CN109055984A - A method of using samarium trichloride as raw material room temperature electrolytic preparation rare earth metal samarium - Google Patents
A method of using samarium trichloride as raw material room temperature electrolytic preparation rare earth metal samarium Download PDFInfo
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- CN109055984A CN109055984A CN201811192283.9A CN201811192283A CN109055984A CN 109055984 A CN109055984 A CN 109055984A CN 201811192283 A CN201811192283 A CN 201811192283A CN 109055984 A CN109055984 A CN 109055984A
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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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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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Abstract
The present invention relates to a kind of using samarium trichloride as the method for raw material room temperature electrolytic preparation rare earth metal samarium, belongs to rare earth metal low temperature and extracts field.A method of using samarium trichloride as raw material room temperature electrolytic preparation rare earth metal samarium, including following processing steps: at room temperature, lithium nitrate being dissolved in the DMI electrolyte for obtaining lithium nitrate in DMI；The DMI electrolyte of lithium nitrate is placed in electrolytic cell, then anhydrous samarium trichloride is added into it, is stirred in electrolytic cell, is allowed to be formed transparent and homogeneous system, control whole system temperature is at 25 ± 5 DEG C, decomposition voltage range -1.8~-2.4V vs Ag；In electrolytic process, anhydrous samarium trichloride is added into electrolytic cell at regular intervals, control samarium trichloride molar concentration is initial concentration ± 3%.The method of the invention significantly reduces energy consumption and production cost while efficiently preparing rare earth metal samarium.
Description
Technical field
The present invention relates to a kind of using samarium trichloride as the method for raw material room temperature electrolytic preparation rare earth metal samarium, belongs to rare earth metal
Low temperature extracts field.
Background technique
Rare earth is valuable strategic resource, has the title of " industrial monosodium glutamate ", " mother of new material ", is widely used in hard-core technology
Field and military industry field.According to the Ministry of Industry and Information Technology's introduction, at present rare earth permanent magnet, shine, hydrogen storage, the functional materials such as catalysis have been
The indispensable raw material of the new high-tech industries such as advanced equipment manufacturing industry, new energy, new industry, are also widely used for electricity
Son, petrochemical industry control gold, machinery, new energy, light industry, environmental protection, agricultural etc..Particularly, rare earth metal samarium is to be used as SmCo
The raw material of based permanent magnet, samarium cobalt permanent magnet body is because its size advantage having is used in lightweight electronic equipment, and it is in height
Possessed function under temperature has received widespread attention.Furthermore samarium has nulcear properties, can be used as the structure of atomic reactor
Material shields worn-out material and control material, nuclear fission is enable to generate huge energy safe utilization.
From technical standpoint, currently, metal vacuum thermal reduction and high temperature fused salt electrolysis are traditional preparation sides of rare earth metal samarium
Method.But the disadvantages of 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.
With the energy growing tension and environmental issue it is increasingly prominent, how while obtaining high quality rare earth metal samarium maximum limit
Degree ground is reduced to the pollution of environment and energy saving, becomes focus concerned by people.If can be in room temperature or close under room temperature
Electro-deposition prepares rare earth metal samarium, not only easy to operate but also low in cost, reliable and secure.Due to abnormal active of rare earth samarium
Property, and its oxidation-reduction potential is very negative, rare earth samarium ion can not directly be reduced to rare earth on the electrode in water solution system
Samarium metal (liberation of hydrogen shielding action), therefore the system of electrodeposit metals samarium is generally nonaqueous solvents.Ionic liquid is as a kind of non-
Aqueous solvent, also referred to as low temperature molten salt, have low melting point, low saturated vapour pressure, and the properties such as electrochemical properties stabilization are used extensively
In the research of electrochemistry metallurgical process.But the synthesis technology of ionic liquid is complicated, and exchange reaction is not thorough, there are competitive reaction and
By-product, and products therefrom needs more purification and separation, this dramatically increases the production cost of ionic liquid and environmental pollutions
A possibility that, reduce the green characteristic of ionic liquid.And water content not can guarantee in last ionic liquid product obtained, sternly
Ionic liquid electrodeposition preparation active metal samarium process is affected again.In addition, conventional ionic liquid electrochemical window is relatively narrow and right
General chloride (such as magnesium chloride, calcium chloride, rare earth chloride etc.) solvability is limited, and some common ion liquid viscosities
Greatly, hygroscopic in air, therefore largely limit the practical application of ionic liquid.At present, ionic liquid development hundred
Year history, but it is limited only to scientific research in metal electrodeposition field, have 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%) room temperature electrolytic chlorine
Change the method that samarium prepares samarium metal.With samarium trichloride (purity be not less than 99.9%) for raw material, be dissolved in containing 0.02~
Electro-deposition prepares the Short flow method of High purity samarium metal in the DMI solvent of 0.6mol/L lithium nitrate, is efficiently preparing rare earth metal
Energy consumption and production cost are significantly reduced while samarium.
