CN102140576A - Method for extracting nickel and molybdenum from nickel-molybdenum ore - Google Patents
Method for extracting nickel and molybdenum from nickel-molybdenum ore Download PDFInfo
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Abstract
The invention discloses a method for extracting nickel and molybdenum from nickel-molybdenum ore, comprising the following steps of: (a) in the presence of an oxidizing agent, leaching the finely-ground nickel-molybdenum ore from an acid solution and filtering to obtain a leachate, wherein the oxidizing agent is sodium chlorate or potassium chlorate; (b) adding a first alkaline compound in the leachate, adjusting the pH value of the leachate to be 1.5-3.5 and filtering to respectively obtain a precipitation and a supernate; (c) adding a second alkaline compound in the supernate, adjusting the pH value of the supernate to be 5-7 and filtering to obtain a nickel-containing compound; and (d) leaching the precipitation in an alkali liquor, filtering to obtain a molybdenum-containing leachate, and extracting and re-extracting the molybdenum-containing leachate to obtain a molybdenum-containing compound. By using the method, the sodium chlorate or potassium chlorate is used as the oxidizing agent, the higher leaching rate of the nickel and molybdenum and the higher recovery rate of the nickel and molybdenum can be obtained.
Description
Technical field
The invention belongs to mineral extractive technique field, relate in particular to a kind of method of from nickel-molybdenum ore, extracting nickel and molybdenum.
Background technology
Nickel-molybdenum ore is a kind of multi-metal complex ore resources, mainly is distributed in China Hunan, Hubei Province, Chongqing, Guizhou Province, river, expensive, Shan, the mine belt such as sweet.Molybdenum content is about 2.5%～11% in the nickel-molybdenum ore, and nickel content is about 0.7%～7.7%, also contains other elements such as carbon, sulphur, iron.
Prior art discloses the multiple method of extracting nickel and molybdenum from nickel-molybdenum ore, as application number is that 95110744.5 Chinese patent literature discloses nickel and the molybdenum that adopts in the method separating nickel molybdenum ore that mechanical beneficiation and cryogenic selective reduction combine, at first with after crushing raw ore, ball milling, the classification, the method that adopts gravity treatment is with the initial gross separation of nickel molybdenum; Suppress nickel flotation molybdenum then; Again with ore at 400 ℃～700 ℃ following desulfurization with roasting technique, continue to select nickel after the reduction under 800 ℃～1100 ℃ the condition, this method can obtain two kinds of furnace charges, a kind of furnace charge contains molybdenum 11%, nickeliferous 2%, another kind of furnace charge contains molybdenum 3%, nickeliferous 8%.Application number is in 88102597.6 the Chinese patent literature disclosed method, at first with nickel-molybdenum ore 530 ℃～570 ℃ roastings, use vitriol oil slaking 2h～3h under heating condition then, leach 1.5h at 85 ℃ then, and add ammoniacal liquor and separate phase, obtain mother liquor; Described mother liquor is extracted the recyclable molybdenum in back, continue to obtain single nickel salt after extraction deironing, the crystallization.Application number is that 97107568.9 Chinese patent literature discloses a kind of method with yellow soda ash conversion processing separation molybdenum and nickel from black shale, at first with the black shale desulphurizing roasting, pulverizing the yellow soda ash of back adding 50% and 30% water sizes mixing, separate through pyrolytic conversion, water logging then, obtain nickel ore concentrate and the immersion liquid that contains molybdenum, immersion liquid promptly obtains the molybdic acid calcium salt through purifying, sinking after molybdenum is handled.Though above-mentioned three kinds of methods can all adopt the method for roasting to carry out desulfurization molybdenum, nickel separation and Extraction, not only need high temperature, higher to equipment requirements, and can produce SO
2, cause environmental pollution.
