CN104310496A - Crystalizing method for nickel sulfate water solution - Google Patents
Crystalizing method for nickel sulfate water solution Download PDFInfo
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- CN104310496A CN104310496A CN201410551542.8A CN201410551542A CN104310496A CN 104310496 A CN104310496 A CN 104310496A CN 201410551542 A CN201410551542 A CN 201410551542A CN 104310496 A CN104310496 A CN 104310496A
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- Prior art keywords
- nickel sulfate
- crystal
- crystalizing
- sulfate solution
- temperature
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- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 title claims abstract description 35
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title abstract description 15
- 239000013078 crystal Substances 0.000 claims abstract description 49
- 238000002425 crystallisation Methods 0.000 claims abstract description 37
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229940053662 nickel sulfate Drugs 0.000 claims abstract description 34
- 229940116202 nickel sulfate hexahydrate Drugs 0.000 claims abstract description 29
- RRIWRJBSCGCBID-UHFFFAOYSA-L nickel sulfate hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-]S([O-])(=O)=O RRIWRJBSCGCBID-UHFFFAOYSA-L 0.000 claims abstract description 28
- 230000008025 crystallization Effects 0.000 claims abstract description 20
- 229960000583 acetic acid Drugs 0.000 claims abstract description 15
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 239000012452 mother liquor Substances 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 33
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 13
- 238000011084 recovery Methods 0.000 claims description 3
- 239000010413 mother solution Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 7
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000001914 filtration Methods 0.000 abstract description 4
- 238000000926 separation method Methods 0.000 abstract description 4
- 239000002904 solvent Substances 0.000 abstract description 3
- 239000012535 impurity Substances 0.000 abstract description 2
- 239000002002 slurry Substances 0.000 abstract 2
- 238000001704 evaporation Methods 0.000 description 4
- HIRWGWMTAVZIPF-UHFFFAOYSA-N nickel;sulfuric acid Chemical compound [Ni].OS(O)(=O)=O HIRWGWMTAVZIPF-UHFFFAOYSA-N 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 229910052793 cadmium Inorganic materials 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 229910052745 lead Inorganic materials 0.000 description 3
- 229910052748 manganese Inorganic materials 0.000 description 3
- 150000002815 nickel Chemical class 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000009713 electroplating Methods 0.000 description 2
- 230000036571 hydration Effects 0.000 description 2
- 238000006703 hydration reaction Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000007614 solvation Methods 0.000 description 2
- VBICKXHEKHSIBG-UHFFFAOYSA-N 1-monostearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 description 1
- DCXXMTOCNZCJGO-UHFFFAOYSA-N Glycerol trioctadecanoate Natural products CCCCCCCCCCCCCCCCCC(=O)OCC(OC(=O)CCCCCCCCCCCCCCCCC)COC(=O)CCCCCCCCCCCCCCCCC DCXXMTOCNZCJGO-UHFFFAOYSA-N 0.000 description 1
- 241000080590 Niso Species 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- DAPUDVOJPZKTSI-UHFFFAOYSA-L ammonium nickel sulfate Chemical compound [NH4+].[NH4+].[Ni+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DAPUDVOJPZKTSI-UHFFFAOYSA-L 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- OJIJEKBXJYRIBZ-UHFFFAOYSA-N cadmium nickel Chemical compound [Ni].[Cd] OJIJEKBXJYRIBZ-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- LKNLEKUNTUVOML-UHFFFAOYSA-L nickel(2+);sulfate;hydrate Chemical compound O.[Ni+2].[O-]S([O-])(=O)=O LKNLEKUNTUVOML-UHFFFAOYSA-L 0.000 description 1
- 229910000008 nickel(II) carbonate Inorganic materials 0.000 description 1
- ZULUUIKRFGGGTL-UHFFFAOYSA-L nickel(ii) carbonate Chemical compound [Ni+2].[O-]C([O-])=O ZULUUIKRFGGGTL-UHFFFAOYSA-L 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000984 vat dye Substances 0.000 description 1
- 235000019154 vitamin C Nutrition 0.000 description 1
- 239000011718 vitamin C Substances 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a crystalizing method for a nickel sulfate water solution. The method comprises the steps of adjusting the temperature of the nickel sulfate water solution to 35-40DEG C; adding glacial acetic acid to separate out the crystal, wherein the volume of the glacial acetic acid is 50-60% of the volume of the nickel sulfate water solution; stirring, and crystalizing for 12-16 hours at constant temperature of 34+/-1DEG C so as to grow the crystal to obtain crystal slurry; filtering the crystal slurry, separating the crystallization mother liquor from the crystal, and drying the obtained crystal so as to obtain alpha-type nickel sulfate hexahydrate crystal. Through temperature adjustment, separation by solvent, and crystalizing at constant temperature, the method prepares the alpha-type nickel sulfate hexahydrate crystal which has regular crystal form, uninform grain size and good glossiness, is not easy to cake, and is superior to existing industrial nickel sulfate in chemical properties; and the method can obviously lower the crystalizing energy consumption and crystalizing temperature, is simple and reliable, has strong operability, has the crystallization rate of over 95%, does not introduce other impurities, has good economic value, and is a new method for crystalizing the nickel sulfate water solution.
