CN108117105A - A kind of process for purification of Copper making by-product crude nickle sulphate - Google Patents
A kind of process for purification of Copper making by-product crude nickle sulphate Download PDFInfo
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- CN108117105A CN108117105A CN201711468426.XA CN201711468426A CN108117105A CN 108117105 A CN108117105 A CN 108117105A CN 201711468426 A CN201711468426 A CN 201711468426A CN 108117105 A CN108117105 A CN 108117105A
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/10—Sulfates
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The present invention dissolves crude nickle sulphate to obtain nickel sulfate solution, using Na2S2O3Make precipitating reagent recycling valuable metal copper;Liquid adds in oxidant and fluorization agent one-step removal iron therein, arsenic, calcium, magnesium after copper removal;Except liquid uses 2 ethylhexyl phosphoric acid list, 2 ethylhexyl after iron, arsenic, calcium, magnesium(P507)And tributyl phosphate(TBP)Saponified Extractants synergic solvent extraction deep impurity-removing obtains pure nickel sulfate solution;Pure nickel sulfate solution obtains refined sulfuric acid nickel product through evaporative crystallization.Present invention process flow is short, of low cost, easy to operate, environmental-friendly, and nickel recovery is high, extractant reusable edible, and products obtained therefrom quality reaches plating 2009 Grade A requirement of grade and LITHIUM BATTERY high-purity sulphuric acid nickel professional standard HG/T2824.
Description
Technical field
The present invention relates to a kind of process for purification of Copper making by-product crude nickle sulphate, particularly belong to nonferrous metallurgy Chemical Engineering Technology
Field.
Background technology
Nickel sulfate is a kind of important nonferrous heavy metal chemical products of nickel, is widely used in chemical industry, light industry, machinery, stone
In the industrial circles such as oil, electronics.A certain amount of nickel is usually contained during Copper making, in copper electrolyte, and with electrolyte
Continuous cycle and raise, when the content of nickel reaches a certain concentration, it will usually at the method progress nickel removal of freezing and crystallizing
Reason, product is crude nickle sulphate, wherein also containing a certain amount of valuable metal copper, while also containing the miscellaneous of other different contents
Matter, such as cobalt, iron, zinc, calcium, magnesium, arsenic.In order to meet the needs of nickel sulfate is growing and resource reclaim be recycled, urgently
Deep purifying, and its valuable metal of synthetical recovery simultaneously need to be carried out to the crude nickle sulphate generated during Copper making.
Usual crude nickle sulphate method for refining and reclaiming includes:Chemical precipitation method, solvent extraction, ion-exchange, chemistry are heavy
It forms sediment and solvent extraction combination method.Chemical precipitation method is obtained by condensing crystallizing after sulfide precipitation, oxydrolysis precipitation, fluorination precipitation
To product, removal of impurity is not high, and can cause a large amount of losses of nickel, is also easy to produce toxic gas, and reagent consumption amount is big, and
Sodium content is excessively high in product.Solvent extraction is with the extractants imurity-removal such as LIX984, P204, P507, Cyanex-272, most
Condensing crystallizing obtains product afterwards, and this method equipment investment is big, and production cost is high, and calcium and magnesium removal rate is low.Ion-exchange is using sun
Ion or anion exchange resin adsorbing and removing impurity, last condensing crystallizing obtain product, and this method requires material composition severe
It carves, accommodation is small, and resin easily blocks.Chemical precipitation and solvent extraction combined purifying method be to crude nickle sulphate simultaneously into
Row chemical precipitation method and solvent extraction purification removal of impurities, final condensing crystallizing obtain product, although product quality that this method obtains
Height, purification are thorough, but technological process is complicated, the production cycle is long, refine cost recovery height.
The content of the invention
The present invention is for a kind of insufficient existing for existing crude nickle sulphate impurity removal process technology, of low cost, operation letter of proposition
Just process for purification, environmental-friendly, technological process is short, the high crude nickle sulphate of product quality refine and recycle the side of valuable metal
Method.
