CN105838882A - Separation and recovery process for molybdenum and nickel in nickel-molybdenum associated ore oxygen pressure acid leaching liquid - Google Patents
Separation and recovery process for molybdenum and nickel in nickel-molybdenum associated ore oxygen pressure acid leaching liquid Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching processes
- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
- C22B23/0461—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/42—Treatment or purification of solutions, e.g. obtained by leaching by ion-exchange extraction
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/34—Obtaining molybdenum
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Abstract
The invention discloses a separation and recovery process for molybdenum and nickel in a nickel-molybdenum associated ore oxygen pressure acid leaching liquid. The separation and recovery process comprises the following steps: (1) nickel-molybdenum associated ore is adopted for neutralization and reduction of a stage I oxygen pressure acid leaching liquid which is obtained from pressure leaching, so that the final acid concentration and the Fe ion concentration in the oxygen pressure acid leaching liquid are effectively reduced below 1 g/L, wherein no other neutralizers need to be added and the loss of nickel-molybdenum main metal is avoided; (2) when the pH value of the obtained neutralization solution is 2.0-3.0, anion resin can be directly adopted for Mo exchange, so that the Mo recovery rate can reach up to 99% or above and the grade of an ammonium molybdate product can be effectively improved to be higher than 95%; and (3) a precipitant is adopted in a solution obtained after the exchange for copper nickel precipitation, so that copper nickel can be recovered and the copper nickel recovery rate can exceed 95%.
Description
Technical field
The invention belongs to non-ferrous metal metallurgy technical field, be specifically related to molybdenum nickel in a kind of nickel-molybdenum symbiotic ore oxygen pressure acid steep
Process for separating and recovering.
Background technology
In the Hunan of China, Guizhou Province, river, Chongqing, Hubei Province, osmanthus, Shan, sweet etc. province contain a molybdenum nickel minerals band up to 1600km.This
Plant mineral reserve and be referred to as bone coal in the past by local common people, and be produced for baking bricks.Molybdenum nickel minerals, in addition to containing molybdenum and nickel, goes back association
There are the valuable elements such as zinc, vanadium, silver, selenium.Because minerogentic condition and geographical position are different, the valuable element of this mineral reserve association is the most not to the utmost
Identical, some place is based on molybdenum, though if the ground such as North Western Hunan, Guizhou Province, osmanthus, Chongqing are based on molybdenum, being the most also associated with nickel, becoming molybdenum nickel
Mineral intergrowth, therefore it is referred to as molybdenum nickel minerals, nickel-molybdenum ore or carbon molybdenum ore by locality.This mineral reserve distribution area containing molybdenum, nickel is big, and
Molybdenum, nickel grade the highest, molybdenum grade is 2%～11%, and nickel content is generally 35% ~ 70% (grade is 0.7% ~ 7.7%) of molybdenum content,
High person's molybdenum nickel ratio reaches 1: 1 (molybdenum mining grade is 0.1%, and nickel is 0.2%)；Additionally, the molybdenum nickel minerals in some place is based on vanadium, such as lake
The Huaihua region in south.Owing to resource reserve is huge and the highest very big pass causing domestic and international mining industry expert of metal content such as molybdenum nickel
Note, if the scientist of the U.S. is by the joint study with domestic and international scientific research personnel, has delivered this ore deposit origin cause of formation relevant, ore deposit phase, composition
Etc. the achievement in research report of aspect, and inquired into the possibility forming similar mineral deposit in the U.S., America.
The process technique of nickel-molybdenum symbiotic ore be broadly divided into ore-dressing technique, selecting smelting combination technique, oxidizing roasting-water logging technique,
Sulfating roasting-normal pressure acid leaching process, desulfurization with roasting technique-sodium hypochlorite intensified leaching process, sodium roasting-water logging-ultrasonic wave are strong
Change acid leaching process, add calcium oxidizing roasting-Sulfur-Vapor of Lower Temperature acidizing fired-water logging technique, liquor natrii hypochloritis's mechanical activation leaching
Technique, normal pressure alkaline leaching technique, hydrochloric acid Oxidation Leaching-acid leaching residue alkali soaking technology, nitric acid pressurized acid leaching technique, alkalescence pressurised oxygen
Change-acid pressure oxidation extract technology etc..And these techniques all also exist some problems, nickel molybdenum can not be carried out by ore-dressing technique
Effective enrichment；Selecting smelting combination technique, must also carry out traditional roasting-leaching after ore dressing and be proceeded in solution by nickel molybdenum；
And the roasting-extract technology of main flow is all first Leaching Molybdenum from nickel-molybdenum ore, the most again extraction nickel from leached mud, roasting by roasting
SO during burning2The problem such as gaseous contamination, main metal molybdenum nickel recovery are the highest；Hydrochloric acid, nitric acid pressure leaching process all also exist
The etching problem of equipment；Alkalescence pressure leaching process also exists the problem that alkali consumption is big；And one section of oxygen pressure acid leaching process also exists
Leachate acid eventually is high, iron concentration is high, solution processing cost is high and iron dross removing carries the drawbacks such as Mo loss is big secretly.