A method of using samarium trichloride as raw material room temperature electrolytic preparation rare earth metal samarium, the method is electrolysis method, including
Following processing steps:
Lithium nitrate is dissolved in DMI by S1 at room temperature, and molar concentration of the lithium nitrate in DMI is 0.02~0.6mol/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 samarium trichloride is added into it by S2, in electrolytic cell
It is stirred, is allowed to form transparent and homogeneous system, wherein samarium trichloride molar concentration is 0.01~0.3mol/L, controls whole system
Temperature is at 25 ± 5 DEG C, decomposition voltage range -1.8~-2.4V vs Ag；
S3 in electrolytic process, adds anhydrous samarium trichloride into electrolytic cell at regular intervals, controls samarium trichloride molar concentration
For initial concentration ± 3%.
In above-mentioned technical proposal, the lithium nitrate, samarium trichloride purity be not less than 99.9%；The DMI purity is not small
In 99.0%.
" control samarium trichloride molar concentration is initial concentration ± 3% " of the present invention refers to that control samarium trichloride molar concentration is
The 97%~103% of initial concentration.
" vs Ag " refers to using silver electrode as reference electricity in " decomposition voltage range -1.8~-2.4V vs Ag " of the present invention
Pole.
Preferably, in the step S1, molar concentration of the lithium nitrate in DMI is 0.05~0.5mol/L.
Preferably, in the step S2, samarium trichloride molar concentration is 0.02~0.2mol/L.
Preferably, the step S3 adds anhydrous samarium trichloride into electrolytic cell every 30min, and control samarium trichloride mole is dense
Degree is initial concentration ± 3%.
Preferably, the method includes the steps S4, every 60min that the samarium metal 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 20mm.
With it is existing prepare samarium metal 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 samarium trichloride 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
Samarium, 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 samarium trichloride 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 samarium 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.
Using samarium trichloride as the method for raw material room temperature electrolytic preparation rare earth metal samarium described in following embodiments, the method is
Electrolysis method, including following processing steps:
Lithium nitrate is dissolved in DMI by S1 at room temperature, and molar concentration 0.02~0.6mol/L of the lithium nitrate in DMI is obtained
The DMI electrolyte of lithium nitrate；
The DMI electrolyte of lithium nitrate is placed in electrolytic cell, then anhydrous samarium trichloride is added into it by S2, in electrolytic cell
It is stirred, is allowed to form transparent and homogeneous system, wherein samarium trichloride molar concentration is 0.01~0.3mol/L, controls whole system
Temperature is at 25 ± 5 DEG C, decomposition voltage range -1.8~-2.4V vs Ag；
S3 in electrolytic process, adds anhydrous samarium trichloride into electrolytic cell at regular intervals, controls samarium trichloride molar concentration
For initial concentration ± 3%.
Embodiment 1
Preparing electrolyte raw material is samarium trichloride and lithium nitrate, and solvent DMI is stirred to form electrolysis plastid in electrolytic cell
System, wherein samarium trichloride and lithium nitrate molar concentration are respectively 0.01mol/L and 0.03mol/L.Control electrolyte system constant temperature 25
± 5 DEG C, decomposition voltage is -1.8V (vs Ag), and anode material is graphite；It is carried out after electrolysis 30min once plus samarium trichloride operation makes
System samarium trichloride concentration is 0.01mol/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 samarium metal, which can be effectively deposited, to be come out, and ICP detects samarium member
Plain total content is 96.63%.
Embodiment 2
Preparing electrolyte raw material is samarium trichloride and lithium nitrate, and solvent DMI is stirred to form electrolysis plastid in electrolytic cell
System, wherein samarium trichloride and lithium nitrate molar concentration are respectively 0.05mol/L and 0.15mol/L.Control electrolyte system constant temperature 25
± 5 DEG C, decomposition voltage is -1.9V (vs Ag), and anode material is tungsten bar；It is carried out after electrolysis 30min once plus samarium trichloride operation makes
System samarium trichloride concentration is 0.05mol/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 samarium metal, which can be effectively deposited, to be come out, and ICP detects samarium member
Plain total content is 97.76%.
Embodiment 3
Preparing electrolyte raw material is samarium trichloride and lithium nitrate, and solvent DMI is stirred to form electrolysis plastid in electrolytic cell
System, wherein samarium trichloride and lithium nitrate molar concentration are respectively 0.1mol/L and 0.1mol/L.Control electrolyte system constant temperature 25 ± 5
DEG C, decomposition voltage is -2.0V (vs Ag), and anode material is molybdenum bar；It is carried out after electrolysis 30min once plus samarium trichloride operation makes body
Be samarium trichloride concentration be 0.1mol/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 samarium metal, which can be effectively deposited, to be come out, and ICP detects samarium element
Total content is 93.84%.
Embodiment 4
Preparing electrolyte raw material is samarium trichloride and lithium nitrate, and solvent DMI is stirred to form electrolysis plastid in electrolytic cell
System, wherein samarium trichloride and lithium nitrate molar concentration are respectively 0.15mol/L and 0.15mol/L.Control electrolyte system constant temperature 25
± 5 DEG C, decomposition voltage is -2.1V (vs Ag), and anode material is graphite rod；It carries out once adding samarium trichloride operation after being electrolysed 30min
Make system samarium trichloride concentration 0.15mol/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 samarium metal, which can be effectively deposited, to be come out, and ICP detects samarium
Element total content is 97.56%.
