CN109208033A - A kind of method of low cost electrolysis praseodymium chloride production metal praseodymium - Google Patents
A kind of method of low cost electrolysis praseodymium chloride production metal praseodymium Download PDFInfo
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- CN109208033A CN109208033A CN201811192280.5A CN201811192280A CN109208033A CN 109208033 A CN109208033 A CN 109208033A CN 201811192280 A CN201811192280 A CN 201811192280A CN 109208033 A CN109208033 A CN 109208033A
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- praseodymium
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/22—Electrolytic production, recovery or refining of metals by electrolysis of solutions of metals not provided for in groups C25C1/02 - C25C1/20
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Abstract
The present invention relates to a kind of methods of low cost electrolysis praseodymium chloride production metal praseodymium, belong to rare earth metal low temperature and extract field.A kind of method of low cost electrolysis praseodymium chloride production metal praseodymium, including following processing steps: at room temperature, lithium nitrate is dissolved in the DMI electrolyte that lithium nitrate is obtained in DMI；The DMI electrolyte of lithium nitrate is placed in electrolytic cell, then anhydrous praseodymium chloride is added into it, is stirred in electrolytic cell, is allowed to be formed uniform system, control whole system temperature is at 30~80 DEG C, decomposition voltage range -2.0~-2.4V vs Ag；In electrolytic process, anhydrous praseodymium chloride is added into electrolytic cell at regular intervals, control praseodymium chloride molar concentration is initial concentration ± 2%.The method of the invention significantly reduces energy consumption and production cost while efficiently preparing rare earth metal praseodymium.
Description
Technical field
The present invention relates to a kind of methods of low cost electrolysis praseodymium chloride production metal praseodymium, belong to rare earth metal low temperature and extract neck
Domain.
Background technique
Rare earth element is known as " industrial vitamin ", has excellent magnetic, light, the electrical property that can not replace, and produces to improving
Moral character energy, increases product variety, and raising production efficiency plays the role of huge.Since rare-earth action is big, dosage is few, it has also become
Improve product structure, technical progress of industry of increasing technology content, promotes important element, be widely applied to metallurgy, military affairs,
The fields such as petrochemical industry, glass ceramics, agricultural and new material.Particularly, praseodymium is widely used in architectural pottery and domestic ceramics
In, it is mixed and made into color glaze with ceramic glaze, can also individually make under-glaze pigment, manufactured pigment is pure color, light in faint yellow
It is refined.Praseodymium can also be used for manufacture permanent magnet, select cheap praseodymium neodymium metal that pure neodymium metal is replaced to manufacture permanent-magnet material, antioxygen property
It is significantly improved with mechanical performance, can be processed into magnet of various shapes, be widely used on all kinds of electronic devices and motor.This
Outside, praseodymium is also applied to petroleum catalytic cracking, prepares cracking of oil in addition Y-type zeolite molecular sieve in the form of pr-nd enriched product and urges
The activity, selectivity and stability of catalyst can be improved in agent.
From technology, currently, metal vacuum thermal reduction and high temperature fused salt electrolysis are the tradition systems of rare earth metal praseodymium
Preparation Method.But all there is energy consumption height in the two, seriously polluted, long flow path, corrosivity is strong, complicated for operation, the high requirements on the equipment etc.