A kind of purification process steps of Copper making by-product crude nickle sulphate of the present invention are as follows:
Step 1:Na2S2O3Selective precipitation copper
In mass ratio 3:1 meter, with crude nickle sulphate of the water dissolution containing As, Ca, Co, Cu, Fe, Mg, Zn impurity, obtains thick sulfuric acid
Nickel solution;
By Na2S2O3The molar ratio computing of nickel sulfate is three times in, using excessive Na2S2O3Crude nickel sulfate solution is made choice
Property cement copper, the initial pH of solution precipitation reaction is 0.5, controls and reacts 2h under the conditions of 85 DEG C of temperature;After reaction to product
It is filtered, obtains copper removal nickel sulfate solution;Wherein the removal rate of Cu is 99.94%~100%, and the loss late of nickel is 0.75%
~0.80%.
Step 2:One step precipitated iron, arsenic, calcium, magnesium
Under the conditions of 85 DEG C, hydrogen peroxide is added in the nickel sulfate solution of step 1 copper removal, oxidation reaction 20min;Oxidation
After, add in excessive sodium fluoride, adjust the pH value of solution as 4.5, react 2h, followed by filter, obtain except iron, arsenic,
The nickel sulfate solution of calcium and magnesium, wherein iron, arsenic, the removal rate of calcium and magnesium be respectively 99.38%~99.97%, 97.83%~
99.85%th, 97.64%~100%, 99.24%~100%.
Step 3:Synergic solvent extraction deep impurity-removing
By 1:The mixed organic solvents that soda soap rate is 65% are added to except iron, arsenic, calcium and magnesium by 1 volume percentage
Nickel sulfate solution in, be stirred 5min, balance pH is 4 or so, clarifies 5min, and three-level counter-current extraction under room temperature, separation has
Machine phase and water phase obtain extracting the nickel sulfate solution of miscellaneous organic phase and deep impurity-removing;Wherein zinc, cobalt, the extraction yield of nickel are respectively
100%th, 98.18%~99.00%, 6.37%~7.82%;Three-level counter-current extraction condition is:The time is stirred as 5min,
It is 4 or so to balance pH, settling time 5min.
By 1:1 compare, first washs the miscellaneous organic phase of extraction, liquid returns to thick sulphur after washing with the acid deionized water of pH=3-4
In sour nickel solution;It is stripped again with 1mol/L sulfuric acid solutions to extracting miscellaneous organic phase, is stirred 5min, clarify 5min;Room temperature
Lower progress two-stage back extraction, separates organic phase and water phase, organic phase is through regeneration.
The mixed organic solvents press volume percentage, and P507 25%, TBP 5%, sulfonated kerosene are
70%.
Step 4:Condensing crystallizing
The nickel sulfate solution of deep impurity-removing is subjected to concentration postcooling to room temperature, then crystallized, separation and drying, obtains essence
Sulphuric acid nickel.
The definition of removal rate, loss late, extraction yield of the present invention:
Removal rate:When the aqueous solution of the A containing solute is removed with chemical precipitation method, it is total in slag phase that removal rate is equal to A
Content and the percentage of total contents of the A in slag liquid two-phase.
Loss late:When the aqueous solution of solute A and B need to separate removal A with chemical precipitation method, loss late is equal to B and exists
The percentage of total content and total contents of the B in slag liquid two-phase in slag phase.
Extraction yield:When the aqueous solution of solute A is extracted with organic solvent, extraction yield is equal to A always containing in organic phase
Amount and the percentage of total contents of the A in two-phase.