Description
Technical field
The invention belongs to crystallization technique field, relate to a kind of crystallization method of nickel sulfate solution.
Background technology
Industrial sulphuric acid nickel is mainly used in electroplating industry, is the main nickel salt of electronickelling and chemical nickel plating, can in electroplating process dissociation nickel ion and sulfate ion.It is the catalyzer of oil hydrogenation in winterized stearin is produced, medicine industry is for the production of the catalyzer of vitamins C oxidizing reaction, the main raw material of nickel ammonium sulfate, nickel oxide, nickelous carbonate etc. is used as in inorganic industrial, for the production of the mordant of the blue or green gorgeous blue complexing agent of phthalein and vat dyes in printing and dyeing industry, also can be used for producing nickel-cadmium cell etc.
The method of nickel sulfate solution evaporation concentration, crystallisation by cooling is generally adopted to produce nickel sulfate hexahydrate product in industrial production.There is following shortcoming in this method: 1) because evaporation of water latent heat is very large, need consume a large amount of energy and boil off unnecessary moisture content, and crystallization terminal temperature is higher, primary crystallization rate is only 40 ~ 60%, and crystalline mother solution needs repeatedly to evaporate, and operating cost is very high; 2) solution evaporation process is fierce, and in operation, the degree of supersaturation of solution is difficult to control, thus the chemical quality of the finished product and physical appearance stable all not; 3) water at low temperature that the consumption of crystallisation by cooling process need is a large amount of, crystallizing cycle is long.
Summary of the invention
The object of this invention is to provide the crystallization method of the nickel sulfate solution that a kind of crystallisation process is gentle, crystallizing cycle is short, reduce energy consumption, improve percent crystallization in massecuite.
For achieving the above object, the technical solution adopted in the present invention is: a kind of crystallization method of nickel sulfate solution, is characterized in that, this crystallization method specifically carries out according to the following steps:
Step 1: the temperature of nickel sulfate solution is adjusted to 35 DEG C ~ 40 DEG C;
Step 2: glacial acetic acid is added in the nickel sulfate solution after step 1 temperature adjustment, add glacial acetic acid volume be 50% ~ 60% of nickel sulfate solution volume, crystallize out;
Step 3: stir, the crystal that step 2 is separated out is micro-suspended state, and crystallization makes crystal grow up in 12 ~ 16 hours under the constant temperature of 34 ± 1 DEG C, obtains magma;
Step 4: filtered by step 3 magma, be separated mother liquor and crystal, namely obtain nickel sulfate hexahydrate crystal after the drying of gained crystal, mother liquor delivers to acetic acid recovery system.
Crystallization method of the present invention prepares nickel sulfate hexahydrate crystal by measures such as temperature adjustment, solubilizing agent precipitation, thermostatical crystallizations, and technique is simple, reliable, workable, and percent crystallization in massecuite is high, and can not introduce other impurity; Obtained α-type nickel sulfate hexahydrate crystal crystal formation rule, uniform particle sizes, glossiness are good, not easily agglomerate, and chemical quality is better than the requirement of applicable industry single nickel salt standard (HG/T2824-2009); And can significantly reduce crystallization energy consumption and Tc, having good economic worth, is a kind of novel method of nickel sulfate solution crystallization.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail.