Disadvantage.With the energy growing tension and environmental issue it is increasingly prominent, how while obtaining high quality rare earth metal praseodymium
The pollution to environment and energy saving is reduced to the maximum extent, becomes focus concerned by people.If can be in room temperature or close to room temperature
Under the conditions of electro-deposition prepare rare earth metal praseodymium, it is not only easy to operate but also low in cost, it is reliable and secure.Due to praseodymium exception
Activity, and its oxidation-reduction potential is very negative, and rare earth praseodymium ion is made since liberation of hydrogen shields on the electrode in water solution system
With can not directly be reduced to rare earth metal praseodymium, therefore the system of electrodeposit metals praseodymium is generally nonaqueous solvents.Ionic liquid is made
For a kind of nonaqueous solvents, also referred to as low temperature molten salt, there is low melting point, low saturated vapour pressure, the properties such as electrochemical properties are stablized,
It is widely used in the research of electrochemistry metallurgical process.But the synthesis technology of ionic liquid is complicated, and exchange reaction is not thorough, and there are competing
Reaction and by-product are striven, and products therefrom needs more purification and separation, this dramatically increases the production costs of ionic liquid and right
A possibility that environmental pollution, reduces the green characteristic of ionic liquid.And in last obtained ionic liquid product water content without
Method guarantees, has seriously affected ionic liquid electrodeposition preparation active metal praseodymium process.In addition, conventional ionic liquid electrochemical window
It is relatively narrow and limited to general chloride (such as magnesium chloride, calcium chloride, rare earth chloride etc.) solvability, and some common ion liquid
Body viscosity is big, hygroscopic in air, therefore largely limits the practical application of ionic liquid.At present, ionic liquid
Develop one-hundred-year history, but be limited only to scientific research in metal electrodeposition field, has no large-scale practical application background.
Summary of the invention
For above-mentioned existing problem, the present invention provides one kind with lithium nitrate (purity is greater than 99.9%) as supporting electrolyte
Utilize novel non-proton intensive polar solvent 1,3- dimethyl-2-imidazolinone (DMI) (purity is greater than 99.0%) low-temperature electrolytic chlorine
Change the method that praseodymium prepares metal praseodymium.With praseodymium chloride (purity be not less than 99.9%) for raw material, be dissolved in containing 0.01~
Electro-deposition prepares the Short flow method of high pure metal praseodymium in the DMI solvent of 0.1mol/L lithium nitrate, is efficiently preparing rare earth metal
Energy consumption and production cost are significantly reduced while praseodymium.
A kind of method of low cost electrolysis praseodymium chloride production metal praseodymium, the method are electrolysis method, including following techniques step
It is rapid:
Lithium nitrate is dissolved in DMI by S1 at room temperature, and molar concentration of the lithium nitrate in DMI is 0.01~0.1mol/L,
The DMI electrolyte of lithium nitrate is obtained, the DMI is that structural formula is as follows:
The DMI electrolyte of lithium nitrate is placed in electrolytic cell, then anhydrous praseodymium chloride is added into it by S2, in electrolytic cell
It is stirred, is allowed to form uniform system, wherein praseodymium chloride molar concentration is 0.001~0.05mol/L, controls whole system temperature
Degree is at 30~80 DEG C, decomposition voltage range -2.0~-2.4V vs Ag；
S3 in electrolytic process, adds anhydrous praseodymium chloride into electrolytic cell at regular intervals, controls praseodymium chloride molar concentration
For initial concentration ± 2%.
In above-mentioned technical proposal, the lithium nitrate, praseodymium chloride purity be not less than 99.9%；The DMI purity is not small
In 99.0%.
" control praseodymium chloride molar concentration is initial concentration ± 2% " of the present invention refers to that control praseodymium chloride molar concentration is
The 98%~102% of initial concentration.
" vs Ag " refers to using silver electrode as reference electricity in " decomposition voltage range -2.0~-2.4V vs Ag " of the present invention
Pole.
Preferably, in the step S1, molar concentration of the lithium nitrate in DMI is 0.02~0.1mol/L.
Preferably, in the step S2, praseodymium chloride molar concentration is 0.002~0.05mol/L.
Preferably, the step S3 adds anhydrous praseodymium chloride into electrolytic cell every 30min, and control praseodymium chloride mole is dense
Degree is initial concentration ± 2%.
Preferably, the method includes the steps S4, every 60min that the metal praseodymium formed on cathode plate sliding is rodlike
Scraper scraped in the closing vessel equipped with dimethyl carbonate or kerosene along cathode plate face；To collection gained rare earth metal
Reprocessing is handled as desired.
Preferably, the electrolytic process with high purity graphite rod or tungsten bar or molybdenum bar material (purity >=99.9%) for anode, with
Fine copper plate (purity >=99.9%) is cathode.
Preferably, the interpolar between the anode and cathode is away from for 15mm.
