CN113277547B - Method for producing zinc sulfate by using low-zinc material - Google Patents
Method for producing zinc sulfate by using low-zinc material Download PDFInfo
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- CN113277547B CN113277547B CN202110514125.6A CN202110514125A CN113277547B CN 113277547 B CN113277547 B CN 113277547B CN 202110514125 A CN202110514125 A CN 202110514125A CN 113277547 B CN113277547 B CN 113277547B
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- sulfuric acid
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- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 71
- 239000011701 zinc Substances 0.000 title claims abstract description 71
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 title claims abstract description 50
- 229960001763 zinc sulfate Drugs 0.000 title claims abstract description 50
- 229910000368 zinc sulfate Inorganic materials 0.000 title claims abstract description 50
- 239000000463 material Substances 0.000 title claims abstract description 40
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 72
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 52
- 238000001914 filtration Methods 0.000 claims abstract description 39
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 38
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 35
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 19
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 19
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 17
- 239000001110 calcium chloride Substances 0.000 claims abstract description 17
- 229910001628 calcium chloride Inorganic materials 0.000 claims abstract description 17
- UOURRHZRLGCVDA-UHFFFAOYSA-D pentazinc;dicarbonate;hexahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Zn+2].[Zn+2].[Zn+2].[Zn+2].[Zn+2].[O-]C([O-])=O.[O-]C([O-])=O UOURRHZRLGCVDA-UHFFFAOYSA-D 0.000 claims abstract description 17
- 210000000582 semen Anatomy 0.000 claims abstract description 15
- 238000001704 evaporation Methods 0.000 claims abstract description 14
- 229910000000 metal hydroxide Inorganic materials 0.000 claims abstract description 14
- 150000004692 metal hydroxides Chemical class 0.000 claims abstract description 14
- 238000000227 grinding Methods 0.000 claims abstract description 13
- 238000002386 leaching Methods 0.000 claims abstract description 10
- 238000001354 calcination Methods 0.000 claims abstract description 7
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 10
- 239000013049 sediment Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 6
- 239000000919 ceramic Substances 0.000 claims description 5
- 239000011521 glass Substances 0.000 claims description 5
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 5
- 229910052737 gold Inorganic materials 0.000 claims description 5
- 239000010931 gold Substances 0.000 claims description 5
- 238000003837 high-temperature calcination Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 229910052697 platinum Inorganic materials 0.000 claims description 5
- 239000002699 waste material Substances 0.000 abstract description 7
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- 239000002351 wastewater Substances 0.000 abstract description 4
- 238000011084 recovery Methods 0.000 abstract 1
- 239000000428 dust Substances 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 229910052797 bismuth Inorganic materials 0.000 description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 3
- 229910052793 cadmium Inorganic materials 0.000 description 3
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 3
- 229910052738 indium Inorganic materials 0.000 description 3
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910001297 Zn alloy Inorganic materials 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- TVZPLCNGKSPOJA-UHFFFAOYSA-N copper zinc Chemical compound [Cu].[Zn] TVZPLCNGKSPOJA-UHFFFAOYSA-N 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- JQJCSZOEVBFDKO-UHFFFAOYSA-N lead zinc Chemical compound [Zn].[Pb] JQJCSZOEVBFDKO-UHFFFAOYSA-N 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- FMRLDPWIRHBCCC-UHFFFAOYSA-L Zinc carbonate Chemical compound [Zn+2].[O-]C([O-])=O FMRLDPWIRHBCCC-UHFFFAOYSA-L 0.000 description 1
- 239000005083 Zinc sulfide Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 238000005246 galvanizing Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 229910001414 potassium ion Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 239000011667 zinc carbonate Substances 0.000 description 1
- 229910000010 zinc carbonate Inorganic materials 0.000 description 1
- 235000004416 zinc carbonate Nutrition 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/06—Sulfates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- 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
Abstract
The invention relates to the technical field of metal recovery in zinc wastewater, in particular to a method for producing zinc sulfate by utilizing low-zinc materials, which mainly comprises the steps of grinding the low-zinc materials, adding water and filtering to obtain zinc primary pulp; adding calcium chloride into the zinc primary pulp, filtering, completely electrolyzing the filtered zinc primary pulp, and then evaporating and crystallizing to obtain metal hydroxide; calcining the metal hydroxide obtained in the second step at high temperature to obtain metal oxide, adding water into the metal oxide to dissolve the metal oxide, adding dilute sulfuric acid into the metal oxide, and filtering the metal oxide to obtain crude zinc sulfate seminal fluid; introducing carbon dioxide into the crude zinc sulfate semen, filtering to obtain basic zinc carbonate, and leaching the basic zinc carbonate; and (3) completely dissolving basic zinc carbonate by using dilute sulfuric acid, adding excessive zinc powder, filtering to obtain refined sulfuric acid refined solution, and evaporating and crystallizing the refined sulfuric acid refined solution to obtain the finished product zinc sulfate. The invention effectively avoids the waste of the existing low-zinc materials, and simultaneously, the zinc in the low-zinc materials can be effectively extracted, and the purity of the extracted zinc sulfate is excellent.
