nickel oxide sulfuric acid leach extraction method in the serpentine, CN200310110839.2,2004-12-08).Although it is less that this technology is invested, can produce high quality nickel sulfide concentrate product, the uncomprehensive magnesium resource that reclaims, the rate of recovery of nickel is not mentioned yet simultaneously.Cao Guohua has obtained nickeliferous greater than 25% nickelous sulfide product from red soil nickel ore by the leaching of sulfuric acid normal pressure, the heavy nickel of sodium sulphite, the nickel deposition rate reaches more than 99.5%, this technology is simple, invest little, energy consumption is low, production cost lower (Cao Guohua, the method for acquisition nickelous sulfide from the red soil nickel ore pickling liquor, CN200510010916.6,2006-02-22).This method has also shown simultaneously from nickeliferous leach liquor can high efficiente callback and prepare qualified nickelous sulfide product.
Contain the magnesium more than 20% in the serpentine ore, have comprehensive recovery value.(CN89106821.X 1991-04-03) provides a kind of comprehensive utilization process of serpentine ore to patent CN89106821.X for Liu Xuqing, the comprehensive utilization of serpentine tailing.Hydrochloric acid leaching ore powder with 5%～9%, use fractionation technique, regulate pH separation of iron and other impurity with milk of lime, with carbonic acid gas carbonization separating calcium and magnesium, and under the certain chlorine ion concentration condition of control, at 102 ℃ of thermal degradation Magnesium hydrogen carbonates, red iron oxide, lime carbonate and light magnesium oxide from serpentine, have been produced.(with the serpentine is the method for raw material production magnesiumcarbonate and/or magnesium oxide and porous silica to Zhang Tianzhong, CN88109734.9,1990-05-02) with the serpentine be raw material, after calcining 2～4 hours through 400～800 ℃ earlier, again with separating after the mineral acid treatment, obtain precipitation of silica and magnesium salt solution, this magnesium salt solution can obtain the magnesiumcarbonate precipitation after handling with the carbonate of ammonium, finally obtains porous silica, magnesiumcarbonate and/or method of magnesium oxide.CN01131802.3 (Wang Yuliang, produce the method for light magnesium oxide, white carbon black and reclaim(ed) sulfuric acid ammonium with serpentine, CN01131802.3,2003-06-11) by with 140～220 purpose serpentine breezes through the magnetic separator magnetic separation, its magneticstrength is removed rich greenalite ore deposit greater than 2800 oersteds; Magnetic tailing acidleach after-filtration, solution are produced light magnesium oxide through carbonization, calcining again through neutralization, removing impurities by oxidation; Leached mud and concentration are that water glass is produced in the reaction of 20～40% white liquor, water glass are transferred through the acid of two steps to generate white carbon black again, and the filtered liquid of magnesium basic carbonate is through the recyclable ammonium sulfate of two steps evaporation.
In the related method of above-mentioned patent, all consider the comprehensive utilization of serpentine ore, fully reclaimed wherein magnesium, silicon resource, also shown the possibility of high efficiente callback magnesium from contain the magnesium leach liquor; It is not enough that but these technologies are considered the rate of recovery of magnesium, and especially under simple normal temperature and pressure conditions, the valuable metal in the silicate is difficult to leach, and must cause the leaching effect of metal target such as magnesium undesirable.
For resources such as can be from the William stone ore efficient comprehensive recovery nickel, magnesium, improve economic benefit of enterprises, make full use of exhausted day by day Mineral resources as far as possible and promote sustainable development, the emphasis of research is the leaching of strengthening nickel, magnesium by new technology, novel process, make it change liquid phase over to, with other impurity initial gross separations such as silicon.Can continue to use existing metallurgical technology as for nickeliferous, the magnesium leach liquor that obtain and realize separation and concentration and recovery preferably, produce qualified Ni, Mg product; Leached mud can reclaim according to market situation based on silicon-dioxide, in order to produce technical grade chemistry of silicones product such as porous silica or water glass.
