CN109911948A - The method of nitrate anion is removed in a kind of ambrose alloy cobalt sulfate liquor - Google Patents
The method of nitrate anion is removed in a kind of ambrose alloy cobalt sulfate liquor Download PDFInfo
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- CN109911948A CN109911948A CN201910214401.XA CN201910214401A CN109911948A CN 109911948 A CN109911948 A CN 109911948A CN 201910214401 A CN201910214401 A CN 201910214401A CN 109911948 A CN109911948 A CN 109911948A
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Abstract
The invention discloses a kind of methods that nitrate anion is removed in ambrose alloy cobalt sulfate liquor, belong to ambrose alloy cobalt technical field of wet metallurgy, solve the problems, such as that the nitrate anion in ambrose alloy cobalt sulfate liquor is difficult to remove.The present invention is the following steps are included: A, adjusting pH value: the pH value of addition sulfuric acid solution adjusting ambrose alloy cobalt sulfate liquor to 1.0 ~ 2.0；B, extraction removing nitrate ion: being extracted using extraction organic phase, and the extractant in the extraction organic phase is N235, and the load organic phases containing nitrate ion and the raffinate containing sulfate are respectively obtained after extraction.The present invention realizes that the selective extraction of nitrate anion separates using N235, and nitrate ion removal efficiency is high, and entire technical process can keep the pure and concentration of metal ions of sulfate liquor.
Description
Technical field
The invention belongs to ambrose alloy cobalt technical field of wet metallurgy, and in particular to remove nitre in a kind of ambrose alloy cobalt sulfate liquor
The method of acid group.
Background technique
In non-ferrous metal nitric acid process wet method smelting process, obtained transition product sulfate liquor is in production plating sulphur
When sour nickel crystallization product salt, due to the residual of nitrate anion, cause nickel sulfate product quality unqualified, product nitrate anion impurity content
Exceeded, in long-term production, the nitrate anion how effectively removed in sulfate liquor is one of technological difficulties.Metal nitrate is all
It is soluble, so being difficult the method removal nitrate ion with precipitating.More possible thinking has distillation, crystallization and purification, anti-
Infiltration, reaction method, anion exchange method etc., but above method is all at high cost, and production practical application is difficult.
The main ingredient of sulfate liquor involved in this method are as follows: 60 ~ 120g/L of Ni, 0.1 ~ 10g/L of Co, Cu 0.1
~25g/L、NO3 -0.5 ~ 10g/L, pH value of solution are 1.0 ~ 6.0.This sulfate liquor is mainly for the production of the production of high-purity sulfuric acid salt
Product, it is desirable that nitrate radical content is less than 0.2g/L.Data looks into new display, does not have also the higher sulfate of concentration of metal ions molten at present
The process report of nitrate ion is removed in liquid.
Summary of the invention
The object of the present invention is to provide a kind of methods that nitrate anion is removed in ambrose alloy cobalt sulfate liquor, to solve ambrose alloy cobalt
Nitrate anion in sulfate liquor is difficult to the problem of removing.
The technical scheme is that a kind of method that nitrate anion is removed in ambrose alloy cobalt sulfate liquor, including following step
It is rapid:
A, it adjusts pH value: the pH value of sulfuric acid solution adjusting ambrose alloy cobalt sulfate liquor is added to 1.0 ~ 2.0, in this acidity condition
Under, nitrate anion can be just extracted；
B, extraction removing nitrate ion: being extracted using extraction organic phase, and the extractant in the extraction organic phase is
N235 respectively obtains the load organic phases containing nitrate ion and the raffinate containing sulfate after extraction.
As a further improvement of the present invention, in stepb, the volumetric concentration for extracting N235 in organic phase is 10% ~ 30%.
As a further improvement of the present invention, in stepb, extraction phase ratio O/A is 1 ~ 2:1, carries out 1 ~ 2 stage countercurrent extraction
It takes, the mixed phase time is 2 ~ 5min, and the split-phase time is 5 ~ 10min.
As a further improvement of the present invention, in stepb, it extracts and contains diluent sulfonated kerosene and modification in organic phase
Agent isooctanol, modifying agent, which is added, can accelerate the split-phase time, and the volumetric concentration for extracting isooctanol in organic phase is 5% ~ 40%.
It as a further improvement of the present invention, further include step C, washing: using sulfuric acid scrubbing load organic phases, cleaning solution
Carry out wash cycle utilization.The purpose of washing is that the ambrose alloy cobalt sulfate liquor that will be become entrained in load organic phases is washed, and is mentioned
The high metal rate of recovery, the acid solution after washing can be repeatedly used for washing, before returning to extraction after metal ion content reaches certain value
Liquid reuse.
