CN108796228A - A kind of niobium element recycling process of enriching - Google Patents

A kind of niobium element recycling process of enriching Download PDF

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Publication number
CN108796228A
CN108796228A CN201810732922.XA CN201810732922A CN108796228A CN 108796228 A CN108796228 A CN 108796228A CN 201810732922 A CN201810732922 A CN 201810732922A CN 108796228 A CN108796228 A CN 108796228A
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China
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niobium
base metal
acid
slag
technique
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CN201810732922.XA
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Chinese (zh)
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不公告发明人
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李雅丽
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00Obtaining refractory metals
    • C22B34/20Obtaining niobium, tantalum or vanadium
    • C22B34/24Obtaining niobium or tantalum
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006Wet processes
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25CPROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C1/00Electrolytic production, recovery or refining of metals by electrolysis of solutions

Abstract

The present invention relates to a kind of niobium elements to recycle process of enriching, by pre-processing ball milling slag, Control granularity, base metal is removed using mixing acidleach, again by the way of sodium carbonate roasting, fired slags are passed through into water logging and twice hydrochloric acid leaching process, further remove impurity metallic elements, obtained niobium enrichment slag hydrofluoric acid, which leaches, obtains feed liquid containing niobium.Meanwhile electrolytic recovery is carried out to the filtrate containing base metal, different base metal elements are recycled by control of Electric potentials, to realize high efficiente callback valuable metal, avoid the wasting of resources, the rate of recovery is high, and cost recovery is low, has significant economic benefit and social benefit.

Description

A kind of niobium element recycling process of enriching

Technical field

The present invention relates to metal recovery fields, are a kind of niobium element recycling process of enriching specifically.

Background technology

China's niobium zirconium Ores grade is low, and disseminated grain size is thin and disperses, be often associated with tantalum, lithium, beryllium, caesium, rubidium, potassium, The various metals such as sodium.Most of niobium zirconium deposit grade is all close or slightly above minimum economic ore grade index, Nb2O5Grade is more than 0.1% mineral deposit for also there was only several carbonatite types, other types mineral deposit Nb2O5Grade is only 0.02% or so.Due to niobium zirconium mine Middle content of niobium is generally very low, general in ore dressing process that gravity separation technology is used to abandon most of gangue mineral first, thus to obtain niobium Rough concentrate.In entire ore dressing process, by gravity treatment, magnetic separation, flotation or multiple steps such as select smelting, a large amount of slags, mine will produce Inevitably carry some niobium-containing minerals in slag secretly, it is clear that be a kind of available secondary resource, causing niobium metal element if abandoning Serious loss and the wasting of resources, therefore, reinforcing the recycling of niobium element in slag containing niobium minerals just seems particularly significant.

Invention content

In order to solve the above technical problem, the present invention provides a kind of niobium elements to recycle process of enriching, and this method can carry The high niobium rate of recovery reduces cost recovery, avoids the wasting of resources, and it is nervous to alleviate niobium resource.

A kind of niobium element recycling process of enriching, the described method comprises the following steps:

1)Association niobium zirconium mine metallurgical slag acid adding is leached, the addition for controlling acid solution is according to liquid volume and slag mass ratio 25~35g/L, extraction temperature are 80~90 DEG C, and when Leach reaction is stirred with the rotating speed of 300~800r/min, the acid solution For the mixed acid of sulfuric acid and hydrochloric acid, sulfuric acid concentration is 0.5~1.0mol/L, and concentration of hydrochloric acid is 1.5~3.0mol/L, and acid solution adds Enter sequence for 0.5~1h of sulfuric acid reaction is first added, adds hydrochloric acid and continue 2~3h of leaching;

2)After Leach reaction, niobium concentration is down to 50mg/L hereinafter, filtrate Direct Electrolysis produces low-priced gold in filtered filtrate Belong to;Filter residue is the thick niobium of mass percentage content >=85%;

3)It after filter residue is dried, while adding additive and being roasted with solid state N aOH, additive dosage is solid state N aOH's 0.5~2.0wt%, solid state N aOH are 2~3 times of niobium mole in thick niobium, and calcination temperature is that 1~2h is reacted at 380~450 DEG C;

4)Slag carries out water logging after roasting, twice using salt Ore Leaching by water logging slag, a concentration of 0.5~2mol/L of hydrochloric acid, and twice The hydrofluoric acid that filter residue after leaching reuses 10~12mol/L is separated by solid-liquid separation, and extraction temperature is 80~100 DEG C, is leached Time is 1~2h, and leachate is the feed liquid as niobium extraction and separation, is contained in the feed liquid:93~96wt% of Nb.