But nickel, the magnesium occurrence status in serpentine ore is complicated.Material phase analysis result according to several mines serpentine, find that the magnesium in the serpentine ore has only minimum part (magnesium in magnesium oxide, the carbonate) to be gone out by acidleach easily, and the magnesium in the indissoluble silicate is the most difficult leaching, and this also is the one of the main reasons that serpentine seldom is used for reclaiming magnesium.The occurrence form of nickel is complicated more, and existing oxidized ore has sulphide ores again, and the oxidized ore major part is given in the silicate minerals, is difficult for leaching.
In order to strengthen the leaching of metals such as Ni, Mg in the serpentine ore, must take appropriate measures: improve leaching agent concentration and increase its consumption, perhaps High Temperature High Pressure leaches, leach activation (mechanical activation, thermal activation etc.) back in advance.People such as Ceng Ying have studied thermal activation-sulfuric acid extract technology and reclaimed magnesium from serpentine ores, have obtained best extract technology condition: earlier breeze is calcined 60min under 700 ℃ of conditions, use 3mol/LH again
2SO
4(liquid-solid ratio L/S=15) leaches 60min at normal temperatures, the leaching yield of Mg can reach more than 93% (Ceng Ying, Zhu Ping, Liu Qiang. activation acidleach serpentine extracts the experimental study [J] of magnesium. mining metallurgical engineering, 2006,26 (2): 57-60.).It is 0.554% serpentine that Luo Xian equality people adopts the sulfuric acid extract technology to handle to contain Ni, less than 0.074mm be 87.1% at grinding fineness, liquid-solid ratio L/S is 5, leach 6h under the sulfuric acid concentration 1.50mol/L, 60 ℃ of conditions, the leaching yield of the nickel that obtains is 85.7%, leach liquor is heavy nickel after purifying, and can get nickeliferous 41.24% Ni (OH)
2Nickel ore concentrate, heavy nickel yield 88.6%, comprehensive yield reach 75.93% (Luo Xianping, Gong Enmin. pickling process is extracted the research [J] of nickel from William stone. non-ferrous metal (smelting part), 2006, (4): 28-31.).
In conventional acidleach process, owing to the kinetics reason, and leach the cause that product or intermediate product are easy to cover mineral, in order to obtain the leaching yield of higher metal target, must strengthen the consumption and the concentration (guaranteeing that free acid content is that 60～200g/L does not wait in the leach liquor) of leaching agent mineral acid.But because the sulfuric acid large usage quantity, it is higher to cause leaching cost on the one hand, on the other hand, must consume a large amount of alkali in follow-up purifying treatment operation, causes production cost higher.Solve the bigger problem of leach liquor acidity, can not leach by simple reduction and use sulfuric acid consumption, otherwise can reduce the leaching yield of metal target, cause resource fully comprehensively not reclaim.
Summary of the invention
Purpose of the present invention aims to provide and a kind ofly can reduce the leaching cost effectively, the follow-up purifying treatment operation of favourable reduction production cost, and comprehensive high-efficiency ground reclaims the multistage counter current acid leaching process in the William stone ore deposit of nickel, magnesium resource.
The objective of the invention is to realize by following manner.
Technology of the present invention is: the William stone ore deposit is ground, and the first immersion of adding agent, water stir and leach reaction, and n leaching reaction carried out in the circulation of gained leached mud; The k time leaching reacted to filter and obtained k section leached mud, and k section leach liquor, k section leached mud are recycled to next section and carry out the k+1 time leaching reaction, and k section leach liquor then is recycled to the immersion agent of the preceding paragraph as the k-1 time leaching reaction; Last immersion agent of leaching reaction is a strong acid; After leach reacting through n time, the final leach liquor of gained is the solution of required nickeliferous magnesium; Wherein, 1≤k≤n, n is not less than 2.
Described first leaching agent is for the second time leaching agent or strong acid.
Described strong acid is selected from one or more in nitric acid, hydrochloric acid, the sulfuric acid.
Described n is 2-5, preferred 2-3.
It is 0-100 ℃ that each section leaches temperature of reaction, preferred 80-95 ℃.
Each section extraction time is 30min～240min, preferred 60～90min.Each section leaching agent volume is 2.0～10.0 than (L/S) with it with ore powder or leached mud quality.
Wash water and the n time leach liquor that described last leaching reaction wash water washs the n time leached mud gained merge the leaching agent that reacts as the n-1 time leaching.
