CN108298564A - A method of it is crystallized using electrodeposition lean solution production vulcanized sodium - Google Patents
A method of it is crystallized using electrodeposition lean solution production vulcanized sodium Download PDFInfo
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- CN108298564A CN108298564A CN201711389052.2A CN201711389052A CN108298564A CN 108298564 A CN108298564 A CN 108298564A CN 201711389052 A CN201711389052 A CN 201711389052A CN 108298564 A CN108298564 A CN 108298564A
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- crystallization
- vulcanized sodium
- lean solution
- solution
- electrodeposition
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- 238000004070 electrodeposition Methods 0.000 title claims abstract description 63
- 239000011734 sodium Substances 0.000 title claims abstract description 53
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 title claims abstract description 48
- 229910052708 sodium Inorganic materials 0.000 title claims abstract description 48
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000002425 crystallisation Methods 0.000 claims abstract description 50
- 230000008025 crystallization Effects 0.000 claims abstract description 48
- 238000002386 leaching Methods 0.000 claims abstract description 20
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 18
- 229910052787 antimony Inorganic materials 0.000 claims abstract description 17
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims abstract description 17
- WBZKQQHYRPRKNJ-UHFFFAOYSA-L disulfite Chemical compound [O-]S(=O)S([O-])(=O)=O WBZKQQHYRPRKNJ-UHFFFAOYSA-L 0.000 claims abstract description 10
- 239000006166 lysate Substances 0.000 claims abstract description 9
- 239000011780 sodium chloride Substances 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 239000003814 drug Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 5
- 230000009467 reduction Effects 0.000 claims abstract description 5
- 238000004073 vulcanization Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 89
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 41
- 238000000605 extraction Methods 0.000 claims description 8
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 8
- 229910052737 gold Inorganic materials 0.000 claims description 8
- 239000010931 gold Substances 0.000 claims description 8
- 238000006386 neutralization reaction Methods 0.000 claims description 8
- 238000000746 purification Methods 0.000 claims description 8
- 238000006722 reduction reaction Methods 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- 238000004458 analytical method Methods 0.000 claims description 4
- 239000003518 caustics Substances 0.000 claims description 4
- 239000003153 chemical reaction reagent Substances 0.000 claims description 4
- 239000012141 concentrate Substances 0.000 claims description 4
- 238000011084 recovery Methods 0.000 claims description 4
- PANBYUAFMMOFOV-UHFFFAOYSA-N sodium;sulfuric acid Chemical compound [Na].OS(O)(=O)=O PANBYUAFMMOFOV-UHFFFAOYSA-N 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 235000010265 sodium sulphite Nutrition 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 2
- 238000005137 deposition process Methods 0.000 abstract description 9
- 239000012535 impurity Substances 0.000 abstract description 5
- 238000005868 electrolysis reaction Methods 0.000 abstract description 4
- 238000002474 experimental method Methods 0.000 description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 7
- 238000002156 mixing Methods 0.000 description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000009835 boiling Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000009854 hydrometallurgy Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000003595 mist Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 229910052979 sodium sulfide Inorganic materials 0.000 description 2
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- UDKNNAHBOVNOOP-UHFFFAOYSA-N [As].[Au].[Sb] Chemical compound [As].[Au].[Sb] UDKNNAHBOVNOOP-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000010425 asbestos Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000010413 mother solution Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 229920001021 polysulfide Polymers 0.000 description 1
- 239000005077 polysulfide Substances 0.000 description 1
- 150000008117 polysulfides Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 229910052895 riebeckite Inorganic materials 0.000 description 1
- 238000010583 slow cooling Methods 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000004457 water analysis Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/22—Alkali metal sulfides or polysulfides
-
- 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
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/12—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic alkaline solutions
-
- 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
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/02—Obtaining antimony
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Geology (AREA)
- Electrolytic Production Of Metals (AREA)
- Electroplating And Plating Baths Therefor (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a kind of methods using the production vulcanized sodium crystallization of electrodeposition lean solution comprising following steps：The first step, electrodeposition lean solution evaporative crystallization：Electrodeposition lean solution is placed in 100 DEG C of hot water and is evaporated, then crystallisation by cooling filters, spontaneously dries and weigh at room temperature；Product after crystallization is vulcanized sodium, and the medicament that system Leaching of Antimony when adds is that the vulcanized sodium that system is self-produced after vulcanization, crystallization is applied and makees leaching agent with leaching system；Vulcanized sodium after being crystallized in the first step is put into lysate and dissolves, forms metabisulfite solution by second step；Third walks, and in metabisulfite solution and purifies；4th step：Reduction prepares sodium chloride product.Method of the present invention using the production vulcanized sodium crystallization of electrodeposition lean solution is evaporated crystallization to electrodeposition lean solution, and the crystallization of output vulcanized sodium returns to leaching section and is reused for producing, and reduces vulcanized sodium dosing, and purifying electrolysis liquid impurity optimizes electrolytic deposition process.