Two sections of oxygen pressure acidleach-normal pressure alkali soaking technologies can effectively carry out nickel molybdenum recovery, and the pressure acid of I section oxygen to nickel-molybdenum symbiotic ore
Acid eventually in immersion liquid, the nickel molybdenum separation and recovery that iron concentration is low, follow-up.Although two sections of oxygen pressure acid leaching process can be the most real
The leaching of existing nickel molybdenum, but the nickel molybdenum in leachate separates not thorough or separating effect is bad, affects the synthetical recovery profit of nickel molybdenum
With.Therefore, the present invention is directed to current I section oxygen pressure acid steep and develop nickel molybdenum process for separating and recovering, efficiently solve nickel molybdenum symbiosis
The comprehensive resource in ore deposit recycles problem.
Summary of the invention
It is an object of the invention to provide separating molybdenum from nickel recovery process in a kind of nickel-molybdenum symbiotic ore oxygen pressure acid steep.
The object of the present invention is achieved like this, comprises the steps:
(1) I section of oxygen pressure acid steep pressure leaching obtained and nickel-molybdenum symbiotic ore liquid-solid ratio be 3 ~ 7:1, temperature be 20 ~ 60
DEG C, be neutralized reduction under conditions of time 10 ~ 120min, obtain neutralizing slag and neutralizer；
(2) neutralizer uses anion exchange resin to carry out Mo ion exchange, obtains carrying liquid after molybdenum resin and exchange；
(3) it is aged after carrying the scrubbed acid adjustment of molybdenum resin, digestion time 1 ~ 4h, after ageing, carries out solid-liquor separation, obtain ammonium molybdate and produce
Liquid after product and heavy molybdenum, after heavy molybdenum, liquid return ion-exchange process is used for washing load molybdenum resin；
(4) liquid after exchange is added precipitating reagent precipitation temperature be 10 ~ 90 DEG C, the sedimentation time be 0.5h ~ 4h, precipitation terminal pH
Value is to carry out copper nickel precipitation under the conditions of 5.0, and copper precipitates in the way of basic copper carbonate, Kocide SD or cupric oxalate, and nickel is with carbonic acid
The mode of nickel, nickel hydroxide or nickel oxalate precipitates, thus prepares corresponding copper, nickel product；
(5) neutralize I section of oxygen pressure acidleach operation of slag return and carry out nickel molybdenum recovery.
The beneficial effect that the present invention produces:
(1) I section of oxygen pressure acid steep uses nickel-molybdenum symbiotic ore to be neutralized reduction, significantly reduces the end in oxygen pressure acid steep
< 1g/L, without the need for adding other nertralizers, it is to avoid the loss of the main metal of nickel molybdenum for acid, Fe ion concentration.
(2) neutralizer pH value is 2.0 ~ 3.0, can directly use resin anion (R.A.) exchange Mo, Mo the rate of recovery be up to 99% with
On, it is effectively improved ammonium molybdate product grade > 95%.
(3) after exchange, liquid uses precipitating reagent to sink copper nickel, it is achieved that the recovery of copper nickel, copper nickel recovery > 95%.
Accompanying drawing explanation
Fig. 1 is the process chart of the present invention.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described, but is any limitation as the present invention never in any form, base
In present invention teach that any conversion made, each fall within scope.