With it is existing prepare metal praseodymium method compared with, the method for the invention has the advantage that
(1) process flow is shortened, and significantly reduces production energy consumption, reduces production cost, improves operating environment；
(2) the novel non-proton intensive polar solvent electro-deposition of low temperature is used, can reduce and eliminate using high temperature fused salt electrolysis matter
When the shortcomings that energy consumption is high, temperature is high, equipment seriously corroded, easy to operate, furthermore DMI solvent not only possesses praseodymium chloride excellent molten
Solution property and high dielectric constant also have nontoxic, good chemical and thermal stability, do not corrode to copper and iron, higher boiling, high-flash,
Low melting point easily recycles, the characteristics of having a safety feature.Importantly, DMI solvent possesses extensive chemical industry production background, cost compared with
Molten salt system and ionic liquid are greatly reduced, and in addition DMI can be synthesized with waste plastics and GHG carbon dioxide, green speciality
Obviously, there is large-scale application ability and prospect.Method and process of the invention electro-deposition can prepare rare earth metal at low temperature
Praseodymium, obtained product purity is high, lower to equipment requirement, is produced on a large scale to improve efficiency and yield, for the dilute of low cost
The preparation of earth metal green provides technological reserve and theories integration.
Detailed description of the invention
Fig. 1 is to scheme in embodiment 8 in copper cathode sheets products therefrom SEM.
Specific embodiment
Following non-limiting embodiments can with a person of ordinary skill in the art will more fully understand the present invention, but not with
Any mode limits the present invention.
Test method described in following embodiments is unless otherwise specified conventional method；The reagent and material, such as
Without specified otherwise, commercially obtain.
The anhydrous praseodymium chloride purity 99.9% used in the embodiment of the present invention, lithium nitrate purity 99.9%, DMI purity
99.0%.
Using Shanghai Chen Hua electrochemical workstation as electrolysis power in the embodiment of the present invention.
Anode of the embodiment of the present invention is high purity graphite rod or tungsten bar or molybdenum bar material (purity >=99.9%), and diameter 0.5cm is inserted
Enter level 1cm, cathode is high-purity copper plates (purity >=99.9%), cathode area 1cm2, reference electrode is filamentary silver (purity
>=99.99%, diameter 0.05cm).
The content of praseodymium element is examined using ICP (inductively coupled plasma atomic emission spectrum) in the embodiment of the present invention
It surveys；Characterization method has SEM (scanning electron microscope) and EDS energy spectrum analysis.
The method that low cost described in following embodiments is electrolysed praseodymium chloride production metal praseodymium, the method is electrolysis method, packet
Include following processing steps:
Lithium nitrate is dissolved in DMI by S1 at room temperature, and molar concentration of the lithium nitrate in DMI is 0.01~0.1mol/L,
Obtain the DMI electrolyte of lithium nitrate；
The DMI electrolyte of lithium nitrate is placed in electrolytic cell, then anhydrous praseodymium chloride is added into it by S2, in electrolytic cell
It is stirred, is allowed to form transparent and homogeneous system, wherein praseodymium chloride molar concentration is 0.001~0.05mol/L, controls entire body
It is temperature at 30~80 DEG C, decomposition voltage range -2.0~-2.4V vs Ag；
S3 in electrolytic process, adds anhydrous praseodymium chloride into electrolytic cell at regular intervals, controls praseodymium chloride molar concentration
For initial concentration ± 2%.
Embodiment 1
Preparing electrolyte raw material is praseodymium chloride and lithium nitrate, and solvent DMI is stirred to form electrolysis plastid in electrolytic cell
System, wherein praseodymium chloride and lithium nitrate molar concentration are respectively 0.001mol/L and 0.01mol/L.Control electrolyte system constant temperature 30
DEG C, decomposition voltage is -2.0V (vs Ag), and anode material is graphite；It is carried out after electrolysis 30min once plus praseodymium chloride operation makes body
Be praseodymium chloride concentration be 0.001mol/L；The deposit collection on substrate is saved after being electrolysed 60min and is deposited to gained is collected
Reprocessing is handled object as desired.It is detected through characterization, the results showed that metal praseodymium, which can be effectively deposited, to be come out, and ICP detects praseodymium member
Plain total content is 72.32%.