Description
Technical field
The present invention relates to a kind of methods producing vulcanized sodium crystallization more particularly to a kind of utilization electrodeposition lean solution to produce vulcanized sodium
The method of crystallization, belongs to metallurgical technology field.
Background technology
Electrodeposition is hydrometallurgy noun, is exactly by the solution electrolytic deposition output cathode of the metal ion after extracting and enriching
Metal.In hydrometallurgy, electrodeposition is exactly by the antimony solution electrolytic deposition output cathode antimony after extracting and enriching.It is electrolysed the antimony of feed liquor
Concentration is generally 45~50g/L, a concentration of 20~30g/L of antimony of electrolytic liquid.Lean electrolyte is back to extraction as back extraction
Agent uses, and according to the accumulation situation of wherein iron, extracts a small amount of lean solution out and returns to leaching, to maintain the balance electrodeposition lean solutions of iron to contain
A large amount of impurity such as vulcanized sodium medicament and sulfate, sulphite, foreign ion influence electrodeposition very big, deterioration electrolytic deposition process, drop
Low electric effect, causes medicament to waste, and increases production cost.
Invention content
It is an object of the invention to：In view of the above problems, a kind of utilization electrodeposition lean solution production vulcanized sodium knot is provided
Brilliant method is evaporated crystallization to electrodeposition lean solution, and the crystallization of output vulcanized sodium returns to leaching section and is reused for producing, reduces
Vulcanized sodium dosing, purifying electrolysis liquid impurity optimize electrolytic deposition process.
The technical proposal of the invention is realized in this way：A method of it is crystallized using electrodeposition lean solution production vulcanized sodium,
Include the following steps：
The first step, electrodeposition lean solution evaporative crystallization：Electrodeposition lean solution is placed in 100 DEG C of hot water and is evaporated, it is then cold at room temperature
But crystallization filters, spontaneously dries and weigh；Product after crystallization is vulcanized sodium, and the medicament that system Leaching of Antimony when adds is sulphur
Change, the self-produced vulcanized sodium of system is applied and makees leaching agent with leaching system after crystallization；
Vulcanized sodium after being crystallized in the first step is put into lysate and dissolves by second step, Cu/Fe=in lysate
30：1, PH=0.5~1, form metabisulfite solution；
Third walks, and in metabisulfite solution and purifies；Use caustic lye of soda as neutralization reagent neutralisation of sulphuric acid sodium solution to pH
=1~2, then filtration, purification, is purified rear liquid；
4th step：According to 15:1 ratio is equipped with liquid and reducing solution after purification, carries out reduction reaction, and reduction prepares sodium chloride
Product.
Method of the present invention using the production vulcanized sodium crystallization of electrodeposition lean solution, in the 4th step, reducing solution is pressed
According to concentration be respectively 200g/L sodium sulfite and sodium hydroxide according to volume ratio be 2:1 volume mixture restores pH=2.0,
Then it is filtered, is dried in vacuo sodium chloride product.
Method of the present invention using the production vulcanized sodium crystallization of electrodeposition lean solution, in the 4th step, the recovery time
For 250min.
Method of the present invention using the production vulcanized sodium crystallization of electrodeposition lean solution, the preparation of the electrodeposition lean solution：It will
Gold Concentrate under Normal Pressure is in liquid-solid ratio 1:1, it is leached under conditions of sodium hydroxide 20g/L, vulcanized sodium 40g/L, extraction time 1h, leaches temperature
40 DEG C of degree；Chemical analysis is carried out to typical leachate, selects main component (g/L):Sb53.2、As0.25、Au1.25、
NaOH15.6、Na2S5.2、SX2-1.5 electrodeposition lean solution.