Application number is that 99114736.7 Chinese patent literature discloses a kind of method that adopts weak base and oxygenant that the molybdenum-nickel paragenetic ore deposit is directly leached, behind raw ore process ball milling, without roasting, with obtaining ammonium molybdate after weak base and oxygenant heating lixiviate, filtration, extraction, the reextraction, can obtain single nickel salt with the raffinate acidifying that obtains after the extraction, after concentrating, wherein, the rate of recovery of molybdenum is 80%, and the rate of recovery of nickel is 88%.Application number is that 99114737.5 Chinese patent literature discloses a kind of method that adopts diluted acid and oxygenant that the molybdenum-nickel paragenetic ore deposit is directly leached, behind raw ore process ball milling, without roasting, with obtaining ammonium molybdate after diluted acid and oxygenant heating lixiviate, extraction, the reextraction, can obtain single nickel salt with the raffinate acidifying that obtains after the extraction, after concentrating, wherein, the rate of recovery of molybdenum is 90%, and the rate of recovery of nickel is 93%.Application number is that 200610031788.8 Chinese patent literature discloses and a kind ofly the nickel-molybdenum ore of exhaling through fine grinding leached as infusion solution with basic solution, in leaching process, in ore pulp, add air, oxygen-rich air or oxygen, metallic elements such as molybdenum, tungsten, vanadium are leached, element such as nickel, copper is retained in the slag, and the leaching yield of molybdenum can reach 94%～98%.Aforesaid method all need not to carry out roasting, can not produce SO
2Contaminate environment, still, aforesaid method is lower to the rate of recovery of molybdenum and nickel, and the product purity that obtains is also lower.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is to provide a kind of method of extracting nickel and molybdenum from nickel-molybdenum ore, and method provided by the invention is higher to the rate of recovery of molybdenum and nickel, and technical process is simple, production cost is low.
The invention provides a kind of method of from nickel-molybdenum ore, extracting nickel and molybdenum, may further comprise the steps:
A) in the presence of oxygenant, the nickel-molybdenum ore stone after the fine grinding is leached in acid solution, after the filtration, obtain leach liquor, described oxygenant is sodium chlorate or Potcrate;
B) in described leach liquor, add first basic cpd, the pH value of leach liquor is transferred to 1.5～3.5, obtain respectively after the filtration precipitating and supernatant liquor;
C) in described supernatant liquor, add second basic cpd, the pH value of described supernatant liquor is transferred to 5～7, obtain nickel compound containing after the filtration;
D) described being deposited in the alkali lye leached, obtain containing the molybdenum leach liquor after the filtration, the described molybdenum leach liquor that contains through after extraction and strip handling, is obtained molybdate compound.
Preferably, the quality of described acid solution is 10%～300% of a described nickel-molybdenum ore stone quality, and described acid solution is industrial sulphuric acid or technical hydrochloric acid.
Preferably, the quality of described oxygenant is 20%～200% of a described nickel-molybdenum ore stone quality.
Preferably, in the described step a), the temperature of described leaching is 50 ℃～100 ℃, and the time of described leaching is 0.5h～5h.
Preferably, described first basic cpd is one or both in lime and the yellow soda ash.
Preferably, in the described step b), the temperature when adding described first basic cpd is 50 ℃～100 ℃, and described first basic cpd adds and leaves standstill 0.5h～3h after finishing and filter.
Preferably, described second basic cpd is sodium hydroxide or yellow soda ash.
Preferably, described step d) specifically comprises:
D1) described being deposited in 50 ℃～100 ℃ the alkali lye leached, obtain containing the molybdenum leach liquor after the filtration;
D2) with acid solution the described pH value that contains the molybdenum leach liquor is adjusted to 1～4;
D3) with the described steps d 2 of anionresin column extracting) obtain contain the molybdenum leach liquor, obtain the anion-exchange column of load molybdenum;
D4) be the anion-exchange column of the described load molybdenum of strippant wash-out with ammoniacal liquor, obtain molybdate compound.
Preferably, described steps d 1) in, described alkali lye is the mixing solutions of sodium hydroxide and yellow soda ash, and the temperature of leaching is 50 ℃～100 ℃, and the time of described leaching is 0.5h～3h.
Preferably, described steps d 4) in, the mass concentration of described ammoniacal liquor is 1%～30%.
