CN116555599A - Method for improving clarification of zinc sulfate solution neutralization indium precipitation solution - Google Patents
Method for improving clarification of zinc sulfate solution neutralization indium precipitation solution Download PDFInfo
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- CN116555599A CN116555599A CN202310600144.XA CN202310600144A CN116555599A CN 116555599 A CN116555599 A CN 116555599A CN 202310600144 A CN202310600144 A CN 202310600144A CN 116555599 A CN116555599 A CN 116555599A
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- indium
- zinc sulfate
- neutralization
- zinc
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- 229910052738 indium Inorganic materials 0.000 title claims abstract description 79
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 238000001556 precipitation Methods 0.000 title claims abstract description 39
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 title claims abstract description 34
- 229960001763 zinc sulfate Drugs 0.000 title claims abstract description 33
- 229910000368 zinc sulfate Inorganic materials 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000006386 neutralization reaction Methods 0.000 title claims abstract description 24
- 238000005352 clarification Methods 0.000 title claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 33
- 239000000843 powder Substances 0.000 claims abstract description 31
- 239000011701 zinc Substances 0.000 claims abstract description 27
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims abstract description 16
- 235000011941 Tilia x europaea Nutrition 0.000 claims abstract description 16
- 239000004571 lime Substances 0.000 claims abstract description 16
- 239000006228 supernatant Substances 0.000 claims abstract description 15
- 239000002893 slag Substances 0.000 claims abstract description 13
- 238000011084 recovery Methods 0.000 claims abstract description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002253 acid Substances 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 230000003472 neutralizing effect Effects 0.000 claims abstract description 7
- 239000002244 precipitate Substances 0.000 claims abstract description 6
- 230000008719 thickening Effects 0.000 claims abstract description 6
- 239000008394 flocculating agent Substances 0.000 claims abstract description 5
- 229910052742 iron Inorganic materials 0.000 claims abstract description 5
- 238000000746 purification Methods 0.000 claims abstract description 4
- 230000001276 controlling effect Effects 0.000 claims abstract description 3
- 230000001376 precipitating effect Effects 0.000 claims abstract description 3
- 230000001105 regulatory effect Effects 0.000 claims abstract description 3
- 230000035484 reaction time Effects 0.000 claims description 6
- 229920002401 polyacrylamide Polymers 0.000 claims description 4
- 235000009529 zinc sulphate Nutrition 0.000 claims 1
- 239000011686 zinc sulphate Substances 0.000 claims 1
- 238000009854 hydrometallurgy Methods 0.000 abstract description 4
- 238000003756 stirring Methods 0.000 description 10
- 239000002245 particle Substances 0.000 description 8
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical group [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 239000000741 silica gel Substances 0.000 description 6
- 229910002027 silica gel Inorganic materials 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 150000002739 metals Chemical class 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 238000001514 detection method Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000011787 zinc oxide Substances 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 125000005610 enamide group Chemical group 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 238000009858 zinc metallurgy Methods 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- 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
- C22B58/00—Obtaining gallium or indium
-
- 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
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
- C22B3/46—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes by substitution, e.g. by cementation
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Geology (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to a method for improving clarification of zinc sulfate solution neutralization indium precipitation solution, belonging to the technical field of zinc hydrometallurgy, comprising the following steps: q1: neutralizing and precipitating indium: slowly and uniformly adding zinc suboxide powder into the zinc sulfate solution to neutralize and precipitate indium, wherein the pH value of the end point of the neutralization and precipitation reaction is controlled to be 3.5-4.5; q2: neutralization of residual acid: adding lime powder into the liquid after indium precipitation in the step Q1 to neutralize residual acid, and regulating and controlling the pH value of a reaction end point to be 5.2-5.4; q3: clarifying and filtering: adding a flocculating agent into the liquid after the reaction in the step Q2 for thickening and clarifying, filtering the liquid, and sending the obtained supernatant to a subsequent iron removal and purification process, and sending the obtained indium slag precipitate to a subsequent indium recovery process; the method improves the recovery amount of indium in the zinc sulfate solution, and improves the clarification degree of the clarified liquid at the same time, thereby being convenient for subsequent utilization.
Description
Technical Field
The invention belongs to the technical field of zinc hydrometallurgy, and particularly relates to a method for improving clarification of zinc sulfate solution neutralization indium precipitation solution.