Method of the present invention using the production vulcanized sodium crystallization of electrodeposition lean solution, the electrodeposition experiment is in diaphragm electrodeposition
It is carried out in slot, Winning cell is double anode area, cathodic region size 22cmX14cmX5cm, anode region size 10cmX15cmX24cm；Together
Pole span 12cm；Cathode-current density 250A/m2, anodic current density 1200A/m2；Catholyte contain Sb53.2, Au1.25,
Na2S5.2, anolyte are the NaOH aqueous solutions of 120g/L.
Beneficial effects of the present invention：Method of the present invention using the production vulcanized sodium crystallization of electrodeposition lean solution, to electrodeposition
Lean solution is evaporated crystallization, and the crystallization of output vulcanized sodium returns to leaching section and is reused for producing, reduces vulcanized sodium dosing,
Purifying electrolysis liquid impurity optimizes electrolytic deposition process.
Figure of description
Attached drawing 1 is that tank voltage varies with temperature curve.
Specific implementation mode
With reference to embodiment, the present invention is described in detail.
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
Technology is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, not
For limiting the present invention.
A method of it is crystallized using electrodeposition lean solution production vulcanized sodium comprising following steps：
The first step, electrodeposition lean solution evaporative crystallization：Electrodeposition lean solution is placed in 100 DEG C of hot water and is evaporated, it is then cold at room temperature
But crystallization filters, spontaneously dries and weigh；Product after crystallization is vulcanized sodium, and the medicament that system Leaching of Antimony when adds is sulphur
Change, the self-produced vulcanized sodium of system is applied and makees leaching agent with leaching system after crystallization；
Vulcanized sodium after being crystallized in the first step is put into lysate and dissolves by second step, Cu/Fe=in lysate
30：1, PH=0.5~1, form metabisulfite solution；
Third walks, and in metabisulfite solution and purifies；Use caustic lye of soda as neutralization reagent neutralisation of sulphuric acid sodium solution to pH
=1~2, then filtration, purification, is purified rear liquid；
4th step：According to 15:1 ratio is equipped with liquid and reducing solution after purification, carries out reduction reaction, and reduction prepares sodium chloride
Product.
Embodiment 1：
Alkaline sulphide solution easily has certain leaching gold in the system of opening wide due to the multiple factors such as aoxidizing, hydrolyzing and being formed
The polysulfide of effect, vulcanization sulfate, sulphite.Using alkaline sodium sulfide solution preimpregnation antimony is carried out to containing arsenic antimony gold concentrate
During, the gold in mineral can be leached along with antimony, constitute a kind of solution system containing gold, antimony, polymorphic sulfur-bearing object.
Test raw material：From certain antimony hydrometallurgy electrodeposition open circuit lean solution, analysis of components is shown in Table 1：
Table 1：Certain electrodeposition lean solution water analysis/mg.L-1；
The method crystallized using electrodeposition lean solution production vulcanized sodium comprising following steps：
First, electrodeposition lean solution is prepared：Since the initial concentration of antimony in electrodeposition solution is much larger than gold, ignore flash-over characteristic polarization
Current potential, it is assumed that solution is perfect solution, using Raoult's law to solution activity carry out simplify processing, in electrolytic deposition process gold and
The deposition potential of antimony is estimated.
AuS+e→Au+S2-
E0=-0.490V, E=-0.790V
SbS3 3-+3c→Sb+3S2-
E0=-0.900V, E=-0.9007V
Estimate that body structure surface, the golden current potential that returns the benefit are higher than antimony, will be preferentially precipitated in cathode electrolytic deposition process.When testing electrodeposition
Between 5h, electric current 6.58A, cathode liquid accumulates 1026mL before electrodeposition, catholyte 976ml, anolyte volume 2984mL after electrodeposition.
Electrodeposition humid test：In electrolytic deposition process, increasing the temperature of electric effusion can be such that the resistance of electric effusion reduces, and be conducive to reduce
Tank voltage, temperature is excessively high to lead to the evaporation capacity that electric effusion evaporates, during diaphragm electrodeposition, due to the concentration of NaOH in anolyte
Up to 120g/L, the alkali mist that electric effusion largely evaporates will obviously deteriorate.Temperature is increased to 50 DEG C of processes such as 1 institute of attached drawing by 20 DEG C
Show：
Tank voltage varies with temperature curve and sees attached drawing 1.