Compared with prior art, the present invention is infusion solution with the acid solution, be under the condition of oxygenant the nickel-molybdenum ore stone after the fine grinding to be leached in Potcrate or sodium chlorate, by precipitation classification nickel is separated with molybdenum then, to with stripping molybdenum be separated by extraction again, obtain nickel compound containing and molybdate compound respectively.The present invention need not the nickel-molybdenum ore roasting, and comparatively cleaning can not produce SO
2Contaminate environment.The present invention is an oxygenant with Potcrate or sodium chlorate, and the leaching yield of molybdenum and nickel is higher; Adopt precipitation classification then, molybdenum and nickel are precipitated respectively, obtain nickel compound containing and molybdate compound after handling respectively by the pH value of regulating leach liquor, all higher to the rate of recovery of molybdenum and nickel.Experiment shows that by method provided by the invention, the yield of nickel can reach 97%, and the yield of molybdenum can reach 93%.In addition, method technical process provided by the invention is simple, and raw material is simple and easy to, and production cost is low.
Embodiment
The invention provides a kind of method of from nickel-molybdenum ore, extracting nickel and molybdenum, may further comprise the steps:
A) in the presence of oxygenant, the nickel-molybdenum ore stone after the fine grinding is leached in acid solution, after the filtration, obtain leach liquor, described oxygenant is sodium chlorate or Potcrate;
B) in described leach liquor, add first basic cpd, the pH value of leach liquor is transferred to 1.5～3.5, obtain respectively after the filtration precipitating and supernatant liquor;
C) in described supernatant liquor, add second basic cpd, the pH value of described supernatant liquor is transferred to 5～7, obtain nickel compound containing after the filtration;
D) described being deposited in the alkali lye leached, obtain containing the molybdenum leach liquor after the filtration, the described molybdenum leach liquor that contains through after extraction and strip handling, is obtained molybdate compound.
The present invention is an oxygenant with sodium chlorate or Potcrate, with the acid solution is that infusion solution leaches described nickel-molybdenum ore stone, obtains leach liquor after the filtration, by precipitation classification nickel is separated with molybdenum then, to with stripping molybdenum be separated by extraction again, obtain nickel compound containing and molybdate compound respectively.
The present invention is raw material with the nickel-molybdenum ore, and described nickel-molybdenum ore can be the ore deposit of mixing of mixing ore deposit, nickel molybdenum sulphide ores and other ores of mixing ore deposit, nickel molybdenum sulphide ores and molybdenum concentrate of nickel molybdenum sulphide ores, nickel molybdenum sulphide ores and molybdenum oxidized ore.The present invention with described nickel-molybdenum ore according to method fragmentation well known to those skilled in the art, ball milling after, promptly can be used for separating and extraction of molybdenum and nickel.According to the present invention, the particle diameter of described nickel-molybdenum ore stone is more preferably less than 0.150mm preferably less than 0.154mm, most preferably less than 0.10mm.
According to the present invention, the nickel-molybdenum ore stone behind the described ball milling leaches in acid solution under the condition that oxygenant exists, and specifically may further comprise the steps:
Nickel-molybdenum ore stone behind described ball milling adds entry pulls an oar, and obtains ore pulp;
In described ore pulp, add acid solution, in described ore pulp, slowly add oxygenant then and leach.
In described leaching process, the quality of described nickel-molybdenum ore stone and the mass ratio of described water be preferably 1: 1～and 1: 10, more preferably 1: 1～1: 8, most preferably be 1: 1～1: 5.
In described leaching process, described acid solution is preferably one or both in hydrochloric acid and the sulfuric acid, more preferably technical hydrochloric acid or industrial sulphuric acid; When described acid solution was the mixing solutions of sulfuric acid and hydrochloric acid, the present invention did not have particular restriction to the ratio of described sulfuric acid and hydrochloric acid.The quality optimization of described acid solution is 10%～300% of a described nickel-molybdenum ore stone quality, more preferably 20%～200%, most preferably be 50%～100%.