Description
Technical Field
The invention relates to the technical field of zinc-containing wastewater treatment, in particular to a method for producing zinc sulfate by utilizing low-zinc materials.
Background
With the development of economy, the recycling of solid waste is becoming more and more interesting, wherein zinc-containing noble metal flue gas and zinc-containing lead dust in steel plants, metallurgical zinc-containing dust mud, blast furnace dust, electric furnace dust, blast furnace gas mud, converter OG mud, phosphating mud, lead-zinc tailings, zinc-containing electroplating wastewater, lead-zinc smelting wastewater, high-concentration waste liquid discharged from hot galvanizing factories, waste dry batteries, waste copper-zinc alloy filter materials, waste copper-zinc alloy catalysts in alcohol dehydrogenation aldehyde and ketone production and the like become the main zinc-containing three-waste sources at present, and are often accompanied with impurity element ions such as copper, manganese, iron, lead, chromium, aluminum, nickel and the like, thereby becoming key factors for restricting the preparation of high-purity zinc sulfate products and application by using the same. For example, when the cobalt content in zinc sulfate is more than 1mg/L, the effect of the zinc electrolysis system current is reduced, and hardening occurs in severe cases. And when the content of copper and the isolator exceeds the standard, a high-purity 0# zinc product cannot be synthesized. When the content of Mn, fe, pb, cr, al and Ni ions exceeds the standard, the synthesized zinc sulfide product is greatly discounted in terms of chromaticity, hiding rate and the like. Therefore, the zinc hydrometallurgy process has strict regulation on the content of impurity elements in the zinc sulfate solution, the impurity content in the finished zinc sulfate is not higher than 0.8ppm, and the requirements on the impurity content are lower in some application fields.
The prior art uses expensive additives when extracting and producing zinc sulfate from low-zinc materials, the process is complex, the production cost is high, and the purity and quality of the extracted zinc sulfate product are not up to the standard. And other elements in the low-zinc material can seriously obstruct the extraction of zinc, and simultaneously, the added sodium and potassium ions in the added medicament can bring great trouble to the extraction of zinc.
Disclosure of Invention
The invention aims to provide a method for producing zinc sulfate by utilizing low-zinc materials, which aims to solve the problems in the background technology.
A method for producing zinc sulfate by using low-zinc materials, comprising the following steps:
step one: grinding the low-zinc material, adding water, and filtering to obtain zinc primary pulp;
step two: adding calcium chloride into the zinc primary pulp, filtering, completely electrolyzing the filtered zinc primary pulp, and then evaporating and crystallizing to obtain metal hydroxide;
step three: calcining the metal hydroxide obtained in the second step at high temperature to obtain metal oxide, adding water into the metal oxide to dissolve the metal oxide, adding dilute sulfuric acid into the metal oxide, and filtering the metal oxide to obtain crude zinc sulfate seminal fluid;
step four: introducing carbon dioxide into the crude zinc sulfate semen, filtering to obtain basic zinc carbonate, and leaching the basic zinc carbonate;
step five: and (3) completely dissolving basic zinc carbonate by using dilute sulfuric acid, adding excessive zinc powder, filtering to obtain refined sulfuric acid refined solution, and evaporating and crystallizing the refined sulfuric acid refined solution to obtain the finished product zinc sulfate.