As shown in Fig. 1, as temperature increases, electrolytic deposition process tank voltage constantly reduces.When temperature increases, the precipitation electricity of antimony
Position influence is little, but as the raising of temperature, the ultra-voltage of hydrogen reduce, causes it to be precipitated in cathode so that current efficiency reduces.
When temperature rise is to 50 DEG C, alkali mist volatile quantity obviously increases, and operating environment is more severe.Continuing raising temperature will be difficult to continue
Operation, so, temperature is controlled at 50 DEG C or so.
The production capacity and labor productivity of electrolytic cell can be improved in actual production using high cathode-current density, but
Increase tank voltage and power consumption simultaneously, cathode potential should be controlled in -1.10V hereinafter, being higher than this current potential, and hydrogen can be precipitated.
By Gold Concentrate under Normal Pressure in liquid-solid ratio 1:1, it is leached under conditions of sodium hydroxide 20g/L, vulcanized sodium 40g/L, when leaching
Between 1h, 40 DEG C of extraction temperature；Chemical analysis is carried out to typical leachate, selects main component (g/L):Sb53.2、As0.25、
Au1.25、NaOH15.6、Na2S5.2、SX2- 1.5 electrodeposition lean solution.Electrodeposition experiment carries out in diaphragm electrodeposition slot, and Winning cell is
Double anode area, cathodic region size 22cmX14cmX5cm, anode region size 10cmX15cmX24cm；With pole span 12cm；Cathode current
Density 250A/m2, anodic current density 1200A/m2；Catholyte contains Sb53.2, Au1.25, Na2S5.2, anolyte 120g/
The NaOH aqueous solutions of L.
Then vulcanized sodium crystallization is produced as follows：The first step, electrodeposition lean solution evaporative crystallization：Electrodeposition lean solution is set
It is evaporated in 100 DEG C of hot water, then crystallisation by cooling filters, spontaneously dries and weigh at room temperature；
Crystalline mother solution after being crystallized in the first step is returned to stockyard by second step, and the sodium sulphate after crystallization is put into lysate
It is dissolved, Cu/Fe=30 in lysate：1, PH=0.5~1, form metabisulfite solution；
Third walks, and in metabisulfite solution and purifies；Use caustic lye of soda as neutralization reagent neutralisation of sulphuric acid sodium solution to pH
=1~2, then filtration, purification, is purified rear liquid；
4th step：According to 15:1 ratio is equipped with liquid and reducing solution after purification, carries out reduction reaction, reducing solution is according to concentration
Respectively the sodium sulfite of 200g/L and sodium hydroxide are 2 according to volume ratio:1 volume mixture restores pH=2.0, when reduction
Between be 250min.Then it is filtered, is dried in vacuo sodium chloride product.As the recovery time extends, sodium chloride recycling takes the lead in increasing
It is reduced after adding, reductase 12 50min sodium chloride rate of recovery highests can reach 93.55%.
Electrodeposition lean solution crystallization experiment purpose：
1, it determines and the water that crystallization need to steam is precipitated；
2, crystallization temperature is determined；
3, general cooling rate is obtained；
4, the boiling point of solution is obtained.
Laboratory apparatus：One, 500mL beakers, one, 1000mL graduated cylinders.Blender and one, holder, electric jacket or Electric stove
One, glass stirring rod one, 200 DEG C of one, thermometers, 0.01 precision balance one.One box of filter paper, bottle,suction, Bu Shi leakages
Bucket, experiment vacuum pump.
Experimentation：
By clean 1000mL graduated cylinder weighings, 1000mL liquid is then taken, outer wall, weighing are dried.Obtain the proportion of solution.
It takes 500mL solution to be put into beaker, is placed on electric furnace and heats, to put asbestos board on electric furnace in advance.Record starts to add
The time of heat and solution state.
When solution boils, liquidus temperature is recorded.
When solution inspissation is to remaining about 350mL, phenomenon in solution is examined, has seen whether that crystallization generates.And record knot
Amount of solution and temperature when crystalline substance generates.In spite of there is crystallization to generate, stops heating, record temperature and time.