The present invention adopts the multistage counter current acid leaching novel process, utilize higher level's leach liquor (containing free acid) to leach original ore powder, the acidity of pending leach liquor not only can neutralize, the pH value of final leach liquor is remained on about 2.0, and can make full use of leaching agent, guaranteeing to reduce the leaching of reagent consumption and impurity as far as possible under the prerequisite of more nickelic, magnesium leaching yield, comprehensive high-efficiency reclaims the nickel magnesium resource, reduces production costs.
The present invention after preliminary fragmentation, is milled to 0.074mm～2.0mm by wet ball-milling with the William stone ore, and ore milling concentration is 20%～60%; The ore pulp that obtains is at reactor, through multistage counter current acid leaching.For slag, final stage and leaching agent-strong acid leaches reaction, and for final leach liquor, be after the leached mud that will obtain repeatedly circulates, the content of metal target reduces piecemeal in the breeze, and the concentration of metal target increases piecemeal in the leach liquor, and the acidity in the leaching agent reduces piecemeal.Final leach liquor utilizes fractional precipitation, solvent extraction technology or ion exchange technique to carry out nickel, magnesium separation and concentration, and prepares corresponding qualified nickel, magnesium products after carrying out removal of impurities operation such as deironing.
In the method for the present invention, being suitable for the inventive method leaching agent can be strong acid, as nitric acid, sulfuric acid, hydrochloric acid etc.; Also can be that wherein two or more are used in combination.
In the method for the present invention, the ore pulp that ball milling obtains adds in the reactor with leaching agent or water (regulating liquid-solid ratio L/S), and multistage counter current leaches.The advantage of the present invention and prior art is, leaches hop count by control, both can guarantee higher nickel, magnesium leaching yield, and is again can the acid consumption minimum, makes full use of leaching agent.Compare with common process, nickel magnesium leaching effect of the present invention is good, its leaching yield all can reach more than 95%, and endpoint pH generally can be controlled at about 2.0, free acid is less in the leach liquor, the leaching agent waste is little, and leach liquor can directly carry out solvent extraction or ion exchange technique and reclaim the nickel magnesium products after removal of impurities, is the Perfected process of handling the William stone ore.
In specific embodiments of the present invention, pulp density can be 10%～80% (mass percent of ore in the ore pulp), preferred 30%～50% (L/S=2～3); Leach hop count and can be 2～5 sections, preferred 2～3 sections; Leach temperature of reaction and can under 0 ℃～100 ℃ temperature, carry out preferred 80 ℃～95 ℃; Leaching reaction pressure can carry out under normal pressure; Every section is leached the reaction times is 30-240 minute, preferred 60～90 minutes.
Method of the present invention can adopt general anticorrosion reactor.
The present invention not only is suitable for handling William stone ore deposit, comprehensive recovery nickel magnesium; And be suitable for from nickeliferous serpentine ore seldom, efficiently leaching and the simple magnesium that reclaims.
Description of drawings
Accompanying drawing 1 is the schema of multistage counter current acid leaching process of the present invention.
Accompanying drawing 2 is two sections adverse current vitriol lixiviations technical process of embodiment 1.
The technical process of 3 three sections adverse current vitriol lixiviations of accompanying drawing.
Embodiment
The present invention is further specified by the following example, but is not subjected to the restriction of these embodiment.All umbers and percentage ratio all refer to quality except as otherwise herein provided among the embodiment.
Embodiment 1
Adopt two sections adverse current sulfuric acid extract technologies to handle William stone (flow process is seen Fig. 2).This sample ore is taken from the mine, Fujian, contains Ni and be 0.20%, Mg is 22.27%.