Preferably, the diameter of the low-zinc material in the first step is 100-300 meshes after grinding.
Preferably, the concentration of calcium chloride in the second step is 0.2mol/L, and 100ml of calcium chloride is continuously added after no precipitation is generated.
Preferably, the electrode in the second step is an inert electrode, specifically platinum and gold.
Preferably, the high temperature calcination temperature in the third step is 600 ° -700 °.
Preferably, the volume of water added in the third step is 3:2 with respect to the volume of the metal oxide.
Preferably, the concentration of the dilute sulfuric acid added in the third step is 0.1mol/L, and the dilute sulfuric acid is continuously stirred by a stirring rod, wherein the stirring rod is made of ceramic and glass materials.
Preferably, the flow rate of carbon dioxide introduced in the fourth step is 1m/s, and the carbon dioxide introducing process is performed in the filter funnel, the operation of carbon dioxide introducing and filtering in the fourth step is repeated at least once, and no sediment is produced in the last step.
Preferably, the number of leaching in the fifth step is 3-5.
Compared with the prior art, the invention has the beneficial effects that: extracting soluble ions in zinc waste by grinding and adding water and filtering insoluble substances, grinding to 100-300 meshes to ensure sufficient water solubility, adding calcium chloride and filtering to remove sulfate ions in the solution, completely removing chloride ions in the solution by inert electrode electrolysis so as to change the solution into metal hydroxide suspension, evaporating and crystallizing, calcining at high temperature to change metal hydroxide into oxide, adding dilute sulfuric acid to extract zinc and filtering to obtain crude zinc sulfate semen, introducing carbon dioxide into the crude zinc sulfate semen and filtering operation to obtain high-purity zinc carbonate, dissolving the high-purity zinc sulfate by secondary sulfuric acid, adding excessive zinc powder to obtain refined zinc sulfate semen, evaporating and crystallizing to obtain high-purity zinc sulfate.
Detailed Description
The invention discloses a method for producing zinc sulfate by utilizing low-zinc materials, and the invention is further described in detail by specific examples.
Example 1
The method for producing zinc sulfate by using the low-zinc material in the embodiment mainly comprises the following steps:
step one: grinding the low-zinc material, adding water, and filtering to obtain zinc primary pulp;
step two: adding calcium chloride into the zinc primary pulp, filtering, completely electrolyzing the filtered zinc primary pulp, and then evaporating and crystallizing to obtain metal hydroxide;
step three: calcining the metal hydroxide obtained in the second step at high temperature to obtain metal oxide, adding water into the metal oxide to dissolve the metal oxide, adding dilute sulfuric acid into the metal oxide, and filtering the metal oxide to obtain crude zinc sulfate seminal fluid;
step four: introducing carbon dioxide into the crude zinc sulfate semen, filtering to obtain basic zinc carbonate, and leaching the basic zinc carbonate;
step five: and (3) completely dissolving basic zinc carbonate by using dilute sulfuric acid, adding excessive zinc powder, filtering to obtain refined sulfuric acid refined solution, and evaporating and crystallizing the refined sulfuric acid refined solution to obtain the finished product zinc sulfate.
The diameter of the low-zinc material after grinding in the first step is 100-300 meshes.
In the second step, the concentration of calcium chloride is 0.2mol/L, and 100ml of calcium chloride is continuously added after no sediment is generated, and the electrode in the second step is an inert electrode, specifically platinum and gold.
The high-temperature calcination temperature in the third step is 600-700 degrees, the volume ratio of water to metal oxide is 3:2, the concentration of the added dilute sulfuric acid is 0.1mol/L, and the dilute sulfuric acid is continuously stirred by a stirring rod which is made of ceramic and glass materials.
And in the fourth step, the flow speed of carbon dioxide is 1m/s, the carbon dioxide is introduced into the filter funnel, the filtering operation is repeated at least once, and no sediment is produced for the last time.