The acid adding first pre-processes slag before leaching.

The pretreatment for by association niobium zirconium mine metallurgical slag it is broken after, carry out ball milling, it is levigate to account for granularity -0.074mm 80~90%.

Slag after the ball milling is sieved, Sieving and casing is controlled<0.048mm.

The additive added in the step 3 is Na2CO3Or NaHCO3Or the mixture of the two.

Solid-liquid separation method in the step 4 includes plate compression, centrifugation or membrane filtration.

The step of electrolysis production base metal in the step 2 is:Positive and negative electrode and electrode plate are inserted into the filtrate Spacing is 2~8cm, and cell reaction temperature is 20~50 DEG C, and DC current flow density is 900~1200A/m2, by different Control of Electric potentials is sequentially depositing the base metal for obtaining different element species on cathode.

Each described base metal sedimentation time is 2~3h, after the base metal deposition under a current potential is complete, is taken immediately Going out deposition has the cathode of the base metal, is reentered into new cathode and continues to deposit other base metal elements.

Successively cleaning described deposit using tap water, absolute ethyl alcohol and deionized water has the cathode of base metal to cleaning solution pH It is in neutrality, up to high-purity base metal after vacuum drying.

The rate of recovery of the metal niobium is not less than 92%.

It is an advantage of the invention that:By pre-processing ball milling slag, Control granularity removes base metal using mixing acidleach, then By the way of sodium carbonate roastings, fired slags are passed through into water logging and twice hydrochloric acid leaching process, further remove impurity metallic elements, Obtained niobium enrichment slag hydrofluoric acid, which leaches, obtains feed liquid containing niobium.Meanwhile electrolytic recovery is carried out to the filtrate containing base metal, pass through Control of Electric potentials recycles different base metal elements, to realize high efficiente callback valuable metal, avoids the wasting of resources, and the rate of recovery is high, Cost recovery is low, has significant economic benefit and social benefit.

Specific implementation mode

The present invention improves the acidleach rate of recovery and product quality, can obtain to improve acid leaching process in the prior art More efficiently slag open pit mining, it is suitable that experiment tests amount of slag, sour dosage, mixed acid ratio, multistep acidleach repeatedly The influence factors such as sequence, extraction time and temperature, and stirring.The factor for influencing niobium element recovery rate presses influence degree size, according to It is secondary to be arranged as amount of slag, extraction time, extraction temperature, sour dosage, mixed acid ratio, acid adding order and stirring number.Most In whole hydrofluoric acid leaching step, key reaction is:

NaNbO3 + 8HF = H2NbF7 + NaF + 3H2O

This patent is further described with reference to embodiment and comparative example.

Embodiment 1:

A kind of niobium element recycling process of enriching, the described method comprises the following steps:

1)Association niobium zirconium mine metallurgical slag acid adding is leached, the addition for controlling acid solution is according to liquid volume and slag mass ratio 30g/L, extraction temperature are 80 DEG C, and when Leach reaction is stirred with the rotating speed of 300r/min, and the acid solution is sulfuric acid and hydrochloric acid Mixed acid, sulfuric acid concentration 0.5mol/L, concentration of hydrochloric acid 1.5mol/L, the addition sequence of acid solution is that sulfuric acid reaction is first added 0.5h adds hydrochloric acid and continues to leach 2h.After the acid adding is first broken to association niobium zirconium mine metallurgical slag before leaching, ball is carried out Mill, it is levigate to account for 80% to granularity -0.074mm.Slag after the ball milling is sieved, Sieving and casing is controlled<0.048mm.