In described leaching process, described oxygenant is Potcrate or sodium chlorate, is preferably sodium chlorate; The quality optimization of described oxygenant is 20%～200% of a described nickel-molybdenum ore stone quality, more preferably 50%～150%, most preferably be 70%～100%.
For the leaching yield that makes nickel and molybdenum is bigger, described nickel-molybdenum ore stone is preferably containing under stirring condition in the acid solution of oxygenant and is leaching, and the temperature of described leaching is preferably 50 ℃～100 ℃, more preferably 60 ℃～90 ℃, most preferably is 70 ℃～80 ℃; The time of described leaching is preferably 0.5h～5h, and more preferably 1h～4h most preferably is 2h～3h.
In leaching process, molybdenum and nickel are dissolved in the acid solution under the effect of oxygenant and acid solution, and other insoluble elements are then stayed in the ore.After leaching is finished, filter the solution that obtains, obtain leach liquor.
After obtaining leach liquor, adopt precipitation classification Separation and Recovery molybdenum and nickel wherein.At first add first basic cpd in described leach liquor, the pH value of leach liquor is transferred to 1.5～3.5, make the molybdenum precipitation, obtain precipitation and supernatant liquor after the filtration respectively, wherein, be precipitated as and contain molybdenum and precipitate, supernatant liquor is the supernatant liquor that contains nickel.
Described first basic cpd is preferably one or both in lime and the yellow soda ash, more preferably lime; When described first basic cpd is the mixture of lime and yellow soda ash, the present invention to the ratio of described lime and yellow soda ash without any restriction.With first basic oxide pH value of described leach liquor is adjusted to 1.5～3.5, is preferably 2～3, the molybdenum ion in the leach liquor precipitates.In order to make molybdenum ion precipitation fully, the temperature when adding described first basic cpd is preferably 50 ℃～100 ℃, more preferably 60 ℃～90 ℃, most preferably is 70 ℃～80 ℃.After the adding of first basic cpd finishes, preferably described leach liquor is left standstill 0.5h～3h, more preferably leave standstill 1h～2.5h, after most preferably being 1.5h～2h, described leach liquor is filtered, obtain containing the precipitation and the nickeliferous supernatant liquor of molybdenum, after respectively described precipitation and supernatant liquor being handled, can obtain molybdate compound and nickel compound containing.
Add second basic cpd in the above-mentioned supernatant liquor that obtains, the pH value of described supernatant liquor is transferred to 5～7, at this moment, nickel ion precipitates, and can obtain nickel compound containing after the filtration.According to the present invention, described second basic cpd is yellow soda ash or sodium hydroxide, is preferably sodium hydroxide.With second basic cpd pH value of described supernatant liquor is adjusted to 5～7, is preferably 5.5～6.5, more preferably 5.8～6.3.According to the difference of second basic cpd, the nickel compound containing that obtains is also different, and as when second basic cpd is sodium hydroxide, the nickel compound containing that obtains is a nickel hydroxide; When second basic cpd was yellow soda ash, the nickel compound containing that obtains was a nickelous carbonate.
Contain molybdenum in the precipitation that obtains after leach liquor filters, described being deposited in the alkali lye leached, obtain containing the molybdenum leach liquor after the filtration, will describedly contain the molybdenum leach liquor through extraction and reextraction processing after, obtain molybdate compound, specifically comprise following process:
Described being deposited in 50 ℃～100 ℃ the alkali lye leached, obtain containing the molybdenum leach liquor after the filtration;
With acid solution the described pH value that contains the molybdenum leach liquor is adjusted to 1～4;
With the described pH value of anionresin column extracting be 1～4 contain the molybdenum leach liquor, obtain the anion-exchange column of load molybdenum;
With ammoniacal liquor is the anion-exchange column of the described load molybdenum of strippant wash-out, obtains molybdate compound.