As a further improvement of the present invention, in step C, the concentration of washing sulfuric acid is 0 ~ 1mol/L(, that is, neutral water
Or sour water is washable), the washing of 1 ~ 3 stage countercurrent is carried out, washing is 1 ~ 2:1 compared to O/A, and the washing mixed phase time is 2 ~ 5min, point
The phase time is 5 ~ 10min.
As a further improvement of the present invention, further include step D, back extraction: using lye will be washed after load it is organic
It is mutually stripped, the strip liquor containing nitrate ion and regeneration organic phase is respectively obtained after back extraction, regeneration organic phase enters step
Rapid B carries out extraction cycle utilization.
As a further improvement of the present invention, in step D, lye selects sodium hydroxide solution.
As a further improvement of the present invention, in step D, the mass concentration of sodium hydroxide solution is 5 ~ 10%, is stripped phase
It is 1 ~ 3:1 than O/A, carries out the back extraction of 1 ~ 3 stage countercurrent, the mixed phase time is 5 ~ 10min, and the split-phase time is 2 ~ 5min.
It is high for nitrate ion content in ambrose alloy cobalt sulfate liquor, be difficult to separate and the requirement of comprehensive utilization of resources,
The invention proposes a kind of method of nitrate anion in efficient removal ambrose alloy cobalt sulfate liquor, achieve it is following the utility model has the advantages that
1, the present invention can extract the feature of acid using N235 using the method for N235 extraction removing nitrate anion, in high ambrose alloy cobalt gold
Belong to extraction removing nitrate anion in the sulfuric acid system of ion, solves the problems, such as to remove nitrate anion in ambrose alloy cobalt sulfate liquor；This
System is the sulfuric acid solution of ambrose alloy cobalt, and nickel cobalt copper and sulfate radical cannot form complex anion, and therefore, ambrose alloy cobalt does not have by N235
The condition (when N235 extracting metals ion, metal ion need to form complex anion with the anion in system) of extraction, so,
N235 will not extract ambrose alloy cobalt metal ion in this system, to realize the selective extraction separation of nitrate anion；
2, nitrate ion removal efficiency of the present invention is high, the solution 0.2g/L of < containing nitrate ion after separation, and extraction efficiency is high, grade
Number is few, and simple process is easy to operate, can save equipment investment, and production cost is low；
3, present invention back extraction effect is good, and regeneration organic phase returns to extraction section and recycles, and entire technical process can keep sulfate
The pure and concentration of metal ions of solution；
4, present invention process process design science, meets the requirement of comprehensive utilization of resources.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
Following examples further illustrate the present invention, but the invention is not limited in any way.
Embodiment 1,
Liquid ingredient is as shown in table 1 before extracting.
The method for removing nitrate anion is as follows:
A, pH value is adjusted: the pH value of the preceding liquid of addition sulfuric acid solution adjusting extraction to 1.0；
B, extraction removing nitrate ion: being extracted using extraction organic phase, and the volumetric concentration for extracting N235 in organic phase is
10%, the volumetric concentration of isooctanol is 5%, the volumetric concentration of sulfonated kerosene is 85%, and extraction phase ratio O/A is 1:1, and it is inverse to carry out single-stage
Stream extraction, mixed phase time are 2min, and the split-phase time is 5min, and the load organic phases containing nitrate ion are respectively obtained after extraction
With the raffinate containing sulfate, raffinate ingredient is as shown in table 2；
C, wash: use sulfuric acid scrubbing load organic phases, the concentration of washing sulfuric acid be 0mol/L(i.e. neutrality water washing), carry out
Single-stage washing, washing are 1:1 compared to O/A, and the washing mixed phase time is 2min, and the split-phase time is 5min, and cleaning solution carries out washing and follows
Ring utilizes；
D, be stripped: using mass concentration be 5% sodium hydroxide solution will be washed after load organic phases be stripped, be stripped
It is 1:1 compared to O/A, carries out single-stage countercurrent reextraction, the mixed phase time is 5min, and the split-phase time is 2min, respectively obtains and contains after back extraction
There are the strip liquor and regeneration organic phase of nitrate ion, strip liquor ingredient is as shown in table 3, and regeneration organic phase enters step B progress
Extraction cycle utilizes.
Embodiment 2,
Liquid ingredient is as shown in table 4 before extracting.