Embodiment 5
Preparing electrolyte raw material is samarium trichloride and lithium nitrate, and solvent DMI is stirred to form electrolysis plastid in electrolytic cell
System, wherein samarium trichloride and lithium nitrate molar concentration are respectively 0.20mol/L and 0.2mol/L.Control electrolyte system constant temperature 25 ±
5 DEG C, decomposition voltage is -2.2V (vs Ag), and anode material is tungsten bar；It is carried out after electrolysis 30min once plus samarium trichloride operation makes body
Be samarium trichloride concentration be 0.20mol/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 samarium metal, which can be effectively deposited, to be come out, and ICP detects samarium element
Total content is 98.82%.
Embodiment 6
Preparing electrolyte raw material is samarium trichloride and lithium nitrate, and solvent DMI is stirred to form electrolysis plastid in electrolytic cell
System, wherein samarium trichloride and lithium nitrate molar concentration are respectively 0.25mol/L and 0.3mol/L.Control electrolyte system constant temperature 25 ±
5 DEG C, decomposition voltage is -2.3V (vs Ag), and anode material is molybdenum bar；It is carried out after electrolysis 30min once plus samarium trichloride operation makes body
Be samarium trichloride concentration be 0.25mol/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 samarium metal, which can be effectively deposited, to be come out, and ICP detects samarium element
Total content is 98.51%.
Embodiment 7
Preparing electrolyte raw material is samarium trichloride and lithium nitrate, and solvent DMI is stirred to form electrolysis plastid in electrolytic cell
System, wherein samarium trichloride and lithium nitrate molar concentration are respectively 0.3mol/L and 0.6mol/L.Control electrolyte system constant temperature 25 ± 5
DEG C, decomposition voltage is -2.4V (vs Ag), and anode material is graphite rod；It is carried out after electrolysis 30min once plus samarium trichloride operation makes
System samarium trichloride concentration is 0.3mol/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 samarium metal, which can be effectively deposited, to be come out, and ICP detects samarium member
Plain total content is 99.86%.
Embodiment 8
Preparing electrolyte raw material is samarium trichloride and lithium nitrate, and solvent DMI is stirred to form electrolysis plastid in electrolytic cell
System, wherein samarium trichloride and lithium nitrate molar concentration are respectively 0.05mol/L and 0.15mol/L.Control electrolyte system constant temperature 25
± 5 DEG C, decomposition voltage is -2.4V (vs Ag), and anode material is tungsten bar；It is carried out after electrolysis 30min once plus samarium trichloride operation makes
System samarium trichloride concentration is 0.05mol/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 samarium metal, which can be effectively deposited, to be come out, and ICP detects samarium member
Plain total content is 99.97%.
Claims (7)
1. a kind of using samarium trichloride as the method for raw material room temperature electrolytic preparation rare earth metal samarium, it is characterised in that: the method is electricity
Solution, including following processing steps:
Lithium nitrate is dissolved in DMI by S1 at room temperature, and molar concentration of the lithium nitrate in DMI is 0.02~0.6mol/L, obtains nitre
The DMI electrolyte of sour lithium, the DMI are that structural formula is as follows:
The DMI electrolyte of lithium nitrate is placed in electrolytic cell, then anhydrous samarium trichloride is added thereto by S2, stirs in electrolytic cell
Mixing, is allowed to form transparent and homogeneous system, and wherein samarium trichloride molar concentration is 0.01~0.3mol/L, controls whole system temperature
At 25 ± 5 DEG C, decomposition voltage range -1.8~-2.4V vs Ag；
S3 in electrolytic process, adds anhydrous samarium trichloride into electrolytic cell at regular intervals, and control samarium trichloride molar concentration is
Beginning concentration ± 3%.
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 0.05~0.5mol/L.
3. according to the method described in claim 1, it is characterized by: in the step S2, samarium trichloride molar concentration is 0.02~
0.2mol/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 samarium trichloride, control samarium trichloride molar concentration are initial concentration ± 3%.
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 samarium metal 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 20mm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111826691A (en) * | 2020-08-21 | 2020-10-27 | 东北大学 | Method for preparing zinc-tantalum alloy by using solvated ionic liquid |
| CN115449874A (en) * | 2022-09-23 | 2022-12-09 | 广州超邦化工有限公司 | Plating rare earth electrolytic protection liquid and electrolytic protection process |
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| CN103205787A (en) * | 2013-04-22 | 2013-07-17 | 南通万宝实业有限公司 | Preparation method of metal permanent magnet thin film with multi-layer thin film structure |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111826691A (en) * | 2020-08-21 | 2020-10-27 | 东北大学 | Method for preparing zinc-tantalum alloy by using solvated ionic liquid |
| CN111826691B (en) * | 2020-08-21 | 2021-09-21 | 东北大学 | Method for preparing zinc-tantalum alloy by using solvated ionic liquid |
| CN115449874A (en) * | 2022-09-23 | 2022-12-09 | 广州超邦化工有限公司 | Plating rare earth electrolytic protection liquid and electrolytic protection process |
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