Beneficial effects of the present invention:The present invention passes through Na2S2O3Selective precipitation copper, a step precipitated iron, arsenic, calcium and magnesium,
P507 (2- ethylhexyl phosphoric acid single 2-ethyls hexyl ester), TBP (tributyl phosphate) and the collaboration of sulfonated kerosene mixed organic solvents
The technical measures such as deep impurity-removing are extracted, refine purification Copper making by-product crude nickle sulphate.Use Na2S2O3Copper is sunk as precipitating reagent, environment
Close friend, heavy copper effect is good, and the loss amount of nickel is few;One step precipitation is short except iron, arsenic, calcium, the flow of magnesium, easy to operate;Synergic solvent extraction
Deep impurity-removing three-level counter-current extraction at normal temperatures, nickel and other impurities separating effect are notable, and split-phase speed is fast, is not likely to produce the 3rd
Mutually and emulsify.The method of the present invention refines of low cost, and easy to operate, the heavy copper stage does not generate the gases such as hydrogen sulfide, to environment friend
Good, technological process is short, and product purity is high.
Description of the drawings
Fig. 1:The process flow chart that crude nickle sulphate of the present invention refines.
Specific embodiment
Embodiment 1
By crude nickle sulphate plus water in mass ratio 3:1 dissolving, solid crude nickle sulphate main component is as shown in table 1, obtained thick
Nickel sulfate solution main component is as shown in table 2.
1 crude nickle sulphate main component (wt%) of table
2 crude nickel sulfate solution essential element mass concentration (unit of table:g/L)
(1)Na2S2O3Selective precipitation copper
Take crude nickel sulfate solution 300mL, Na2S2O3Molar ratio is 3, and the initial pH of solution is 0.5, controlling reaction temperature 85
DEG C, the reaction time is for 2h or so.It is filtered after heavy copper, the rate of deposition of Cu is 99.97%, and the loss late of nickel is only 0.78%.
Filtrate main component:As0.454g/L, Ca1.482g/L, Co0.108g/L, Cu0.0017g/L, Fe2.614g/L,
Mg2.597g/L, Ni44.252g/L, Zn1.296g/L.
(2) one steps precipitation is except iron, arsenic, calcium, magnesium
Liquid 300mL is added in reaction vessel after taking heavy copper, and it is 85 DEG C to adjust reaction temperature, is slowly added to 10mL dioxygens
Water, oxidization time control in 20min or so, after add in the sodium fluoride that molar ratio is 4, it is 4.5 to adjust pH value, control reaction
Time, filtering, the removal rate of As, Ca, Fe and Mg were respectively 97.83%, 99.76%, 99.77%, 99.92% in 2h or so,
Ni hardly loses.
Filtrate main component:As0.0099g/L, Ca0.0035g/L, Co0.100g/L, Cu0.0012g/L,
Fe0.0061g/L, Mg0.002g/L, Ni44.181g/L, Zn1.289g/L.Filtrate carries out solvent extraction processing.
(3) extract
Mixed organic solvents are added in liquid after removal of impurities, mix organic phase volume percentage as 25%P507,5%TBP,
70% sulfonated kerosene, soda soap rate are 65%, three-level counter-current extraction under room temperature.
Extraction conditions is:It is 1/1 compared to O/A, is stirred the time as 5min, balance pH is 4 or so, and settling time is
5min, separation organic phase mutually obtain extracting the nickel sulfate solution of miscellaneous organic phase and deep impurity-removing, the extraction yield point of Zn, Co, Ni with water
It Wei 100%, 99%, 7.82%;
Main component in liquid after purification:As0.0093g/L, Ca0.0007g/L, Co0.001g/L, Cu0.0001g/L,
Fe0.001g/L, Mg0.0018g/L, Ni40.724g/L, Zn0.0001g/L.Extract miscellaneous organic phase first with acid deionized water (pH
=3-4) it presses compared to 1:1 is washed, and only containing nickel, cobalt, iron in liquid after washing, content is respectively 3.28g/L, 0.0013g/
L, 0.0008g/L, liquid returns to crude nickle sulphate dissolving after washing.