2)After Leach reaction, niobium concentration is down to 50mg/L hereinafter, filtrate Direct Electrolysis produces in filtered filtrate Base metal, filter residue are the thick niobium of mass percentage content >=85%.Positive and negative electrode and electrode plate spacing are inserted into the filtrate For 2cm, cell reaction temperature is 20 DEG C, and DC current flow density is 900A/m2, by different control of Electric potentials, on cathode It is sequentially depositing the base metal for obtaining different element species.Each base metal sedimentation time is 3h, the low-priced gold under a current potential After belonging to deposition completely, taking out deposition immediately has the cathode of the base metal, is reentered into new cathode and continues to deposit other low-priced gold Belong to element.Successively cleaning described deposit using tap water, absolute ethyl alcohol and deionized water has the cathode of base metal to cleaning solution pH It is in neutrality, up to high-purity base metal after vacuum drying.

3)After filter residue is dried, while adding Na2CO3It is roasted with solid state N aOH, Na2CO3Dosage is solid state N aOH 2.0wt%, solid state N aOH is 3 times of niobium mole in thick niobium, and calcination temperature is to react 1h at 380 DEG C;

4)Slag carries out water logging after roasting, twice using salt Ore Leaching by water logging slag, a concentration of 0.5mol/L of hydrochloric acid, two-stage leaching The hydrofluoric acid that filter residue afterwards reuses 12mol/L carries out plate compression, and extraction temperature is 90 DEG C, extraction time 2h, is leached Liquid is the feed liquid as niobium extraction and separation, is contained in the feed liquid:Nb 93wt%.The rate of recovery of the metal niobium is 92%.

Embodiment 2:

A kind of niobium element recycling process of enriching, the described method comprises the following steps:

1)Association niobium zirconium mine metallurgical slag acid adding is leached, the addition for controlling acid solution is according to liquid volume and slag mass ratio 25g/L, extraction temperature are 90 DEG C, and when Leach reaction is stirred with the rotating speed of 500r/min, and the acid solution is sulfuric acid and hydrochloric acid Mixed acid, sulfuric acid concentration 1mol/L, concentration of hydrochloric acid 2mol/L, the addition sequence of acid solution is that sulfuric acid reaction 1h is first added, Hydrochloric acid is added to continue to leach 3h.After the acid adding is first broken to association niobium zirconium mine metallurgical slag before leaching, ball milling is carried out, it is levigate 90% is accounted for granularity -0.074mm.Slag after the ball milling is sieved, Sieving and casing is controlled<0.048mm.

2)After Leach reaction, niobium concentration is down to 50mg/L hereinafter, filtrate Direct Electrolysis produces in filtered filtrate Base metal, filter residue are the thick niobium of mass percentage content >=85%.Positive and negative electrode and electrode plate spacing are inserted into the filtrate For 8cm, cell reaction temperature is 50 DEG C, and DC current flow density is 1200A/m2, by different control of Electric potentials, on cathode It is sequentially depositing the base metal for obtaining different element species.Each base metal sedimentation time is 3h, the low-priced gold under a current potential After belonging to deposition completely, taking out deposition immediately has the cathode of the base metal, is reentered into new cathode and continues to deposit other low-priced gold Belong to element.Successively cleaning described deposit using tap water, absolute ethyl alcohol and deionized water has the cathode of base metal to cleaning solution pH It is in neutrality, up to high-purity base metal after vacuum drying.

3)After filter residue is dried, while adding NaHCO3It is roasted with solid state N aOH, Na2CO3Dosage is solid state N aOH 1.0wt%, solid state N aOH is 2.5 times of niobium mole in thick niobium, and calcination temperature is to react 1h at 450 DEG C;

4)Slag carries out water logging after roasting, twice using salt Ore Leaching by water logging slag, a concentration of 1.5mol/L of hydrochloric acid, two-stage leaching The hydrofluoric acid that filter residue afterwards reuses 11mol/L is centrifuged, and extraction temperature is 80 DEG C, extraction time 2h, is leached Liquid is the feed liquid as niobium extraction and separation, is contained in the feed liquid:Nb 96wt%.The rate of recovery of the metal niobium is 95%.