Embodiment 2
Preparing electrolyte raw material is praseodymium chloride and lithium nitrate, and solvent DMI is stirred to form electrolysis plastid in electrolytic cell
System, wherein praseodymium chloride and lithium nitrate molar concentration are respectively 0.002mol/L and 0.02mol/L.Control electrolyte system constant temperature 45
DEG C, decomposition voltage is -2.1V (vs Ag), and anode material is tungsten bar；It is carried out after electrolysis 30min once plus praseodymium chloride operation makes body
Be praseodymium chloride concentration be 0.002mol/L；The deposit collection on substrate is saved after being electrolysed 60min and is deposited to gained is collected
Reprocessing is handled object as desired.It is detected through characterization, the results showed that metal praseodymium, which can be effectively deposited, to be come out, and ICP detects praseodymium member
Plain total content is 96.57%.
Embodiment 3
Preparing electrolyte raw material is praseodymium chloride and lithium nitrate, and solvent DMI is stirred to form electrolysis plastid in electrolytic cell
System, wherein praseodymium chloride and lithium nitrate molar concentration are respectively 0.01mol/L and 0.03mol/L.Control electrolyte system constant temperature 55
DEG C, decomposition voltage is -2.2V (vs Ag), and anode material is molybdenum bar；It is carried out after electrolysis 30min once plus praseodymium chloride operation makes body
Be praseodymium chloride concentration be 0.01mol/L；The deposit collection on substrate is saved after being electrolysed 60min and to collection gained deposit
Reprocessing is handled as desired.It is detected through characterization, the results showed that metal praseodymium, which can be effectively deposited, to be come out, and ICP detects praseodymium element
Total content is 97.94%.
Embodiment 4
Preparing electrolyte raw material is praseodymium chloride and lithium nitrate, and solvent DMI is stirred to form electrolysis plastid in electrolytic cell
System, wherein praseodymium chloride and lithium nitrate molar concentration are respectively 0.015mol/L and 0.04mol/L.Control electrolyte system constant temperature 65
DEG C, decomposition voltage is -2.3V (vs Ag), and anode material is graphite rod；It is carried out after electrolysis 30min once plus praseodymium chloride operation makes
System praseodymium chloride concentration is 0.015mol/L；The deposit collection on substrate is saved after being electrolysed 60min and heavy to gained is collected
Reprocessing is handled product object as desired.It is detected through characterization, the results showed that metal praseodymium, which can be effectively deposited, to be come out, and ICP detects praseodymium
Element total content is 99.75%.
Embodiment 5
Preparing electrolyte raw material is praseodymium chloride and lithium nitrate, and solvent DMI is stirred to form electrolysis plastid in electrolytic cell
System, wherein praseodymium chloride and lithium nitrate molar concentration are respectively 0.02mol/L and 0.06mol/L.Control electrolyte system constant temperature 75
DEG C, decomposition voltage is -2.4V (vs Ag), and anode material is tungsten bar；It is carried out after electrolysis 30min once plus praseodymium chloride operation makes body
Be praseodymium chloride concentration be 0.02mol/L；The deposit collection on substrate is saved after being electrolysed 60min and to collection gained deposit
Reprocessing is handled as desired.It is detected through characterization, the results showed that metal praseodymium, which can be effectively deposited, to be come out, and ICP detects praseodymium element
Total content is 99.62%.
Embodiment 6
Preparing electrolyte raw material is praseodymium chloride and lithium nitrate, and solvent DMI is stirred to form electrolysis plastid in electrolytic cell
System, wherein praseodymium chloride and lithium nitrate molar concentration are respectively 0.025mol/L and 0.08mol/L.Control electrolyte system constant temperature 75
DEG C, decomposition voltage is -2.4V (vs Ag), and anode material is molybdenum bar；It is carried out after electrolysis 30min once plus praseodymium chloride operation makes body
Be praseodymium chloride concentration be 0.025mol/L；The deposit collection on substrate is saved after being electrolysed 60min and is deposited to gained is collected
Reprocessing is handled object as desired.It is detected through characterization, the results showed that metal praseodymium, which can be effectively deposited, to be come out, and ICP detects praseodymium member
Plain total content is 99.71%.