The method for removing nitrate anion is as follows:
A, pH value is adjusted: the pH value of the preceding liquid of addition sulfuric acid solution adjusting extraction to 1.5；
B, extraction removing nitrate ion: being extracted using extraction organic phase, and the volumetric concentration for extracting N235 in organic phase is
15%, the volumetric concentration of isooctanol is 20%, the volumetric concentration of sulfonated kerosene is 65%, and extraction phase ratio O/A is 1.5:1, carries out 2 grades
Counter-current extraction, mixed phase time are 3min, and the split-phase time is 7min, and it is organic that the load containing nitrate ion is respectively obtained after extraction
Mutually and the raffinate containing sulfate, raffinate ingredient are as shown in table 5；
C, it washs: using sulfuric acid scrubbing load organic phases, the concentration of washing sulfuric acid is 0.5mol/L, 2 stage countercurrents of progress wash,
Washing is 1.5:1 compared to O/A, and the washing mixed phase time is 3min, and the split-phase time is 7min, and cleaning solution carries out wash cycle utilization；
D, be stripped: using mass concentration be 7% sodium hydroxide solution will be washed after load organic phases be stripped, be stripped
Compared to O/A be 2:1, carry out 2 stage countercurrent back extraction, the mixed phase time be 7min, the split-phase time be 3min, respectively obtained after back extraction containing
The strip liquor and regeneration organic phase of nitrate ion, strip liquor ingredient is as shown in table 6, and regeneration organic phase enters step B and extracted
It takes and recycles.
Embodiment 3,
Liquid ingredient is as shown in table 7 before extracting.
The method for removing nitrate anion is as follows:
A, pH value is adjusted: the pH value of the preceding liquid of addition sulfuric acid solution adjusting extraction to 1.75；
B, extraction removing nitrate ion: being extracted using extraction organic phase, and the volumetric concentration for extracting N235 in organic phase is
25%, the volumetric concentration of isooctanol is 30%, the volumetric concentration of sulfonated kerosene is 45%, and extraction phase ratio O/A is 1.5:1, carries out 2 grades
Counter-current extraction, mixed phase time are 4min, and the split-phase time is 10min, and the load containing nitrate ion is respectively obtained after extraction to be had
Machine phase and raffinate containing sulfate, raffinate ingredient are as shown in table 8；
C, it washs: using sulfuric acid scrubbing load organic phases, the concentration of washing sulfuric acid, which is 0.75mol/L, carries out 3 stage countercurrents washes
Washing, washing compared to O/A is 2:1, and the washing mixed phase time is 4min, and the split-phase time is 8min, and cleaning solution carries out wash cycle utilization；
D, be stripped: using mass concentration be 8% sodium hydroxide solution will be washed after load organic phases be stripped, be stripped
It is 3:1 compared to O/A, carries out single-stage countercurrent reextraction, the mixed phase time is 8min, and the split-phase time is 4min, respectively obtains and contains after back extraction
There are the strip liquor and regeneration organic phase of nitrate ion, strip liquor ingredient is as shown in table 9, and regeneration organic phase enters step B progress
Extraction cycle utilizes.
Embodiment 4,
Liquid ingredient is as shown in table 10 before extracting.
The method for removing nitrate anion is as follows:
A, pH value is adjusted: the pH value of the preceding liquid of addition sulfuric acid solution adjusting extraction to 2.0；
B, extraction removing nitrate ion: being extracted using extraction organic phase, and the volumetric concentration for extracting N235 in organic phase is
30%, the volumetric concentration of isooctanol is 40%, the volumetric concentration of sulfonated kerosene is 30%, and extraction phase ratio O/A is 2:1, and 2 grades of progress is inverse
Stream extraction, mixed phase time are 5min, and the split-phase time is 10min, and it is organic that the load containing nitrate ion is respectively obtained after extraction
Mutually and the raffinate containing sulfate, raffinate ingredient are as shown in table 11；
C, it washs: using sulfuric acid scrubbing load organic phases, the concentration of washing sulfuric acid is 1mol/L, 3 stage countercurrents of progress are washed, washed
Washing compared to O/A is 2:1, and the washing mixed phase time is 5min, and the split-phase time is 10min, and cleaning solution carries out wash cycle utilization；
D, be stripped: using mass concentration be 10% sodium hydroxide solution will be washed after load organic phases be stripped, be stripped
It is 3:1 compared to O/A, carries out three-level countercurrent reextraction, the mixed phase time is 10min, and the split-phase time is 5min, respectively obtains and contains after back extraction
There are the strip liquor and regeneration organic phase of nitrate ion, strip liquor ingredient is as shown in table 12, and regeneration organic phase enters step B progress
Extraction cycle utilizes.