It is stripped again to extracting miscellaneous organic phase afterwards, back extraction condition is:O/A is 1/1, sulfuric acid concentration 1mol/L, stirring
Incorporation time is 5min, settling time 5min, and two-stage back extraction is carried out under room temperature.Last organic phase after regeneration, returns again sharp
With.
(4) condensing crystallizing
Liquid carries out condensing crystallizing after purifying, and after testing, liquid-tight degree 1.23g/mL before concentration, heating evaporation is concentrated into density
For 1.65g/mL postcoolings to room temperature, emerald refined sulfuric acid nickel is obtained after crystallization, drying.
Its product quality and the comparison of national sector standard HG/T2824-2009 industrial sulphuric acid nickel are as shown in table 3.
The nickel sulfate product quality that 3 embodiment 1 of table is refining to obtain and the comparison of national sector standard HG/T2824-2009
As can be seen from Table 3, the nickel sulfate product quality that embodiment 1 obtains is higher than national standard《HG/T2824-2009》
Technology requirement, can be widely applied to plating and battery industry.
Embodiment 2
By crude nickle sulphate plus water in mass ratio 3:1 dissolving, solid crude nickle sulphate main component is as shown in table 4, obtained thick
Nickel sulfate solution main component is as shown in table 5.
4 crude nickle sulphate main component (wt%) of table
5 crude nickel sulfate solution essential element mass concentration (unit of table:g/L)
(1)Na2S2O3Selective precipitation copper
Take crude nickel sulfate solution 300mL, Na2S2O3Molar ratio is 3, and the initial pH of solution is 0.5, controlling reaction temperature 85
DEG C, the reaction time is for 2h or so.After heavy copper, filtering, the rate of deposition of Cu is 100%, and the loss late of nickel is only 0.80%.
Filtrate main component:As0.100g/L, Ca1.679g/L, Co0.058g/L, Cu0.0001g/L, Fe1.030g/L,
Mg1.69g/L, Ni65.47g/L, Zn0.758g/L.
(2) one steps precipitation is except iron, arsenic, calcium, magnesium
Liquid 300mL is added in reaction vessel after taking heavy copper, and it is 85 DEG C to adjust reaction temperature, is slowly added to 10mL dioxygens
Water, oxidization time control in 20min or so, after add in the sodium fluoride that molar ratio is 5 or so, it is 4.5 or so to adjust pH value,
The reaction time is controlled in 2h or so, filtering, the removal rate of As, Ca, Fe and Mg is respectively 98.96%, 99.85%, 99.85%,
100%, Ni hardly lose.
Filtrate main component:As0.001g/L, Ca0.0024g/L, Co0.055g/L, Cu0.0001g/L, Fe0.0015g/
L, Mg0.0001g/L, Ni65.339g/L, Zn0.733g/L.Filtrate carries out solvent extraction processing.
(3) extract
Mixed organic solvents are added in liquid after removal of impurities, mix organic phase volume percentage as 25%P507,5%TBP,
70% sulfonated kerosene, soda soap rate are 65%, three-level counter-current extraction under room temperature.
Extraction conditions is:It is 1/1 compared to O/A, is stirred the time as 5min, balance pH is 4 or so, and settling time is
5min, separation organic phase mutually obtain extracting the nickel sulfate solution of miscellaneous organic phase and deep impurity-removing, the extraction yield point of Zn, Co, Ni with water
It Wei 100%, 98.18%, 6.76%.
Main component in liquid after purification:As0.001g/L, Ca0.0004g/L, Co0.001g/L, Cu0.0001g/L,
Fe0.0003g/L, Mg0.0001g/L, Ni60.924g/L, Zn0.0001g/L.Extract miscellaneous organic phase first with acid deionized water (pH
=3-4) it presses compared to 1:1 is washed, and only containing nickel, cobalt in liquid after washing, content is respectively 4.19g/L, 0.001g/L, is washed
It washs rear liquid and returns to crude nickle sulphate dissolving.