Beaker with extraction raffinate is statically placed in air, slow cooling, with glass bar agitated liquid.The time is recorded simultaneously, and
About mixing speed.
When solution temperature is down to about 60 DEG C, it is replaced by cold bath cooling, continues to stir, and record experimental phenomena, time
And about mixing speed.
When solution temperature is down to about 25 DEG C, it is depending on circumstances changed to more ice block cooling, or be put into refrigerator, makes solution temperature
It is down to 10 DEG C.Record mixing speed, time and experimental phenomena.
Brilliant liquid is filtered with bottle,suction, weighing after filtering, observes crystalline form size and the rate of filtration, experiment terminate.
If the amount of solid of 30~40g is not achieved after experiment, evaporation time and extraction raffinate amount need to be changed, until reaching knot
Crystalline substance amount requires.If granularity requirements are not achieved in crystalline product, cooling velocity and mixing speed are changed.It may need many experiments that can obtain
Complete requirement of experiment.
Experiment conclusion：According to experimentation and record, the data needed for experiment purpose are obtained, experimentation are carried out total
Knot, general scheme is provided to the processing mode of solution.
It is 1188.6g/L to take electrodeposition lean solution 5L on the 6.2nd or so, measurement lean solution proportion.Na2S a concentration of 58.55g/L, NaOH
A concentration of 34.4g/L.
Lean solution is initially brown liquid, and 500ml lean solutions are heated to boiling, and it is 102 DEG C to need 12min, boiling point.
When solution inspissation is to 350ml, nodeless mesh generates in solution.Glass bar stirs, and is cooled to 60 DEG C in air, does not have yet
Crystallization occurs.Cold bath is cooled to 25 DEG C, does not have crystallization to occur.
When from coming to life to solution inspissation to 250ml, 35min is taken, temperature is 104 DEG C at this time, has crystallization to occur.Glass
Glass stick stirs, and about 60 revs/min of speed is cooled to 60 DEG C in air by 104 DEG C, takes 13min.Continue cold bath drop by 60 DEG C
When temperature is to 25 DEG C, 15min is taken, ice water is continuing with and is cooled to 10 DEG C, taken 25min, there is mass crystallization generation at this time.Glass
Stick mixing speed whole process is 60 revs/min.Bottle,suction filters 10min, obtains shallow green powder shape crystal.It dries, claims in air
It is 29.4g to obtain crystal weight.
When vulcanization na concn is higher (such as higher than 150g/L), degree of oxidation increases electrodeposition lean solution, needs to carry out vacuum
It is concentrated by evaporation to reduce vulcanization na concn, Containing Sulfur na concn is not high in electrodeposition lean solution at present, can directly return to leaching.
Method of the present invention using the production vulcanized sodium crystallization of electrodeposition lean solution is evaporated crystallization to electrodeposition lean solution,
Output vulcanized sodium crystallizes, and returns to leaching section and is reused for producing, reduce vulcanized sodium dosing, purifying electrolysis liquid impurity is excellent
Change electrolytic deposition process.Vulcanized sodium dosing 10% is reduced, antimony direct current unit consumption reduces by 10%.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement etc., should all be included in the protection scope of the present invention made by within refreshing and principle.
Claims (6)
1. a kind of method using the production vulcanized sodium crystallization of electrodeposition lean solution, it is characterised in that：It includes the following steps：
The first step, electrodeposition lean solution evaporative crystallization：Electrodeposition lean solution is placed in 100 DEG C of hot water and is evaporated, it is then cooling at room temperature to tie
Crystalline substance filtering is spontaneously dried and is weighed；Product after crystallization is vulcanized sodium, and the medicament that system Leaching of Antimony when adds is vulcanization, knot
The self-produced vulcanized sodium of system is applied after crystalline substance makees leaching agent with leaching system；
Vulcanized sodium after being crystallized in the first step is put into lysate and dissolves by second step, Cu/Fe=30 in lysate：1,
PH=0.5~1 forms metabisulfite solution；
Third walks, and in metabisulfite solution and purifies；Use caustic lye of soda as neutralization reagent neutralisation of sulphuric acid sodium solution to pH=1~
2, then filtration, purification, is purified rear liquid；
4th step：According to 15:1 ratio is equipped with liquid and reducing solution after purification, carries out reduction reaction, and reduction prepares sodium chloride production
Product.