The present invention comprises the steps:
(1) I section of oxygen pressure acid steep pressure leaching obtained and nickel-molybdenum symbiotic ore liquid-solid ratio be 3 ~ 7:1, temperature be 20 ~ 60
DEG C, be neutralized reduction under conditions of time 10 ~ 120min, make the Fe in I section of oxygen pressure acid steep3+1g/L is down in reduction, whole acid
Below, pH value be 2.0 ~ 3.0, obtain neutralizing slag and neutralizer；
(2) neutralizer uses anion exchange resin to carry out Mo ion exchange, obtains carrying liquid after molybdenum resin and exchange；Anion
Exchanger resin reaction mechanism such as formula 1:
2R-Cl+MO4 2-= R- MO4-R+2Cl-(formula 1)
(3) it is aged after carrying the scrubbed acid adjustment of molybdenum resin, digestion time 1 ~ 4h, after ageing, carries out solid-liquor separation, obtain ammonium molybdate and produce
Liquid after product and heavy molybdenum, after heavy molybdenum, liquid return ion-exchange process is used for washing load molybdenum resin；
(4) liquid after exchange is added precipitating reagent precipitation temperature be 10 ~ 90 DEG C, the sedimentation time be 0.5h ~ 4h, precipitation terminal pH
Value is to carry out copper nickel precipitation under the conditions of 5.0, and copper precipitates in the way of basic copper carbonate, Kocide SD or cupric oxalate, and nickel is with carbonic acid
The mode of nickel, nickel hydroxide or nickel oxalate precipitates, thus prepares corresponding copper, nickel product；Heavy copper nickel reactant such as (formula 2)-(formula 6):
2NaOH+Ni2+=Ni (OH)2 +2Na+(formula 2)
Ca(OH)2+Ni2+=Ni (OH)2 +Ca2+(formula 3)
CaO+H2O+Ni2+=Ni (OH)2 +Ca2+(formula 4)
Na2CO3+Ni2+=Ni CO3 +2Na+(formula 5)
Ni2++H2C2O4= Ni C2O4 +2H+(formula 6)
(5) neutralize I section of oxygen pressure acidleach operation of slag return and carry out nickel molybdenum recovery.
Nickel-molybdenum symbiotic ore oxygen pressure acid steep composition is: Mo 3 ~ 10g/L, Ni 3 ~ 15g/L, Fe 1 ~ 3 g/L, H2SO4 2~
15g/L、Cu 0.2~1 g/L。
Anion exchange resin in described step (2) includes: D501, D231,711,401S, 330, the highly basic such as A1003
Property ion exchange resin, swap time be 1 ~ 60min, exchange temperature is 10 ~ 90 DEG C, flow is 0.1L/min ~ 100L/min, friendship
Change column dimension be φ 200mm × 2000mm, pH value be 2.0 ~ 3.5.
Precipitating reagent in described step (4), including: NaOH, Ca (OH)2、CaO、Na2CO3Or H2C2O4In one or several
Kind.
Embodiment 1
The nickel-molybdenum symbiotic ore oxygen pressure acid steep composition of the present embodiment is: Mo 5.75g/L, Ni 12.53g/L, Fe 2.45 g/L,
H2SO4 5.31g/L、Cu 0.42g/L。
The I section of oxygen pressure acid steep 600L first, obtained by pressure leaching adds nickel-molybdenum symbiotic ore 200kg, temperature is 45 DEG C,
Time is to be neutralized reduction under conditions of 30min, makes the Fe in I section of oxygen pressure acid steep3+Reduction, whole acid be down to below 1g/L,
Endpoint pH is 2.5.Then carry out solid-liquor separation to obtain neutralizing slag and neutralizer.Neutralize slag and return one section of oxygen pressure acidleach operation,
Neutralizer carries out nickel molybdenum recovery, and neutralizer composition is: Mo 6.01g/L, Ni 12.66g/L, Fe 0.87 g/L, H2SO40.69g/
L、Cu 0.43g/L。
Secondly, neutralizer carrying out Mo ion exchange, exchanger resin is D501 anion exchange resin, swap time to be
40min, exchange temperature are 40 DEG C, flow is 15L/min, exchange column a size of φ 200mm × 2000mm, pH value is 2.5.
Above-mentioned load molybdenum resin is aged after resolving acid adjustment, digestion time 2h, carries out solid-liquor separation after ageing, obtain molybdic acid
Liquid after ammonium product and heavy molybdenum, after heavy molybdenum, liquid return ion-exchange process is used for washing load molybdenum resin, and ammonium molybdate content is 95.73%.