Background
In the zinc hydrometallurgy process, the leached zinc sulfate solution contains impurity elements such as indium, the indium belongs to valuable metals, the recovery value is achieved, if the indium in the zinc sulfate solution is not separated and recovered, the impurities such as indium in the zinc sulfate solution affect the quality of final zinc metallurgy, the metals with the recovery value become negative factors affecting main metals, the zinc metallurgy products are affected, and the valuable metals are lost. Therefore, in the zinc hydrometallurgy process, indium in the zinc sulfate solution is required to be separated out for recovery, and the separated clarified liquid can be reused after iron removal and purification. The more indium slag is obtained after indium precipitation, the more thorough the impurity removal is, and of course, more valuable metals can be recovered, meanwhile, the higher the clarification degree of the clarified liquid is, the subsequent utilization is facilitated, and the clarification degree of the clarified liquid is determined by the quantity and the state of various substances in the liquid.
In the existing neutralization indium precipitation process, the neutralization reaction end point is usually in a weak acid state, the pH is usually between 4.0 and 4.5, as disclosed in the patent application number 202110963801.8, wherein when indium slag is obtained by neutralization precipitation, the pH value of the solution is stirred and kept to be 4.0, and under the weak acid condition of the pH value of 4.0 to 4.5, on one hand, solid particles containing indium are easily formed in the zinc sulfate solution to be suspended in the solution, so that the recovery amount of indium is reduced, valuable metal loss is caused, and meanwhile, the degree of clarified liquid is influenced to a certain extent; on the other hand, when zinc suboxide is used for neutralization and indium precipitation, since acid-soluble silicon is generally contained in zinc suboxide, silica gel is easily formed under weak acidic conditions, and the clarity of clarified liquid is greatly affected.
Therefore, it is necessary to provide a method for improving the clarification of the neutralization indium precipitation solution of zinc sulfate solution, which improves the clarification degree of the clarified solution and facilitates the subsequent utilization while improving the recovery amount of indium in the zinc sulfate solution.
Disclosure of Invention
In order to overcome the problems in the background technology, the invention provides a method for improving the clarification of zinc sulfate solution neutralization indium precipitation liquid, which comprises the steps of neutralizing indium precipitation by using zinc suboxide, separating indium precipitation slag from liquid by flocculation filtration, removing iron from supernatant liquid, purifying the supernatant liquid, recycling the supernatant liquid, and recovering indium from the indium precipitation slag; the pH value is improved, so that the dissolubility of acid-soluble silicon in the zinc suboxide is reduced, the amount of silica gel formed by the zinc suboxide is reduced, the liquid clarity is improved, the improvement of the pH value is combined with the action of a flocculating agent, indium is reduced to suspend in a solution in an indium-containing solid particle state, and the effect of improving the clarity of the solution is also achieved while more indium is recovered.
In order to achieve the above purpose, the invention is realized by the following technical scheme:
the method for improving the clarification of the zinc sulfate solution neutralization indium precipitation solution comprises the following steps:
q1: neutralizing and precipitating indium: slowly and uniformly adding zinc suboxide powder into the zinc sulfate solution to neutralize and precipitate indium, wherein the pH value of the end point of the neutralization and precipitation reaction is controlled to be 3.5-4.5;
q2: neutralization of residual acid: adding lime powder into the liquid after indium precipitation in the step Q1 to neutralize residual acid, and regulating and controlling the pH value of a reaction end point to be 5.2-5.4;
q3: clarifying and filtering: adding a flocculating agent into the liquid after the reaction in the step Q2 for thickening and clarifying, filtering the liquid, and sending the obtained supernatant to a subsequent iron removal and purification process, and sending the obtained indium slag precipitate to a subsequent indium recovery process.
Preferably, in the step Q1, the zinc sulfate solution is added to the zinc suboxide powder according to the mass of the zinc suboxide powder so that the pH value of the solution reaches 3.5.
Preferably, in the step Q2, lime powder is added to make the pH value of the solution reach 5.2.
Preferably, the main components of the lime powder comprise CaO and Ca (OH) 2 、CaCO 3 One or more of the following.
Preferably, the flocculant is polyacrylamide.