In described precipitation, add alkali lye, molybdenum is wherein leached, after the filtration, obtain containing the molybdenum leach liquor.Described alkali lye is preferably the mixing solutions of sodium hydroxide and yellow soda ash, and wherein, the mass ratio of described sodium hydroxide and yellow soda ash is preferably 10: 1～and 1: 10, more preferably 8: 1～1: 8, most preferably be 5: 1～1: 5.For molybdenum is leached fully, the temperature of described leaching is preferably 50 ℃～100 ℃, more preferably 60 ℃～90 ℃, most preferably is 70 ℃～80 ℃; The time of described leaching is excellent in selecting 0.5h～3h, and more preferably 1h～2.5h most preferably is 1.5h～2h.Containing in the sedimentary process of molybdenum with the alkali lye leaching, the temperature of described leaching is the temperature of described alkali lye.
After obtaining containing the molybdenum leach liquor, the described pH value that contains the molybdenum leach liquor is adjusted to 1～4, is preferably 2～3, be convenient to the extraction of molybdenum wherein with acid solution.Described acid solution is preferably one or both in sulfuric acid and the hydrochloric acid, and when described acid solution was the mixed solution of sulfuric acid and hydrochloric acid, the present invention did not have particular restriction to the ratio of described sulfuric acid and hydrochloric acid.
After the described pH value that contains the molybdenum leach liquor is adjusted to 1～4, extraction molybdenum wherein.The present invention can be extraction agents such as TBP well known to those skilled in the art, N235 or P350 to the used extraction agent kerosene particular restriction of extraction molybdenum.The present invention preferably extracts the described molybdenum leach liquor that contains with anion-exchange column, obtains the anion-exchange column of load molybdenum.
After extracting the molybdenum that obtains containing in the molybdenum leach liquor, described extraction liquid is stripped.The present invention does not have particular restriction to described strippant, is preferably ammoniacal liquor, and the concentration of described ammoniacal liquor is preferably 1%～30%, and more preferably 5%～25%.With anion-exchange column the described molybdenum leach liquor that contains is being extracted, after obtaining the anion-exchange column of load molybdenum, be the anion-exchange column of the described load molybdenum of strippant wash-out with ammoniacal liquor preferably, obtain the molybdate compound that exists with aqueous solution form, described molybdate compound is an ammonium molybdate.
In order to improve the purity of described ammonium molybdate, the present invention preferably adds magnesium chloride and carries out removal of impurities in described ammonium molybdate solution, and the quality optimization of described magnesium chloride is 1 times～3 times of described ammonium molybdate solution quality, more preferably 1.5 times～2.5 times.
Ammonium molybdate solution after the removal of impurities is evaporated, after the crystallization, obtains ammonium molybdate crystal according to method well known to those skilled in the art.
Compared with prior art, the present invention is infusion solution with the acid solution, be under the condition of oxygenant the nickel-molybdenum ore stone after the fine grinding to be leached in Potcrate or sodium chlorate, by precipitation classification nickel is separated with molybdenum then, to with stripping molybdenum be separated by extraction again, obtain nickel compound containing and molybdate compound respectively.The present invention need not the nickel-molybdenum ore roasting, and comparatively cleaning can not produce SO
2Contaminate environment.The present invention is an oxygenant with Potcrate or sodium chlorate, and the leaching yield of molybdenum and nickel is higher; Adopt precipitation classification then, molybdenum and nickel are precipitated respectively, obtain nickel compound containing and molybdate compound after handling respectively by the pH value of regulating leach liquor, all higher to the rate of recovery of molybdenum and nickel.Experiment shows that by method provided by the invention, the yield of nickel can reach 97%, and the yield of molybdenum can reach 93%.In addition, method technical process provided by the invention is simple, and raw material is simple and easy to, and production cost is low.
In order to further specify the present invention, the method for extracting nickel and molybdenum from nickel-molybdenum ore provided by the invention is described in detail below in conjunction with embodiment.
Below among each embodiment, the molybdenum nickel minerals that nickeliferous and sulphide ores molybdenum is the western Hunan, Hunan wherein, molybdenum content is 3.5%, nickel content is 2.8%, iron level is 14%; Other each raw materials are the commercially available prod.