Ion is exchanged the neutralizer after Mo and adds precipitating reagent Na2CO3, precipitation temperature be 30 DEG C, the sedimentation time be
Under conditions of 2h, precipitation endpoint pH are 5.0, copper nickel precipitates with the form of nickelous carbonate, basic copper carbonate, thus prepares corresponding copper
In nickel product, gained nickelous carbonate and basic carbonate copper products nickel content be 36.78%, copper content be 3.45%.Neutralize slag and return I section
Oxygen pressure acidleach operation carries out nickel molybdenum recovery.
Embodiment 2
The nickel-molybdenum symbiotic ore oxygen pressure acid steep composition of the present embodiment is: Mo 6.35g/L, Ni 14.15g/L, Fe 2.73 g/L,
H2SO4 4.85g/L、Cu 0.68g/L。
The I section of oxygen pressure acid steep 600L first, obtained by pressure leaching adds nickel-molybdenum symbiotic ore 150kg, temperature is 60 DEG C,
Time is to be neutralized reduction under conditions of 20min, makes the Fe in I section of oxygen pressure acid steep3+Reduction, whole acid be down to below 1g/L,
PH value is 2.5.Then carry out solid-liquor separation to obtain neutralizing slag and neutralizer.Neutralize slag and return one section of oxygen pressure acidleach operation, neutralize
Liquid carries out nickel molybdenum recovery, and neutralizer composition is: Mo 7.03g/L, Ni 14.33g/L, Fe 0.93 g/L, H2SO40.78g/L、Cu
0.71g/L。
Neutralizer is carried out Mo ion exchange, exchanger resin be 401S anion exchange resin, swap time be 30min,
Exchange temperature is 60 DEG C, flow is 20L/min, exchange column a size of φ 200mm × 2000mm, pH value is 2.5.
Above-mentioned load molybdenum resin is aged after resolving acid adjustment, digestion time 1h, carries out solid-liquor separation after ageing, obtain molybdic acid
Liquid after ammonium product and heavy molybdenum, after heavy molybdenum, liquid return ion-exchange process is used for washing load molybdenum resin, and ammonium molybdate content is 96.81%.
Ion is exchanged the neutralizer after Mo and adds precipitating reagent H2C2O4, precipitation temperature be 60 DEG C, the sedimentation time be
Under conditions of 1h, precipitation endpoint pH are 5.0, copper nickel precipitates with the form of nickel oxalate, cupric oxalate, thus prepares corresponding copper nickel and produce
In product, gained nickel oxalate and cupric oxalate product nickel content be 40.12%, copper content be 3.71%.Neutralize slag and return I section of oxygen pressure acidleach
Operation carries out nickel molybdenum recovery.
Embodiment 3
The nickel-molybdenum symbiotic ore oxygen pressure acid steep composition of the present embodiment is: Mo 5.13g/L, Ni 13.79g/L, Fe 2.01 g/L,
H2SO4 3.12g/L、Cu 0.37g/L。
The I section of oxygen pressure acid steep 600L first, obtained by pressure leaching adds nickel-molybdenum symbiotic ore 100kg, temperature is 50 DEG C,
Time is to be neutralized reduction under conditions of 20min, makes the Fe in I section of oxygen pressure acid steep3+Reduction, whole acid be down to below 1g/L,
PH value is 2.5.Then carry out solid-liquor separation to obtain neutralizing slag and neutralizer.Neutralize slag and return one section of oxygen pressure acidleach operation, neutralize
Liquid carries out nickel molybdenum recovery, and neutralizer composition is: Mo 5.41g/L, Ni 13.92g/L, Fe 0.82 g/L, H2SO40.91g/L、Cu
0.40g/L。
Neutralizer is carried out Mo ion exchange, exchanger resin be 711 anion exchange resin, swap time be 15min, friendship
Change temperature be 40 DEG C, flow be 40L/min, exchange column a size of φ 200mm × 2000mm, pH value be 3.0.
Above-mentioned load molybdenum resin is aged after resolving acid adjustment, digestion time 3h, carries out solid-liquor separation after ageing, obtain molybdic acid
Liquid after ammonium product and heavy molybdenum, after heavy molybdenum, liquid return ion-exchange process is used for washing load molybdenum resin, and ammonium molybdate content is 92.13%.