Get 100 parts of ore samples, add 150 fens water for ball milling after the fragmentation to accounting for 74.5%) less than 0.074mm, the ore pulp that obtains joins in the reactor together with 160 parts of vitriol oils (98%), 50 fens water together, start stirring (500rpm), utilizing Dilution of sulphuric acid and exothermic heat of reaction that system temperature is raised to is 95 ℃, blowing filters behind the control reaction 120min, obtains leach liquor nickeliferous, magnesium and (contains magnesium 70.4g/L, nickel 0.62g/L, H
2SO
474g/L); The leach liquor that obtains and 100 parts of ore samples (add 150 fens water for ball milling, account for 74.5% less than 0.074mm) filter at 75 ℃ of following stirring reaction 90min, and the filtrate that obtains (one section leach liquor also is final leach liquor) contains magnesium 85.4g/L, nickel 0.68g/L, H
2SO
44g/L; Filter cake joins in the reactor together with 160 parts of vitriol oils (98%), 50 fens water together, start stirring (500rpm), blowing filters behind reaction 120min under 95 ℃, filtrate is as one section leaching agent that leaches reaction, abandon after the filter cake chemical examination, the leaching yield that records magnesium, nickel reaches 96.5%, 98.8% respectively.
Leach liquor adopts yellow modumite ([NaFe
3(SO
4)
3(OH)
6]) the method deironing, make neutralizing agent with yellow soda ash, adjusting pH value is 2.0～2.4, be warmed up to 90 ℃ down reaction 60min generate iron vitriol slags, the deironing rate can reach 97.2%, the nickel loss amount is 4.5% in the slag, magnesium loss is 2.4%; The deironing scavenging solution that obtains adopts P204 (extraction phase is made up of the 15%P204+85% sulfonated kerosene) as extraction agent, carries out the Pyatyi counter-current extraction; Organic phase washing back adopts the sulphuric acid soln of 1mol/L to carry out three stage countercurrent back extractions, and the rate of recovery of nickel is 98.8% in extraction and the back extraction process; The nickel sulfate solution that obtains can obtain the single nickel salt product through evaporating, concentrating and crystallizing, and the ult rec of nickel is 93.2%.Raffinate adopts 30% sodium hydroxide solution adjustment pH value to 12, produce precipitated magnesium hydroxide (heavy magnesium filter is 97.0%), the magnesium hydroxide that obtains is calcined 60min down through 800 ℃, obtain magnesium oxide product, magnesian content is 98.5%, quality index reaches the top grade product and requires (HG/T2573-94), and the ult rec of magnesium is 91.4% in the whole process.
Embodiment 2
The William stone sample ore adopts three sections adverse current sulfuric acid extract technologies to handle with embodiment one.See shown in Figure 3.
Original ore powder is for getting 100 parts of ore samples, adds 150 fens water for ball milling after the fragmentation and refers to account for less than 0.074mm 80.0% ore pulp sample.
One section, two sections leaching temperature of reaction all are controlled at about 75 ℃, and the reaction times is 60min.Obtain final leach liquor and contain magnesium 95.4g/L, nickel 0.85g/L, H
2SO
42.5g/L.
The leaching agent of three sections leachings is 160 parts of vitriol oils (98%) and 100 fens water, and the temperature of three sections leachings is controlled at about 95 ℃, stirs (500rpm) reaction 90min, filters, and filtrate and filter cake washing water also synthesize the leaching agent of two sections leachings; The chemical examination filter cake wherein contains Ni, Mg and is respectively 0.0092% and 0.98%.According to the content of metal in the filter cake, the leaching yield that calculates metal target Ni and Mg is respectively 98.8%, 99.2%.
Leach liquor adopts yellow modumite ([NaFe
3(SO
4)
3(OH)
6]) the method deironing, make neutralizing agent with yellow soda ash, adjusting pH value is 2.0～2.4, be warmed up to 90 ℃ down reaction 60min generate iron vitriol slags, the deironing rate can reach 97.2%, the nickel loss amount is 4.5% in the slag, magnesium loss is 2.4%; The deironing scavenging solution that obtains adopts P204 (extraction phase is made up of the 15%P204+85% sulfonated kerosene) as extraction agent, carries out the Pyatyi counter-current extraction; Organic phase washing back adopts the sulphuric acid soln of 1mol/L to carry out three stage countercurrent back extractions, and the rate of recovery of nickel is 98.8% in extraction and the back extraction process; The nickel sulfate solution that obtains can obtain the single nickel salt product through evaporating, concentrating and crystallizing, and the ult rec of nickel is 94.2%.Raffinate adopts 30% sodium hydroxide solution adjustment pH value to 4.5, prepares MgSO by evaporative crystallization
47H
2O, purity reaches the first grade requirement greater than 99%; Contain Mg10g/L (returning in one section leach liquor) in the final mother liquor, the ult rec of Mg is 90.2%.