Embodiment 3:

A kind of niobium element recycling process of enriching, the described method comprises the following steps:

1)Association niobium zirconium mine metallurgical slag acid adding is leached, the addition for controlling acid solution is according to liquid volume and slag mass ratio 35g/L, extraction temperature are 85 DEG C, and when Leach reaction is stirred with the rotating speed of 800r/min, and the acid solution is sulfuric acid and hydrochloric acid Mixed acid, sulfuric acid concentration 1mol/L, concentration of hydrochloric acid 3mol/L, the addition sequence of acid solution is that sulfuric acid reaction 1h is first added, Hydrochloric acid is added to continue to leach 2h.After the acid adding is first broken to association niobium zirconium mine metallurgical slag before leaching, ball milling is carried out, it is levigate 85% is accounted for granularity -0.074mm.Slag after the ball milling is sieved, Sieving and casing is controlled<0.048mm.

2)After Leach reaction, niobium concentration is down to 50mg/L hereinafter, filtrate Direct Electrolysis produces in filtered filtrate Base metal, filter residue are the thick niobium of mass percentage content >=85%.Positive and negative electrode and electrode plate spacing are inserted into the filtrate For 2~8cm, cell reaction temperature is 40 DEG C, and DC current flow density is 1000A/m2, by different control of Electric potentials, in the moon The base metal for obtaining different element species is sequentially depositing on extremely.Each base metal sedimentation time is 2h, under a current potential After base metal deposition is complete, taking out deposition immediately has the cathode of the base metal, is reentered into new cathode and continues to deposit other Base metal elements.Described deposit successively is cleaned using tap water, absolute ethyl alcohol and deionized water has the cathode of base metal extremely to clean Liquid pH is in neutrality, up to high-purity base metal after vacuum drying.

3)After filter residue is dried, while adding Na2CO3、NaHCO3It is roasted with solid state N aOH, Na2CO3And NaHCO3It throws Dosage summation is the 2.0wt% of solid state N aOH, and solid state N aOH is 3 times of niobium mole in thick niobium, and calcination temperature is anti-at 400 DEG C Answer 2h;

4)Slag carries out water logging after roasting, and water logging slag is used salt Ore Leaching twice, a concentration of 2mol/L of hydrochloric acid, after two-stage leaching Filter residue reuse the hydrofluoric acid of 10mol/L and carry out membrane filtration, extraction temperature is 100 DEG C, extraction time 1h, and leachate is As the feed liquid of niobium extraction and separation, contain in the feed liquid:Nb 95wt%.The rate of recovery of the metal niobium is 93%.

The additive added in the step 3 be or, or the two mixture.

Comparative example 1:

In the recovery method of the present invention, leached and when sodium carbonate roasting step when changing multistep, especially the acid concentration of multistep acidleach It is excessive or insufficient, and when the amount of alkali is added higher than 4 times of parts of tantalum mole or less than 1 times of part, will influence to mix in final feed liquid Miscellaneous other excessive base metal elements, or cause the rate of recovery of tantalum too low.

Comparative example 2:

When acid concentration, extraction time and the temperature parameter in hydrofluoric acid leaching step change, it will cause tantalum element cannot It fully leaches, and then reduces the tantalum rate of recovery in subsequent feed liquid.

The present invention is levigate by slag by that will pre-process it can be seen from embodiment 1-3 and comparative example 1 and 2, mixes acidleach Base metal is removed, is leached step by step twice by water logging and hydrochloric acid after sodium carbonate roasting and further removes impurity metallic elements, obtain tantalum It is enriched with slag, finally utilizes hydrofluoric acid to leach and obtains feed liquid containing tantalum, while electrolytic recovery is carried out to the filtrate containing base metal, pass through electricity Position control recycles different base metal elements and avoids rare precious metal from being lost in, the rate of recovery to realize high efficiente callback valuable metal Height, cost recovery is low, has significant economic benefit and social benefit.

While there has been shown and described that the embodiment of this patent, it will be understood by those skilled in the art that:Not In the case of being detached from the principle and objective of this patent a variety of change, modification, replacement and modification can be carried out to these embodiments, this The range of patent is limited by claim and its equivalent.