Ion is exchanged neutralizer after Mo and adds precipitating reagent CaO, precipitation temperature be 80 DEG C, the sedimentation time be 3h,
Under conditions of precipitation endpoint pH is 5.0, copper nickel precipitates with the form of nickel hydroxide, Kocide SD, thus prepares corresponding copper nickel
In product, gained nickel hydroxide and Kocide SD product nickel content be 31.35%, copper content be 2.14%.Neutralize slag and return I section of oxygen
Pressure acidleach operation carries out nickel molybdenum recovery.
Claims (4)
1. separating molybdenum from nickel recovery process in a nickel-molybdenum symbiotic ore oxygen pressure acid steep, it is characterised in that comprise the steps:
(1) I section of oxygen pressure acid steep pressure leaching obtained and nickel-molybdenum symbiotic ore liquid-solid ratio be 3 ~ 7:1, temperature be 20 ~ 60
DEG C, be neutralized reduction under conditions of time 10 ~ 120min, obtain neutralizing slag and neutralizer；
(2) neutralizer uses anion exchange resin to carry out Mo ion exchange, obtains carrying liquid after molybdenum resin and exchange；
(3) it is aged after carrying the scrubbed acid adjustment of molybdenum resin, digestion time 1 ~ 4h, after ageing, carries out solid-liquor separation, obtain ammonium molybdate and produce
Liquid after product and heavy molybdenum, after heavy molybdenum, liquid return ion-exchange process is used for washing load molybdenum resin；
(4) liquid after exchange is added precipitating reagent precipitation temperature be 10 ~ 90 DEG C, the sedimentation time be 0.5h ~ 4h, precipitation terminal pH
Value is to carry out copper nickel precipitation under the conditions of 5.0, and copper precipitates in the way of basic copper carbonate, Kocide SD or cupric oxalate, and nickel is with carbonic acid
The mode of nickel, nickel hydroxide or nickel oxalate precipitates, thus prepares corresponding copper, nickel product；
(5) neutralize I section of oxygen pressure acidleach operation of slag return and carry out nickel molybdenum recovery.
Separating molybdenum from nickel recovery process in nickel-molybdenum symbiotic ore oxygen pressure acid steep the most according to claim 1, it is characterised in that nickel
Molybdenum symbiotic ore oxygen pressure acid steep composition is: Mo 3 ~ 10g/L, Ni 3 ~ 15g/L, Fe 1 ~ 3 g/L, H2SO4 2~15g/L、Cu 0.2
~1 g/L。
Separating molybdenum from nickel recovery process in nickel-molybdenum symbiotic ore oxygen pressure acid steep the most according to claim 1, it is characterised in that institute
The anion exchange resin stated in step (2) includes: D501, D231,711,401S, 330, the exchange of the strong basic ion such as A1003
Resin, swap time be 1 ~ 60min, exchange temperature is 10 ~ 90 DEG C, flow be 0.1L/min ~ 100L/min, exchange column a size of
φ 200mm × 2000mm, pH value are 2.0 ~ 3.5.
Separating molybdenum from nickel recovery process in nickel-molybdenum symbiotic ore oxygen pressure acid steep the most according to claim 1, it is characterised in that institute
State the precipitating reagent in step (4), including: NaOH, Ca (OH)2、CaO、Na2CO3Or H2C2O4In one or more.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108342591A (en) * | 2018-02-11 | 2018-07-31 | 眉山顺应动力电池材料有限公司 | A kind of molybdenum copper novel method for separating |
| CN111363927A (en) * | 2020-04-27 | 2020-07-03 | 北京理工大学 | Method for recycling electroplating sludge based on nickel recovery |
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| CN105002354A (en) * | 2015-07-28 | 2015-10-28 | 昆明理工大学 | Method for leaching zinc and other valuable metal in zinc sulfide ore through medium-and-low-pressure oxygen enrichment |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108342591A (en) * | 2018-02-11 | 2018-07-31 | 眉山顺应动力电池材料有限公司 | A kind of molybdenum copper novel method for separating |
| CN108342591B (en) * | 2018-02-11 | 2019-12-20 | 眉山顺应动力电池材料有限公司 | New method for separating molybdenum and copper |
| CN111363927A (en) * | 2020-04-27 | 2020-07-03 | 北京理工大学 | Method for recycling electroplating sludge based on nickel recovery |
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