The deficiency of nickel sulfate hexahydrate crystal is prepared in order to overcome traditional evaporative crystallization, solve the problem that nickel sulfate solution evaporating concentration process energy consumption is large, primary crystallization rate is low, the invention provides a kind of method of the α-type of crystalline in a mild condition nickel sulfate hexahydrate crystal, specifically carry out according to the following steps:
Step 1: the temperature of nickel sulfate solution in crystallizer tank is adjusted to 35 DEG C ~ 40 DEG C;
Each concentration of component in this nickel sulfate solution: Ni:105.97g/L, Co:0.0016g/L, Cu:0.00038g/L, Fe:0.00065g/L, Pb; 0.0029g/L, Zn:0.00063g/L, Mn:0.0009g/L, Cd:0.00061g/L, Ca:0.0056g/L, Mg:0.0059g/L, Na:0.056g/L, pH4.0.
Step 2: solvent is separated out: add in the nickel sulfate solution after step 1 temperature adjustment by glacial acetic acid (normal temperature), add glacial acetic acid volume be 50% ~ 60% of nickel sulfate solution volume, crystallize out;
Step 3: stir with the rotating speed of 110 ± 10r/min, the crystal that step 2 is separated out is in micro-suspended state, and under the constant temperature of 34 ± 1 DEG C, crystallization makes crystal grow up in 12 ~ 16 hours, obtains magma;
Step 4: filtered by step 3 magma, be separated mother liquor and crystal, namely obtain nickel sulfate hexahydrate crystal after the drying of gained crystal, mother liquor delivers to acetic acid recovery system.
The principle of crystallization method of the present invention: in the water that polarity is stronger, water molecules can with Ni
2+and SO
4 2-solvation and be accumulated in Ni
2+and SO
4 2-form hydration layer around, but after adding the polarity acetic acid weak compared with water in nickel sulfate solution, molecular acid meeting and Ni
2+and SO
4 2-competition water molecules, weakens water molecules to Ni
2+and SO
4 2-solvation, make the portion of water in hydration layer seized by molecular acid, water molecules and Ni
2+and SO
4 2-form supersaturated solution, separate out nickel sulfate hexahydrate crystal.Because the quantity of single nickel salt crystalline water molecules and crystal habit change with temperature, be the α-type nickel sulfate hexahydrate crystal (α-NiSO of single crystal form for making the nickel sulfate hexahydrate crystal of precipitation
46H
2o), precipitation seven water nickel sulfate hexahydrate crystal (NiSO is avoided
47H
2or β-type nickel sulfate hexahydrate crystal (β-NiSO O)
46H
2o), experiment determines that nickel sulfate solution initial temperature is 35 DEG C ~ 40 DEG C, and crystallization temperature perseverance is 34 ± 1 DEG C, crystallization time 12 ~ 16h.
embodiment 1
By the temperature adjustment to 40 DEG C of 10.0L nickel sulfate solution, add 6.0L glacial acetic acid, rotating speed 110r/min stirs, and keep 34 DEG C of constant temperature 16 hours, then filtering separation, obtains nickel sulfate hexahydrate crystal 4.55kg after drying.
This nickel sulfate hexahydrate crystal is tested: this nickel sulfate hexahydrate crystal well-grown, particle diameter are 0.5 ~ 1.0mm, percent crystallization in massecuite is 95.66%, its chemical constitution is Ni:22.28%, Co:0.00039%, Cu:0.0001%, Fe:0.00042%, Pb:0.00048%, Zn:0.00029%, Mn:0.00015%, Cd:0.00012%, Ca:0.00055%, Mg:0.00084%, Na:0.00026%, water-insoluble: 0.0015%; Quality is better than the nickel sulfate hexahydrate crystal that industrial sulphuric acid nickel industry standard (HG/T2824-2009) requires.
embodiment 2
By the temperature adjustment to 38 DEG C of 10.0L nickel sulfate solution, add 5.0L glacial acetic acid, rotating speed 100r/min stirs, and keeps 35 DEG C of constant temperature 12 hours, then obtains nickel sulfate hexahydrate crystal 4.53kg after filtering separation, drying.