And in the fifth step, the leaching times are 3-5 times.
Example 2
The method for producing zinc sulfate by using the low-zinc material in the embodiment mainly comprises the following steps:
the method for recycling zinc, lead, indium, cadmium and bismuth from zinc-containing wastewater mainly comprises the following steps:
step one: grinding the low-zinc material, adding water, and filtering to obtain zinc primary pulp;
step two: adding calcium chloride into the zinc primary pulp, filtering, completely electrolyzing the filtered zinc primary pulp, and then evaporating and crystallizing to obtain metal hydroxide;
step three: calcining the metal hydroxide obtained in the second step at high temperature to obtain metal oxide, adding water into the metal oxide to dissolve the metal oxide, adding dilute sulfuric acid into the metal oxide, and filtering the metal oxide to obtain crude zinc sulfate seminal fluid;
step four: introducing carbon dioxide into the crude zinc sulfate semen and filtering to obtain basic zinc carbonate;
step five: and (3) completely dissolving basic zinc carbonate by using dilute sulfuric acid, adding excessive zinc powder, filtering to obtain refined sulfuric acid refined solution, and evaporating and crystallizing the refined sulfuric acid refined solution to obtain the finished product zinc sulfate.
The diameter of the low-zinc material after grinding in the first step is 100-300 meshes.
In the second step, the concentration of calcium chloride is 0.2mol/L, and 100ml of calcium chloride is continuously added after no sediment is generated, and the electrode in the second step is an inert electrode, specifically platinum and gold.
The high-temperature calcination temperature in the third step is 600-700 degrees, the volume ratio of water to metal oxide is 3:2, the concentration of the added dilute sulfuric acid is 0.1mol/L, and the dilute sulfuric acid is continuously stirred by a stirring rod which is made of ceramic and glass materials.
And in the fourth step, the flow speed of carbon dioxide is 1m/s, the carbon dioxide is introduced into the filter funnel, the filtering operation is repeated at least once, and no sediment is produced for the last time.
And in the fifth step, the leaching times are 3-5 times.
Example 3
The method for producing zinc sulfate by using the low-zinc material in the embodiment mainly comprises the following steps:
step one: grinding the low-zinc material, adding water, and filtering to obtain zinc primary pulp;
step two: adding calcium chloride into the zinc primary pulp, filtering, completely electrolyzing the filtered zinc primary pulp, and then evaporating and crystallizing to obtain metal hydroxide;
step three: calcining the metal hydroxide obtained in the second step at high temperature to obtain metal oxide, adding water into the metal oxide to dissolve the metal oxide, adding dilute sulfuric acid into the metal oxide, and filtering the metal oxide to obtain crude zinc sulfate seminal fluid;
step four: introducing carbon dioxide into the crude zinc sulfate semen, filtering to obtain basic zinc carbonate, and leaching the basic zinc carbonate by deionized water;
step five: and (3) completely dissolving basic zinc carbonate by using dilute sulfuric acid, adding excessive zinc powder, filtering to obtain refined sulfuric acid refined solution, and evaporating and crystallizing the refined sulfuric acid refined solution to obtain the finished product zinc sulfate.
The diameter of the low-zinc material after grinding in the first step is 100-300 meshes.
In the second step, the concentration of calcium chloride is 0.2mol/L, and 100ml of calcium chloride is continuously added after no sediment is generated, and the electrode in the second step is an inert electrode, specifically platinum and gold.
The high-temperature calcination temperature in the third step is 600-700 degrees, the volume ratio of water to metal oxide is 3:2, the concentration of the added dilute sulfuric acid is 0.1mol/L, and the dilute sulfuric acid is continuously stirred by a stirring rod which is made of ceramic and glass materials.
And in the fourth step, the flow speed of carbon dioxide is 1m/s, the carbon dioxide is introduced into the filter funnel, the filtering operation is repeated at least once, and no sediment is produced for the last time.
And in the fifth step, the leaching times are 3-5 times.