Embodiment 1
100g is nickeliferous and sulphide ores molybdenum is crushed to the fine ore of particle diameter less than 0.154mm, 300g water joined in the described fine ore pull an oar, add the 300g technical hydrochloric acid again, slowly add the 50g potassium perchlorate then, be warming up to 90 ℃, agitation leach 2h, obtain leach liquor after the filtration; In described leach liquor, add lime, regulate its pH value to 2 back and stir 30min, obtain rich molybdenum slag and rich nickel supernatant liquor after the filtration;
Adding yellow soda ash to pH value in described rich nickel supernatant liquor is 5, obtains throw out after the filtration; Described throw out is carried out composition analysis, and it is a nickelous carbonate, and wherein the content of nickel is 22.05%, and the yield of nickel is 96.03%;
In described rich molybdenum slag, add the making beating of 100mL water, add 50g yellow soda ash and 50g sodium hydroxide then, be heated to 70 ℃, stir 1h, obtain rich molybdenum supernatant liquor and scum after the filtration; After with sulfuric acid the pH value of described rich molybdenum liquid being adjusted to 2, cross D314 resin anion(R.A) exchange column absorption molybdenum, when molybdenum content was greater than 0.01g/L in the anion-exchange column effluent liquid, the molybdenum with in 7% the ammoniacal liquor wash-out anion-exchange column obtained thick ammonium molybdate solution; In described thick ammonium molybdate solution, add MgCl
2Removal of impurities obtains crystal after filtering, evaporating, and described crystal is carried out composition analysis, and it is an ammonium molybdate, and wherein the content of molybdenum is 58.32%, and the yield of molybdenum is 92.85%.
Embodiment 2
100g is nickeliferous and sulphide ores molybdenum is crushed to the fine ore of particle diameter less than 0.154mm, 300g water joined in the described fine ore pull an oar, add the 300g industrial sulphuric acid again, slowly add the 50g sodium perchlorate then, be warming up to 90 ℃, agitation leach 2h, obtain leach liquor after the filtration; In described leach liquor, add industrial sodium carbonate, regulate its pH value to 4 back and stir 30min, obtain rich molybdenum slag and rich nickel supernatant liquor after the filtration;
Adding yellow soda ash to pH value in described rich nickel supernatant liquor is 7, obtains throw out after the filtration; Described throw out is carried out composition analysis, and it is a nickelous carbonate, and wherein the content of nickel is 21.83%, and the yield of nickel is 96.57%;
In described rich molybdenum slag, add the making beating of 100mL water, add 50g yellow soda ash and 50g sodium hydroxide then, be heated to 90 ℃, stir 1h, obtain rich molybdenum supernatant liquor and scum after the filtration; After with sulfuric acid the pH value of described rich molybdenum liquid being adjusted to 4, cross D314 resin anion(R.A) exchange column absorption molybdenum, when molybdenum content was greater than 0.01g/L in the anion-exchange column effluent liquid, the molybdenum with in 7% the ammoniacal liquor wash-out anion-exchange column obtained thick ammonium molybdate solution; In described thick ammonium molybdate solution, add MgCl
2Removal of impurities obtains crystal after filtering, evaporating, and described crystal is carried out composition analysis, and it is an ammonium molybdate, and wherein the content of molybdenum is 61.21%, and the yield of molybdenum is 93.13%.