Preferably, the reaction time in the step Q1 is from the end of the addition of the secondary zinc oxide powder, the reaction time in the step Q2 is from the end of the addition of the lime powder, the reaction time in the steps Q1 and Q2 is 0.5h, and the reaction temperature is 70-90 ℃.
Firstly, zinc sulfate solution and secondary zinc oxide are subjected to neutralization indium precipitation reaction in an optimal pH environment, then lime powder is added to neutralize residual acid in the solution, the pH value of the solution is properly increased to 5.2-5.4, and in an environment close to neutrality, the acid-soluble silicon solubility in the secondary zinc oxide is reduced, so that the probability of forming silica gel is also reduced, the amount of silica gel in the solution is reduced or eliminated, and the influence of the silica gel on the clarity of the solution is reduced. In the same pH environment, the suspension effect of a part of indium-containing solid particles is weakened, and after the flocculant is added, more indium-containing solid enters the indium-precipitating slag, so that the recovery amount of indium is improved.
The invention has the beneficial effects that:
according to the invention, lime powder is adopted to neutralize zinc sulfate solution to neutralize acid in indium precipitation solution, the pH value is adjusted, so that the pH value is improved compared with that when zinc oxide is used for neutralizing indium precipitation, on one hand, the suspension effect of indium-containing solid particles is weakened, more indium-containing solid particles are deposited by combining with the action of a flocculating agent and are filtered out together with indium precipitation slag, the indium content in the indium precipitation slag is higher, the indium recovery amount is improved, and the reduction of suspended particles is also beneficial to the improvement of the clarity of the indium precipitation solution; on the other hand, the solution environment close to neutrality reduces the dissolubility of acid-soluble silicon in the zinc suboxide, thereby reducing or eliminating silica gel formed by the zinc suboxide and improving the clarity of the neutral indium precipitation solution. And in the process of neutralizing indium precipitation of zinc suboxide, the pH value is kept in the optimal range of neutralizing indium precipitation effect.
Drawings
FIG. 1 is a process flow diagram of the present invention
Detailed Description
In order to make the objects, technical solutions and advantageous effects of the present invention more apparent, preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings, so as to facilitate understanding of the skilled person.
The zinc suboxide powders used in the examples of the invention all contained Zn 60%, indium 150g/t, with less than 320 mesh powder accounting for 90%.
Example 1
1L of a zinc sulfate solution containing 145g of zinc, 50mg of indium and 3g of sulfuric acid was placed in a 2L beaker. Slowly and uniformly adding 3.8g of zinc suboxide powder into the zinc sulfate solution, mechanically stirring, and stirring for 0.5h at 70 ℃ with the pH value of the reaction end point being 4.0; adding 0.05g of lime powder into the liquid, wherein the content of CaO in the lime powder is 90%, the content of powder smaller than 200 meshes is 90%, stirring for 0.5h at 70 ℃, and the pH value at the end of the reaction is 5.2; finally, adding polyacrylamide flocculant with the concentration of 1g/L into the liquid, wherein the adding amount is 10mg/L based on the volume of the liquid, pouring the mixture into a 2L measuring cylinder for thickening and clarifying after stirring for 30 seconds, and filtering the liquid after 1 minute to obtain supernatant and indium precipitation slag, wherein the clear supernatant accounts for 90%, and the supernatant contains 3mg of indium and the loss rate of indium is 6.0% through detection.
Example 2
1L of a zinc sulfate solution containing 150g of zinc, 75mg of indium and 5g of sulfuric acid was placed in a 2L beaker. Slowly and uniformly adding 5.9g of zinc suboxide powder into the zinc sulfate solution, mechanically stirring, and stirring for 0.5h at 90 ℃ with the pH value of the reaction end point being 4.5; 0.06g of lime powder, ca (OH) in which was added to the above-mentioned liquid 2 95% of the powder with the particle size smaller than 200 accounts for 90%, and the mixture is stirred for 0.5h at 90 ℃ with the pH value of the reaction end point of 5.4; finally, adding polypropylene with the concentration of 1g/L into the liquidThe addition amount of the enamide flocculant is 10mg/L calculated by the volume of the liquid, the enamide flocculant is poured into a 2L measuring cylinder for thickening and clarifying after stirring for 30s, the liquid is filtered after 50s to obtain supernatant and indium precipitation slag, wherein the clear supernatant accounts for 90%, and the supernatant contains 2.5mg of indium and the loss rate of indium is 3.3% through detection.