It is stripped again to extracting miscellaneous organic phase afterwards, back extraction condition is:O/A is 1/1, sulfuric acid concentration 1mol/L, stirring
Incorporation time is 5min, settling time 5min, and two-stage back extraction is carried out under room temperature.Last organic phase after regeneration, returns again sharp
With.
(4) condensing crystallizing
Liquid carries out condensing crystallizing after purifying, and after testing, liquid-tight degree 1.24g/mL before concentration, heating evaporation is concentrated into density
For 1.65g/mL postcoolings to room temperature, emerald refined sulfuric acid nickel is obtained after crystallization, drying.
Its product quality and the comparison of national sector standard HG/T2824-2009 industrial sulphuric acid nickel are as shown in table 6.
The nickel sulfate product quality that 6 embodiment 2 of table is refining to obtain and the comparison of national sector standard HG/T2824-2009
As can be seen from Table 6, the nickel sulfate product quality that embodiment 2 obtains is higher than national standard《HG/T2824-2009》
Technology requirement, can be widely applied to plating and battery industry.
Embodiment 3
By crude nickle sulphate plus water in mass ratio 3:1 dissolving, solid crude nickle sulphate main component is as shown in table 7, obtained thick
Nickel sulfate solution main component is as shown in table 8.
7 crude nickle sulphate main component (wt%) of table
8 crude nickel sulfate solution essential element mass concentration (unit of table:g/L)
(1)Na2S2O3Selective precipitation copper
Take crude nickel sulfate solution 300mL, Na2S2O3Molar ratio is 3, and the initial pH of solution is 0.5, controlling reaction temperature 85
DEG C, the reaction time is for 2h or so.After heavy copper, filtering, the rate of deposition of Cu is 99.94%, and the loss late of nickel is only 0.75%.
Filtrate main component:As0.743g/L, Ca0.981g/L, Co0.070g/L, Cu0.0007g/L, Fe3.602g/L,
Mg1.307g/L, Ni58.172g/L, Zn0.837g/L.
(2) one steps precipitation is except iron, arsenic, calcium, magnesium
Liquid 300mL is added in reaction vessel after taking heavy copper, and it is 85 DEG C to adjust reaction temperature, is slowly added to 10mL dioxygens
Water, oxidization time control in 20min or so, after add in the sodium fluoride that molar ratio is 6 or so, it is 4.5 or so to adjust pH value,
The reaction time is controlled in 2h or so, filtering, the removal rate of As, Ca, Fe and Mg is respectively 99.85%, 100%, 99.97%,
100%, Ni hardly lose.
Filtrate main component:As0.001g/L, Ca0.0001g/L, Co0.065g/L, Cu0.0006g/L, Fe0.001g/
L, Mg0.0001g/L, Ni58.012g/L, Zn0.833g/L.Filtrate carries out solvent extraction processing.
(3) extract
Mixed organic solvents are added in liquid after removal of impurities, mix organic phase volume percentage as 25%P507,5%TBP,
70% sulfonated kerosene, soda soap rate are 65%, three-level counter-current extraction under room temperature.
Extraction conditions is:It is 1/1 compared to O/A, is stirred the time as 5min, balance pH is 4 or so, and settling time is
5min, separation organic phase mutually obtain extracting the nickel sulfate solution of miscellaneous organic phase and deep impurity-removing, the extraction yield point of Zn, Co, Ni with water
It Wei 100%, 98.46%, 6.37%.
Main component in liquid after purification:As0.001g/L, Ca0.0001g/L, Co0.001g/L, Cu0.0001g/L,
Fe0.0001g/L, Mg0.0001g/L, Ni54.317g/L, Zn0.0001g/L.Extract miscellaneous organic phase first with acid deionized water (pH
=3-4) it presses compared to 1:1 is washed, and only containing nickel, cobalt in liquid after washing, content is respectively 3.51g/L, 0.0021g/L,
Liquid returns to crude nickle sulphate dissolving after washing.