Embodiment 3
100g is nickeliferous and sulphide ores molybdenum is crushed to the fine ore of particle diameter less than 0.154mm, 500g water joined in the described fine ore pull an oar, add the 500g technical hydrochloric acid again, slowly add the 100g potassium perchlorate then, be warming up to 90 ℃, agitation leach 2h, obtain leach liquor after the filtration; In described leach liquor, add lime, regulate its pH value to 3 back and stir 30min, obtain rich molybdenum slag and rich nickel supernatant liquor after the filtration;
Adding yellow soda ash to pH value in described rich nickel supernatant liquor is 6, obtains throw out after the filtration; Described throw out is carried out composition analysis, and it is a nickelous carbonate, and wherein the content of nickel is 22.79%, and the yield of nickel is 97.16%;
In described rich molybdenum slag, add the making beating of 100mL water, add 50g yellow soda ash and 50g sodium hydroxide then, be heated to 80 ℃, stir 1h, obtain rich molybdenum supernatant liquor and scum after the filtration; After with sulfuric acid the pH value of described rich molybdenum liquid being adjusted to 2, cross D314 resin anion(R.A) exchange column absorption molybdenum, when molybdenum content was greater than 0.01g/L in the anion-exchange column effluent liquid, the molybdenum with in 7% the ammoniacal liquor wash-out anion-exchange column obtained thick ammonium molybdate solution; In described thick ammonium molybdate solution, add MgCl
2Removal of impurities obtains crystal after filtering, evaporating, and described crystal is carried out composition analysis, and it is an ammonium molybdate, and wherein the content of molybdenum is 59.96%, and the yield of molybdenum is 92.86%.
Embodiment 4
100g is nickeliferous and sulphide ores molybdenum is crushed to the fine ore of particle diameter less than 0.154mm, 300g water joined in the described fine ore pull an oar, adding total mass again is the technical hydrochloric acid of 200g and the mixing acid of industrial sulphuric acid, wherein the volume ratio of technical hydrochloric acid and industrial sulphuric acid is 1: 1, slowly add the 50g sodium perchlorate then, be warming up to 90 ℃, agitation leach 2h, obtain leach liquor after the filtration; In described leach liquor, add lime, regulate its pH value to 3.5 back and stir 30min, obtain rich molybdenum slag and rich nickel supernatant liquor after the filtration;
Adding yellow soda ash to pH value in described rich nickel supernatant liquor is 6.5, obtains throw out after the filtration; Described throw out is carried out composition analysis, and it is a nickelous carbonate, and wherein the content of nickel is 20.95%, and the yield of nickel is 95.93%;
In described rich molybdenum slag, add the making beating of 100mL water, add 50g yellow soda ash and 50g sodium hydroxide then, be heated to 70 ℃, stir 1h, obtain rich molybdenum supernatant liquor and scum after the filtration; After with sulfuric acid the pH value of described rich molybdenum liquid being adjusted to 2, cross D314 resin anion(R.A) exchange column absorption molybdenum, when molybdenum content was greater than 0.01g/L in the anion-exchange column effluent liquid, the molybdenum with in 7% the ammoniacal liquor wash-out anion-exchange column obtained thick ammonium molybdate solution; In described thick ammonium molybdate solution, add MgCl
2Removal of impurities obtains crystal after filtering, evaporating, and described crystal is carried out composition analysis, and it is an ammonium molybdate, and wherein the content of molybdenum is 60.79%, and the yield of molybdenum is 93.35%.
The above only is a preferred implementation of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. method of extracting nickel and molybdenum from nickel-molybdenum ore may further comprise the steps:
A) in the presence of oxygenant, the nickel-molybdenum ore stone after the fine grinding is leached in acid solution, after the filtration, obtain leach liquor, described oxygenant is sodium chlorate or Potcrate;
B) in described leach liquor, add first basic cpd, the pH value of leach liquor is transferred to 1.5～3.5, obtain respectively after the filtration precipitating and supernatant liquor;
C) in described supernatant liquor, add second basic cpd, the pH value of described supernatant liquor is transferred to 5～7, obtain nickel compound containing after the filtration;
D) described being deposited in the alkali lye leached, obtain containing the molybdenum leach liquor after the filtration, the described molybdenum leach liquor that contains through after extraction and strip handling, is obtained molybdate compound.
2. method according to claim 1 is characterized in that, the quality of described acid solution is 10%～300% of a described nickel-molybdenum ore stone quality, and described acid solution is industrial sulphuric acid or technical hydrochloric acid.
3. method according to claim 1 is characterized in that, the quality of described oxygenant is 20%～200% of a described nickel-molybdenum ore stone quality.
4. method according to claim 1 is characterized in that, in the described step a), the temperature of described leaching is 50 ℃～100 ℃, and the time of described leaching is 0.5h～5h.