Example 3
1L of a zinc sulfate solution containing 148g of zinc, 60mg of indium and 4g of sulfuric acid was placed in a 2L beaker. Slowly and uniformly adding 5.0g of zinc suboxide powder into the zinc sulfate solution, mechanically stirring, and stirring for 0.5h at 80 ℃ with the pH value of the reaction end point being 3.5; adding 0.6g of lime powder into the liquid, wherein CaCO in the lime powder 3 85% of the powder with the particle size less than 200 accounts for 90%, the mixture is stirred for 0.5h at 80 ℃, and the pH value at the end of the reaction is 5.4; finally, adding polyacrylamide flocculant with the concentration of 1g/L into the liquid, wherein the adding amount is 10mg/L based on the volume of the liquid, pouring the mixture into a 2L measuring cylinder for thickening and clarifying after stirring for 30s, filtering the liquid after 70s to obtain supernatant and indium precipitation slag, wherein the clear supernatant accounts for 90%, and the supernatant contains 3mg of indium and the loss rate of indium is 5.0% through detection.
Finally, it is noted that the above-mentioned preferred embodiments illustrate rather than limit the invention, and that, although the invention has been described in detail with reference to the above-mentioned preferred embodiments, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the scope of the invention as defined by the appended claims.
Claims (6)
1. A method for improving clarification of zinc sulfate solution neutralization indium precipitation solution is characterized in that: the method for improving the clarification of the zinc sulfate solution neutralization indium precipitation solution comprises the following steps:
q1: neutralizing and precipitating indium: slowly and uniformly adding zinc suboxide powder into the zinc sulfate solution to neutralize and precipitate indium, wherein the pH value of the end point of the neutralization and precipitation reaction is controlled to be 3.5-4.5;
q2: neutralization of residual acid: adding lime powder into the liquid after indium precipitation in the step Q1 to neutralize residual acid, and regulating and controlling the pH value of a reaction end point to be 5.2-5.4;
q3: clarifying and filtering: adding a flocculating agent into the liquid after the reaction in the step Q2 for thickening and clarifying, filtering the liquid, and sending the obtained supernatant to a subsequent iron removal and purification process, and sending the obtained indium slag precipitate to a subsequent indium recovery process.
2. The method for improving the clarification of zinc sulfate solution neutralization indium precipitation solution according to claim 1, wherein the method comprises the following steps: the quality of the zinc sulfate solution added with the zinc suboxide powder in the step Q1 is determined to ensure that the PH value of the solution reaches 3.5.
3. The method for improving the clarification of zinc sulfate solution neutralization indium precipitation solution according to claim 1, wherein the method comprises the following steps: and in the step Q2, lime powder is added in an amount to ensure that the pH value of the solution reaches 5.2.
4. The method for improving the clarification of zinc sulfate solution neutralization indium precipitation solution according to claim 1, wherein the method comprises the following steps: the main component of the lime powder comprises CaO, ca (OH) 2 、CaCO 3 One or more of the following.
5. The method for improving the clarification of zinc sulfate solution neutralization indium precipitation solution according to claim 1, wherein the method comprises the following steps: the flocculant is polyacrylamide.
6. A method for improving the clarification of a zinc sulphate solution and indium precipitation solution according to any one of claims 1-5, wherein: the reaction time in the step Q1 is calculated from the completion of adding the zinc suboxide powder, the reaction time in the step Q2 is calculated from the completion of adding the lime powder, the reaction time in the steps Q1 and Q2 is 0.5h, and the reaction temperature is 70-90 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310600144.XA CN116555599A (en) | 2023-05-25 | 2023-05-25 | Method for improving clarification of zinc sulfate solution neutralization indium precipitation solution |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310600144.XA CN116555599A (en) | 2023-05-25 | 2023-05-25 | Method for improving clarification of zinc sulfate solution neutralization indium precipitation solution |
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| Publication Number | Publication Date |
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| CN116555599A true CN116555599A (en) | 2023-08-08 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202310600144.XA Pending CN116555599A (en) | 2023-05-25 | 2023-05-25 | Method for improving clarification of zinc sulfate solution neutralization indium precipitation solution |
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| Country | Link |
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| CN (1) | CN116555599A (en) |
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- 2023-05-25 CN CN202310600144.XA patent/CN116555599A/en active Pending
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