Claims (9)
1. removing the method for nitrate anion in a kind of ambrose alloy cobalt sulfate liquor, it is characterised in that the following steps are included:
A, pH value is adjusted: the pH value of addition sulfuric acid solution adjusting ambrose alloy cobalt sulfate liquor to 1.0 ~ 2.0；
B, extraction removing nitrate ion: being extracted using extraction organic phase, and the extractant in the extraction organic phase is
N235 respectively obtains the load organic phases containing nitrate ion and the raffinate containing sulfate after extraction.
2. removing the method for nitrate anion in a kind of ambrose alloy cobalt sulfate liquor according to claim 1, it is characterised in that:
In step B, the volumetric concentration of N235 is 10% ~ 30% in the extraction organic phase.
3. removing the method for nitrate anion in a kind of ambrose alloy cobalt sulfate liquor according to claim 2, it is characterised in that:
In step B, extraction phase ratio O/A be 1 ~ 2:1, carry out 1 ~ 2 stage countercurrent extraction, the mixed phase time be 2 ~ 5min, the split-phase time be 5 ~
10min。
4. removing the method for nitrate anion in a kind of ambrose alloy cobalt sulfate liquor according to claim 3, it is characterised in that:
In step B, diluent sulfonated kerosene and modifying agent isooctanol are contained in the extraction organic phase, extracts isooctanol in organic phase
Volumetric concentration is 5% ~ 40%.
5. a kind of method for removing nitrate anion described in any one of -4 in ambrose alloy cobalt sulfate liquor according to claim 1,
Be characterized in that: further including step C, washing: using sulfuric acid scrubbing load organic phases, cleaning solution carries out wash cycle utilization.
6. removing the method for nitrate anion in a kind of ambrose alloy cobalt sulfate liquor according to claim 5, it is characterised in that:
In step C, the concentration of washing sulfuric acid is 0 ~ 1mol/L, carries out the washing of 1 ~ 3 stage countercurrent, and washing is 1 ~ 2:1, washing compared to O/A
The mixed phase time is 2 ~ 5min, and the split-phase time is 5 ~ 10min.
7. removing the method for nitrate anion in a kind of ambrose alloy cobalt sulfate liquor according to claim 6, it is characterised in that: also
Including step D, back extraction: using lye will be washed after load organic phases be stripped, respectively obtain after back extraction containing nitric acid
The strip liquor and regeneration organic phase of radical ion, regeneration organic phase enter step B and carry out extraction cycle utilization.
8. removing the method for nitrate anion in a kind of ambrose alloy cobalt sulfate liquor according to claim 7, it is characterised in that:
In step D, the lye selects sodium hydroxide solution.
9. removing the method for nitrate anion in a kind of ambrose alloy cobalt sulfate liquor according to claim 8, it is characterised in that:
In step D, the mass concentration of sodium hydroxide solution is 5 ~ 10%, back extraction compared to O/A be 1 ~ 3:1, carries out the back extraction of 1 ~ 3 stage countercurrent, mixed
The phase time is 5 ~ 10min, and the split-phase time is 2 ~ 5min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112811728A (en) * | 2020-12-30 | 2021-05-18 | 广东先导稀材股份有限公司 | Method for standard treatment of mother liquor for producing superfine spherical silver powder and recycling valuable components |
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| US3870060A (en) * | 1974-02-26 | 1975-03-11 | Stora Kopparbergs Bergslags Ab | Method of removing monovalent inorganic acids from an aqueous solution containing metal salts of the acids |
| CN105905951A (en) * | 2016-06-08 | 2016-08-31 | 广东光华科技股份有限公司 | Method for efficiently removing nitrate radical impurities in cobalt sulfate solution |
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2019
- 2019-03-20 CN CN201910214401.XA patent/CN109911948A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3870060A (en) * | 1974-02-26 | 1975-03-11 | Stora Kopparbergs Bergslags Ab | Method of removing monovalent inorganic acids from an aqueous solution containing metal salts of the acids |
| CN105905951A (en) * | 2016-06-08 | 2016-08-31 | 广东光华科技股份有限公司 | Method for efficiently removing nitrate radical impurities in cobalt sulfate solution |
Non-Patent Citations (1)
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| 朱晓达等: ""制纯磷酸及其盐类的过程开发-溶剂萃取法净化磷酸的工艺研究"", 《化肥工业》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112811728A (en) * | 2020-12-30 | 2021-05-18 | 广东先导稀材股份有限公司 | Method for standard treatment of mother liquor for producing superfine spherical silver powder and recycling valuable components |
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