5. method according to claim 1 is characterized in that, described first basic cpd is one or both in lime and the yellow soda ash.
6. method according to claim 5 is characterized in that, in the described step b), the temperature when adding described first basic cpd is 50 ℃～100 ℃, and described first basic cpd adds and leaves standstill 0.5h～3h after finishing and filter.
7. method according to claim 1 is characterized in that, described second basic cpd is sodium hydroxide or yellow soda ash.
8. method according to claim 1 is characterized in that, described step d) specifically comprises:
D1) described being deposited in 50 ℃～100 ℃ the alkali lye leached, obtain containing the molybdenum leach liquor after the filtration;
D2) with acid solution the described pH value that contains the molybdenum leach liquor is adjusted to 1～4;
D3) with the described steps d 2 of anionresin column extracting) obtain contain the molybdenum leach liquor, obtain the anion-exchange column of load molybdenum;
D4) be the anion-exchange column of the described load molybdenum of strippant wash-out with ammoniacal liquor, obtain molybdate compound.
9. method according to claim 8 is characterized in that, described steps d 1) in, described alkali lye is the mixing solutions of sodium hydroxide and yellow soda ash, and the temperature of leaching is 50 ℃～100 ℃, and the time of described leaching is 0.5h～3h.
10. method according to claim 8 is characterized in that, described steps d 4) in, the mass concentration of described ammoniacal liquor is 1%～30%.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102560102A (en) * | 2012-01-18 | 2012-07-11 | 长沙矿冶研究院有限责任公司 | Method for leaching nickel and molybdenum from nickel-molybdenum ores by catalytic oxidation |
| CN102676803A (en) * | 2012-06-05 | 2012-09-19 | 南京元泰环保科技有限公司 | Resource utilization method for catalytic oxidation leaching of molybdenum and nickel from molybdenum-nickel ore |
| CN105925796A (en) * | 2016-04-29 | 2016-09-07 | 昆明理工大学 | Method for separating and recycling nickel-molybdenum iron from black rock series nickel-molybdenum iron sulfide ores |
| CN109022787A (en) * | 2018-11-05 | 2018-12-18 | 中南大学 | The method of nickel molybdenum is extracted from nickel-molybdenum ore acid leaching solution |
| CN109837393A (en) * | 2019-01-31 | 2019-06-04 | 中南大学 | A kind of selective recovery is given up the method for valuable metal in hydrogenation catalyst |
| CN115043434A (en) * | 2022-08-03 | 2022-09-13 | 贵州金瑞新材料有限责任公司 | Manganese sulfate production system based on manganese oxide ore |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102560102A (en) * | 2012-01-18 | 2012-07-11 | 长沙矿冶研究院有限责任公司 | Method for leaching nickel and molybdenum from nickel-molybdenum ores by catalytic oxidation |
| CN102560102B (en) * | 2012-01-18 | 2014-02-12 | 长沙矿冶研究院有限责任公司 | Method for leaching nickel and molybdenum from nickel-molybdenum ores by catalytic oxidation |
| CN102676803A (en) * | 2012-06-05 | 2012-09-19 | 南京元泰环保科技有限公司 | Resource utilization method for catalytic oxidation leaching of molybdenum and nickel from molybdenum-nickel ore |
| CN105925796A (en) * | 2016-04-29 | 2016-09-07 | 昆明理工大学 | Method for separating and recycling nickel-molybdenum iron from black rock series nickel-molybdenum iron sulfide ores |
| CN109022787A (en) * | 2018-11-05 | 2018-12-18 | 中南大学 | The method of nickel molybdenum is extracted from nickel-molybdenum ore acid leaching solution |
| CN109837393A (en) * | 2019-01-31 | 2019-06-04 | 中南大学 | A kind of selective recovery is given up the method for valuable metal in hydrogenation catalyst |
| CN115043434A (en) * | 2022-08-03 | 2022-09-13 | 贵州金瑞新材料有限责任公司 | Manganese sulfate production system based on manganese oxide ore |
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