The William stone sample ore adopts two sections adverse current hydrochloric acid extract technologies to handle with embodiment one.
One section is leached sample is 100 parts of ore samples, add 200 parts of water for ball milling after the fragmentation to accounting for 90% ore pulp that obtains less than 0.074mm, one section is leached 60 ℃ of temperature of reaction controls, and the reaction times is 60min, final leach liquor contains magnesium 82.4g/L, nickel 0.67g/L, and the pH value of solution value is 2.5; Filter cake enters two sections and leaches reaction.
Two sections leaching agents adopt 125 parts of concentrated hydrochloric acids (31%, industrial goods), and controlled temperature is 90 ℃, and blowing filters behind stirring (400rpm) the reaction 90min, filter cake washing, and wash water and filtrate merge as first section leaches the leaching agent that reacts; Metal target Ni in the chemical examination filter cake, the content of Mg, the leaching yield that calculates them successively is respectively 96.8%, 97.2%.
Nickeliferous, the magnesium leach liquor that obtains is through oxyhydroxide deironing (rate of loss of nickel, magnesium is respectively 10.5%, 7.5% in the scum), adopt 40% sodium hydroxide solution fractional precipitation then, obtain nickel hydroxide and magnesium hydroxide products respectively, the ult rec of nickel, magnesium is respectively 81.2%, 79.5%.
Embodiment 4
The William stone sample ore is with embodiment 1, changes two sections leaching agents the solution of 109 parts of concentrated nitric acids (98%, industrial goods) and 100 parts of water into, and other is with embodiment 3.
The final pH of leaching solution that obtains is 3.0, and final leached mud contains magnesium 1.06%, nickeliferous 0.005%; The leaching yield of nickel, magnesium reaches 95.8%, 98.3% respectively.
Embodiment 5
The William stone sample ore is taken from Henan nickel serpentine ore, nickeliferous 0.24%, MgO 40.8%.
Adopt two sections adverse current sulfuric acid extract technologies to handle this sample ore, institute is in steps with embodiment 1.Obtaining pH of leaching solution nickeliferous, magnesium is 2.0, and leached mud contains magnesium 1.05%, nickeliferous 0.010%; The leaching yield of nickel, magnesium reaches 96.6%, 98.7% respectively.
Claims (7)
1, the multistage counter current acid leaching process in William stone ore deposit is characterized in that, the William stone ore deposit is ground, and the first immersion of adding agent, water stir and leaches reaction, and n leaching reaction carried out in the circulation of gained leached mud; The k time leaching reacted to filter and obtained k section leached mud, and k section leach liquor, k section leached mud are recycled to next section and carry out the k+1 time leaching reaction, and k section leach liquor then is recycled to the immersion agent of the preceding paragraph as the k-1 time leaching reaction; Last immersion agent of leaching reaction is a strong acid; After leach reacting through n time, the final leach liquor of gained is the solution of required nickeliferous magnesium; Wherein, 1≤k≤n, n is not less than 2.
2, the multistage counter current acid leaching process in William stone according to claim 1 ore deposit is characterized in that, described first leaching agent is leaching agent or strong acid for the second time.
3, the multistage counter current acid leaching process in William stone according to claim 1 and 2 ore deposit is characterized in that described strong acid is selected from one or more in nitric acid, hydrochloric acid, the sulfuric acid.
4, the multistage counter current acid leaching process in William stone according to claim 1 ore deposit is characterized in that described n is 2-5, preferred 2-3.
5, the multistage counter current acid leaching process in William stone according to claim 1 ore deposit is characterized in that, it is 0-100 ℃ that each section leaches temperature of reaction.
6, the multistage counter current acid leaching process in William stone according to claim 1 ore deposit is characterized in that each section extraction time is 30min～240min, and the liquid-solid ratio between leaching agent volume and ore powder or the leached mud quality is 2.0～10.0.
7, the multistage counter current acid leaching process in William stone according to claim 1 ore deposit, it is characterized in that wash water and the n time leach liquor that described last leaching reaction wash water washs the n time leached mud gained merge the leaching agent that reacts as the n-1 time leaching.
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