2. the method according to claim 1 using the production vulcanized sodium crystallization of electrodeposition lean solution, it is characterised in that：4th step
In, reducing solution according to concentration be respectively 200g/L sodium sulfite and sodium hydroxide according to volume ratio be 2:1 volume mixture, also
Former pH=2.0, is then filtered, and is dried in vacuo sodium chloride product.
3. the method according to claim 2 using the production vulcanized sodium crystallization of electrodeposition lean solution, it is characterised in that：4th step
In, recovery time 250min.
4. the method according to claim 1 using the production vulcanized sodium crystallization of electrodeposition lean solution, it is characterised in that：Electrodeposition lean solution
Preparation：By Gold Concentrate under Normal Pressure in liquid-solid ratio 1:1, it is leached under conditions of sodium hydroxide 20g/L, vulcanized sodium 40g/L, extraction time
1h, 40 DEG C of extraction temperature；Chemical analysis is carried out to typical leachate, selects main component (g/L):Sb53.2、As0.25、
Au1.25、NaOH15.6、Na2S5.2、SX2-1.5 electrodeposition lean solution.
5. the method according to claim 1 using the production vulcanized sodium crystallization of electrodeposition lean solution, it is characterised in that：Electrodeposition is tested
It is carried out in diaphragm electrodeposition slot, Winning cell is double anode area, cathodic region size 22cmX14cmX5cm, anode region size
10cmX15cmX24cm；With pole span 12cm；Cathode-current density 250A/m2, anodic current density 1200A/m2。
6. the method according to claim 5 using the production vulcanized sodium crystallization of electrodeposition lean solution, it is characterised in that：Catholyte contains
There are Sb53.2, Au1.25, Na2S5.2, anolyte are the NaOH aqueous solutions of 120g/L.
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|---|---|---|---|---|
| CN110565120A (en) * | 2019-10-18 | 2019-12-13 | 东北大学 | A method for removing and recovering copper in copper-containing molten iron |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102502531A (en) * | 2011-11-03 | 2012-06-20 | 云南铜业股份有限公司 | Novel and environment-friendly method for extracting tellurium from tellurium slag |
| CN102534238A (en) * | 2012-03-07 | 2012-07-04 | 怀化市洪发资源综合利用科技有限公司 | Harmless and comprehensive utilization method for vanadium-extraction liquid leached residue |
| CN104862484A (en) * | 2015-05-15 | 2015-08-26 | 西北矿冶研究院 | Method for extracting antimony from lead anode slime |
| CN205500875U (en) * | 2016-01-15 | 2016-08-24 | 中国瑞林工程技术有限公司 | Waste water treatment system |
| CN106367780A (en) * | 2016-08-31 | 2017-02-01 | 北京矿冶研究总院 | Method for producing antimony by rotational flow electrodeposition of antimony-containing solution |
-
2017
- 2017-12-20 CN CN201711389052.2A patent/CN108298564A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102502531A (en) * | 2011-11-03 | 2012-06-20 | 云南铜业股份有限公司 | Novel and environment-friendly method for extracting tellurium from tellurium slag |
| CN102534238A (en) * | 2012-03-07 | 2012-07-04 | 怀化市洪发资源综合利用科技有限公司 | Harmless and comprehensive utilization method for vanadium-extraction liquid leached residue |
| CN104862484A (en) * | 2015-05-15 | 2015-08-26 | 西北矿冶研究院 | Method for extracting antimony from lead anode slime |
| CN205500875U (en) * | 2016-01-15 | 2016-08-24 | 中国瑞林工程技术有限公司 | Waste water treatment system |
| CN106367780A (en) * | 2016-08-31 | 2017-02-01 | 北京矿冶研究总院 | Method for producing antimony by rotational flow electrodeposition of antimony-containing solution |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110565120A (en) * | 2019-10-18 | 2019-12-13 | 东北大学 | A method for removing and recovering copper in copper-containing molten iron |
| CN110565120B (en) * | 2019-10-18 | 2021-09-07 | 东北大学 | A kind of method for removing and recovering copper in copper-containing molten iron |
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