Claims (10)

1. a kind of niobium element recycles process of enriching, which is characterized in that the described method comprises the following steps:
1)Association niobium zirconium mine metallurgical slag acid adding is leached, the addition for controlling acid solution is according to liquid volume and slag mass ratio 25~35g/L, extraction temperature are 80~90 DEG C, and when Leach reaction is stirred with the rotating speed of 300~800r/min, the acid solution For the mixed acid of sulfuric acid and hydrochloric acid, sulfuric acid concentration is 0.5~1.0mol/L, and concentration of hydrochloric acid is 1.5~3.0mol/L, and acid solution adds Enter sequence for 0.5~1h of sulfuric acid reaction is first added, adds hydrochloric acid and continue 2~3h of leaching;
2)After Leach reaction, niobium concentration is down to 50mg/L hereinafter, filtrate Direct Electrolysis produces low-priced gold in filtered filtrate Belong to, filter residue is the thick niobium of mass percentage content >=85%;
3)It after filter residue is dried, while adding additive and being roasted with solid state N aOH, additive dosage is solid state N aOH's 0.5~2.0wt%, solid state N aOH are 2~3 times of niobium mole in thick niobium, and calcination temperature is that 1~2h is reacted at 380~450 DEG C;
4)Slag carries out water logging after roasting, twice using salt Ore Leaching by water logging slag, a concentration of 0.5~2mol/L of hydrochloric acid, and twice The hydrofluoric acid that filter residue after leaching reuses 10~12mol/L is separated by solid-liquid separation, and extraction temperature is 80~100 DEG C, is leached Time is 1~2h, and leachate is the feed liquid as niobium extraction and separation, is contained in the feed liquid:93~96wt% of Nb.
2. technique according to claim 1, characterized in that the acid adding first pre-processes slag before leaching.
3. technique according to claim 2, characterized in that the pretreatment is to be crushed association niobium zirconium mine metallurgical slag Afterwards, ball milling is carried out, it is levigate to account for 80~90% to granularity -0.074mm.
4. technique according to claim 3, characterized in that sieve the slag after the ball milling, control screening grain Diameter<0.048mm.
5. technique according to claim 1, characterized in that the additive added in the step 3 is Na2CO3Or NaHCO3Or the mixture of the two.
6. technique according to claim 1, characterized in that the solid-liquid separation method in the step 4 include plate compression, Centrifugation or membrane filtration.
7. according to the technique described in claim 1 to 6, characterized in that the step of electrolysis production base metal in the step 2 For:It is 2~8cm that positive and negative electrode and electrode plate spacing are inserted into the filtrate, and cell reaction temperature is 20~50 DEG C, direct current Electric current density is 900~1200A/m2, by different control of Electric potentials, it is sequentially depositing on cathode and obtains different element species Base metal.
8. technique according to claim 7, characterized in that each described base metal sedimentation time is 2~3h, at one After base metal under current potential deposits completely, taking out deposition immediately has the cathode of the base metal, is reentered into new cathode and continues Deposit other base metal elements.
9. technique according to claim 7 or 8, characterized in that successively clear using tap water, absolute ethyl alcohol and deionized water Washing described deposit has the cathode of base metal to be in neutrality to cleaning solution pH, up to high-purity base metal after vacuum drying.
10. according to the technique described in claim 1 to 9, characterized in that the rate of recovery of the metal niobium is not less than 92%.
CN201810732922.XA 2018-07-06 2018-07-06 A kind of niobium element recycling process of enriching CN108796228A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB960432A (en) * 1960-10-17 1964-06-10 Nat Res Dev Treatment of columbite and tantalite ores
CN103361495A (en) * 2013-07-17 2013-10-23 内蒙古科技大学 Method for extracting niobium from Bayan Obo mine tailing
CN105331811A (en) * 2014-08-06 2016-02-17 北京有色金属研究总院 Method for extracting tantalum, niobium and rare earth elements in multi-metal associated tantalum-niobium ores
CN105568003A (en) * 2015-12-31 2016-05-11 包头稀土研究院 Method for enriching niobium from Bayan obo tailings

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB960432A (en) * 1960-10-17 1964-06-10 Nat Res Dev Treatment of columbite and tantalite ores
CN103361495A (en) * 2013-07-17 2013-10-23 内蒙古科技大学 Method for extracting niobium from Bayan Obo mine tailing
CN105331811A (en) * 2014-08-06 2016-02-17 北京有色金属研究总院 Method for extracting tantalum, niobium and rare earth elements in multi-metal associated tantalum-niobium ores
CN105568003A (en) * 2015-12-31 2016-05-11 包头稀土研究院 Method for enriching niobium from Bayan obo tailings

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