It is stripped again to extracting miscellaneous organic phase afterwards, back extraction condition is:O/A is 1/1, sulfuric acid concentration 1mol/L, stirring
Incorporation time is 5min, settling time 5min, and two-stage back extraction is carried out under room temperature.Last organic phase after regeneration, returns again sharp
With.
(4) condensing crystallizing
Liquid carries out condensing crystallizing after purifying, and after testing, liquid-tight degree 1.25g/mL before concentration, heating evaporation is concentrated into density
For 1.65g/mL postcoolings to room temperature, emerald refined sulfuric acid nickel is obtained after crystallization, drying.
Its product quality and the comparison of national sector standard HG/T2824-2009 industrial sulphuric acid nickel are as shown in table 9.
The nickel sulfate product quality that 9 embodiment 3 of table is refining to obtain and the comparison of national sector standard HG/T2824-2009
As can be seen from Table 9, the nickel sulfate product quality that embodiment 3 obtains is higher than national standard《HG/T2824-2009》
Technology requirement, can be widely applied to plating and battery industry.
Claims (1)
1. a kind of process for purification of Copper making by-product crude nickle sulphate, it is characterised in that:The purification process steps are as follows:
Step 1:Na2S2O3Selective precipitation copper
In mass ratio 3:1 meter, with crude nickle sulphate of the water dissolution containing As, Ca, Co, Cu, Fe, Mg, Zn impurity, it is molten to obtain crude nickle sulphate
Liquid;
By Na2S2O3The molar ratio computing of nickel sulfate is three times in, using excessive Na2S2O3To making choice property of crude nickel sulfate solution
Cement copper, the initial pH of solution precipitation reaction is 0.5, reacts 2h under the conditions of 85 DEG C of temperature of control;After reaction to product into
Row filtering, obtains copper removal nickel sulfate solution;Wherein the removal rate of Cu is 99.94%~100%, the loss late of nickel for 0.75%~
0.80%;
Step 2:One step precipitated iron, arsenic, calcium, magnesium
Under the conditions of 85 DEG C, hydrogen peroxide is added in the nickel sulfate solution of step 1 copper removal, oxidation reaction 20min;Oxidation terminates
Afterwards, add in excessive sodium fluoride, adjust the pH value of solution as 4.5, react 2h, followed by filter, obtain except iron, arsenic, calcium and
The nickel sulfate solution of magnesium, wherein iron, arsenic, the removal rate of calcium and magnesium are respectively 99.38%~99.97%, 97.83%~99.85%,
97.64%~100%, 99.24%~100%;
Step 3:Synergic solvent extraction deep impurity-removing
By 1:The mixed organic solvents that soda soap rate is 65% are added to except the sulfuric acid of iron, arsenic, calcium and magnesium by 1 volume percentage
In nickel solution, be stirred 5min, balance pH is 4 or so, clarifies 5min, three-level counter-current extraction under room temperature, separation organic phase and
Water phase obtains extracting the nickel sulfate solution of miscellaneous organic phase and deep impurity-removing;Wherein zinc, cobalt, the extraction yield of nickel be respectively 100%,
98.18%~99.00%, 6.37%~7.82%;Three-level counter-current extraction condition is:The time is stirred as 5min, balance pH is left for 4
The right side, settling time 5min;
By 1:1 compare, first washs the miscellaneous organic phase of extraction, it is molten to return to crude nickle sulphate for liquid after washing with the acid deionized water of pH=3-4
In liquid;It is stripped again with 1mol/L sulfuric acid solutions to extracting miscellaneous organic phase, is stirred 5min, clarify 5min;It is carried out under room temperature
Two-stage is stripped, and separates organic phase and water phase, organic phase is through regeneration;
The mixed organic solvents press volume percentage, P507 25%, TBP 5%, sulfonated kerosene 70%;
Step 4:Condensing crystallizing
The nickel sulfate solution of deep impurity-removing is subjected to concentration postcooling to room temperature, then crystallized, separation and drying, obtains refined sulphur
Sour nickel.
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