The results of the purity analysis of each metal are shown below
| Comparison item | Example 1 | Example 2 | Example 3 |
| Purity of zinc sulfate | 99.32％ | 96.54％ | 98.88％ |
Wherein I is the metal content of zinc, lead, indium, cadmium and bismuth in the finished product of the example II, the metal content of zinc, lead, indium, cadmium and bismuth in the finished product of the example III.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the above-described embodiments, and that the above-described embodiments and descriptions are only preferred embodiments of the present invention, and are not intended to limit the invention, and that various changes and modifications may be made therein without departing from the spirit and scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (9)
1. A method for producing zinc sulfate by using low-zinc materials is characterized in that: comprises the following steps:
step one: grinding the low-zinc material, adding water, and filtering to obtain zinc primary pulp;
step two: adding calcium chloride into the zinc primary pulp, filtering, completely electrolyzing the filtered zinc primary pulp, and then evaporating and crystallizing to obtain metal hydroxide;
step three: calcining the metal hydroxide obtained in the second step at high temperature to obtain metal oxide, adding water into the metal oxide to dissolve the metal oxide, adding dilute sulfuric acid into the metal oxide, and filtering the metal oxide to obtain crude zinc sulfate seminal fluid;
step four: introducing carbon dioxide into the crude zinc sulfate semen, filtering to obtain basic zinc carbonate, and leaching the basic zinc carbonate;
step five: and (3) completely dissolving basic zinc carbonate by using dilute sulfuric acid, adding excessive zinc powder, filtering to obtain refined sulfuric acid refined solution, and evaporating and crystallizing the refined sulfuric acid refined solution to obtain the finished product zinc sulfate.
2. A method for producing zinc sulfate from a low zinc material according to claim 1, wherein: the diameter of the low-zinc material in the first step is 100-300 meshes after grinding.
3. A method for producing zinc sulfate from low zinc material according to claim 2, wherein: in the second step, the concentration of calcium chloride is 0.2mol/L, and 100ml of calcium chloride is continuously added until no sediment is generated.
4. A method for producing zinc sulfate from a low zinc material according to claim 1, wherein: the electrode in the second step is an inert electrode, and is specifically platinum and gold.
5. A method for producing zinc sulfate from a low zinc material according to claim 1, wherein: the high-temperature calcination temperature in the third step is 600-700 ℃.
6. A method for producing zinc sulfate from a low zinc material according to claim 1, wherein: the volume of water added in the third step and the volume ratio of the metal oxide are 3:2.
7. A method for producing zinc sulfate from a low zinc material according to claim 1, wherein: the concentration of the dilute sulfuric acid added in the third step is 0.1mol/L, and the dilute sulfuric acid is continuously stirred by a stirring rod which is made of ceramic and glass materials.
8. A method for producing zinc sulfate from a low zinc material according to claim 1, wherein: the flow speed of carbon dioxide introduced in the fourth step is 1m/s, the carbon dioxide introducing process is carried out in the filter funnel, the operation of carbon dioxide introducing and filtering in the fourth step is repeated at least once, and no sediment is produced in the last step.
9. A method for producing zinc sulfate from a low zinc material according to claim 1, wherein: and in the fifth step, the leaching times are 3-5 times.
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Citations (21)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB249609A (en) * | 1924-12-29 | 1926-03-29 | Samuel Field | Improvements in or relating to the electrolytic production of zinc from ores or the like |
| AT266778B (en) * | 1964-10-02 | 1968-11-25 | Asturienne Mines Comp Royale | Process for obtaining a zinc sulphate solution from ferrites |
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| AT266778B (en) * | 1964-10-02 | 1968-11-25 | Asturienne Mines Comp Royale | Process for obtaining a zinc sulphate solution from ferrites |
| US3655538A (en) * | 1969-05-19 | 1972-04-11 | Texas Gulf Sulphur Co | Process for electrowinning zinc from sulfide concentrates |
| CA1133228A (en) * | 1980-10-24 | 1982-10-12 | Robert C. Kerby | Purification of zinc sulphate solution |
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| CN113277547A (en) | 2021-08-20 |
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