Embodiment 7
Preparing electrolyte raw material is praseodymium chloride and lithium nitrate, and solvent DMI is stirred to form electrolysis plastid in electrolytic cell
System, wherein praseodymium chloride and lithium nitrate molar concentration are respectively 0.03mol/L and 0.1mol/L.Control electrolyte system constant temperature 80
DEG C, decomposition voltage is -2.3V (vs Ag), and anode material is graphite rod；It is carried out after electrolysis 30min once plus praseodymium chloride operation makes
System praseodymium chloride concentration is 0.03mol/L；The deposit collection on substrate is saved after being electrolysed 60min and is deposited to gained is collected
Reprocessing is handled object as desired.It is detected through characterization, the results showed that metal praseodymium, which can be effectively deposited, to be come out, and ICP detects praseodymium member
Plain total content is 99.84%.
Embodiment 8
Preparing electrolyte raw material is praseodymium chloride and lithium nitrate, and solvent DMI is stirred to form electrolysis plastid in electrolytic cell
System, wherein praseodymium chloride and lithium nitrate molar concentration are respectively 0.05mol/L and 0.1mol/L.Control electrolyte system constant temperature 55
DEG C, decomposition voltage is -2.3V (vs Ag), and anode material is tungsten bar；It is carried out after electrolysis 30min once plus praseodymium chloride operation makes body
Be praseodymium chloride concentration be 0.05mol/L；The deposit collection on substrate is saved after being electrolysed 60min and to collection gained deposit
Reprocessing is handled as desired.It is detected through characterization, the results showed that metal praseodymium, which can be effectively deposited, to be come out, and ICP detects praseodymium element
Total content is 99.98%.
Claims (7)
1. a kind of method of low cost electrolysis praseodymium chloride production metal praseodymium, it is characterised in that: the method is electrolysis method, including under
State processing step:
Lithium nitrate is dissolved in DMI by S1 at room temperature, and molar concentration of the lithium nitrate in DMI is 0.01~0.1mol/L, is obtained
The DMI electrolyte of lithium nitrate, the DMI are that structural formula is as follows:
The DMI electrolyte of lithium nitrate is placed in electrolytic cell, then anhydrous praseodymium chloride is added thereto by S2, stirs in electrolytic cell
Mixing, is allowed to form uniform system, and wherein praseodymium chloride molar concentration is 0.001~0.05mol/L, and control whole system temperature exists
30~80 DEG C, decomposition voltage range -2.0~-2.4V vs Ag；
S3 in electrolytic process, adds anhydrous praseodymium chloride into electrolytic cell at regular intervals, and control praseodymium chloride molar concentration is
Beginning concentration ± 2%.
2. according to the method described in claim 1, it is characterized by: in the step S1, molar concentration of the lithium nitrate in DMI
For 0.02~0.1mol/L.
3. according to the method described in claim 1, it is characterized by: in the step S2, praseodymium chloride molar concentration is 0.002~
0.05mol/L。
4. according to the method described in claim 1, it is characterized by: the step S3, adds nothing into electrolytic cell every 30min
Water praseodymium chloride, control praseodymium chloride molar concentration are initial concentration ± 2%.
5. according to the method described in claim 1, it is characterized by: the method includes the steps S4, every 60min by cathode pole
The metal praseodymium formed on plate slides rodlike scraper along cathode plate face scraping in the envelope equipped with dimethyl carbonate or kerosene
It closes in vessel；To gained rare earth metal is collected, reprocessing is handled as desired.
6. according to the method described in claim 1, it is characterized by: the electrolytic process is with high purity graphite rod or tungsten bar or molybdenum bar
Material is anode, using fine copper plate as cathode.
7. according to the method described in claim 6, it is characterized by: interpolar between the anode and cathode is away from for 15mm.
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