This nickel sulfate hexahydrate crystal is tested: this nickel sulfate hexahydrate crystal well-grown, particle diameter are 0.5 ~ 1.0mm, percent crystallization in massecuite is 95.03%, its chemical constitution is Ni:22.23%, Co:0.00041%, Cu:0.00011%, Fe:0.00040%, Pb:0.00049%, Zn:0.00029%, Mn:0.00014%, Cd:0.00012%, Ca:0.00054%, Mg:0.00082%, Na:0.00024%, water-insoluble: 0.0015%; Quality is better than the nickel sulfate hexahydrate crystal that industrial sulphuric acid nickel industry standard (HG/T2824-2009) requires.
embodiment 3
By the temperature adjustment to 35 DEG C of 10.0L nickel sulfate solution, add 5.5L glacial acetic acid, rotating speed 120r/min stirs, and keeps 33 DEG C of constant temperature 15 hours, then obtains nickel sulfate hexahydrate crystal 4.54kg after filtering separation, drying.
This nickel sulfate hexahydrate crystal is tested: this nickel sulfate hexahydrate crystal well-grown, particle diameter are 0.5 ~ 1.0mm, percent crystallization in massecuite is 95.41%, its chemical constitution is Ni:22.27%, Co:0.00039%, Cu:0.0001%, Fe:0.00041%, Pb:0.00049%, Zn:0.00028%, Mn:0.00015%, Cd:0.00011%, Ca:0.00055%, Mg:0.00081%, Na:0.00026%, water-insoluble: 0.0015%; Quality is better than the nickel sulfate hexahydrate crystal that industrial sulphuric acid nickel industry standard (HG/T2824-2009) requires.
Claims (6)
1. a crystallization method for nickel sulfate solution, is characterized in that, this crystallization method specifically carries out according to the following steps:
Step 1: the temperature of nickel sulfate solution is adjusted to 35 DEG C ~ 40 DEG C;
Step 2: glacial acetic acid is added in the nickel sulfate solution after step 1 temperature adjustment, add glacial acetic acid volume be 50% ~ 60% of nickel sulfate solution volume, crystallize out;
Step 3: stir, the crystal that step 2 is separated out is micro-suspended state, under the constant temperature of 34 ± 1 DEG C 12 ~ 16 hours, crystal is grown up, obtains magma;
Step 4: filtered by step 3 magma, is separated mother liquor and crystal, namely obtains nickel sulfate hexahydrate crystal after the drying of gained crystal.
2. the crystallization method of nickel sulfate solution according to claim 1, is characterized in that, the concentration of component of nickel sulfate solution in described step 1: Ni:105.97g/L, Co:0.0016g/L, Cu:0.00038g/L, Fe:0.00065g/L, Pb; 0.0029g/L, Zn:0.00063g/L, Mn:0.0009g/L, Cd:0.00061g/L, Ca:0.0056g/L, Mg:0.0059g/L, Na:0.056g/L.
3. the crystallization method of nickel sulfate solution according to claim 1, is characterized in that, the mixing speed in described step 3 is 110 ± 10r/min.
4. the crystallization method of nickel sulfate solution according to claim 1, is characterized in that, the crystallization time in described step 3 12 ~ 16 hours.
5. the crystallization method of nickel sulfate solution according to claim 1, is characterized in that, the nickel sulfate hexahydrate crystal in described step 4 is α-type nickel sulfate hexahydrate.
6. the crystallization method of nickel sulfate solution according to claim 1, is characterized in that, the crystalline mother solution in described step 4 delivers to acetic acid recovery system.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410551542.8A CN104310496B (en) | 2014-10-17 | 2014-10-17 | A kind of method for crystallising of nickel sulfate solution |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410551542.8A CN104310496B (en) | 2014-10-17 | 2014-10-17 | A kind of method for crystallising of nickel sulfate solution |
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| Publication Number | Publication Date |
|---|---|
| CN104310496A true CN104310496A (en) | 2015-01-28 |
| CN104310496B CN104310496B (en) | 2016-01-13 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10995014B1 (en) | 2020-07-10 | 2021-05-04 | Northvolt Ab | Process for producing crystallized metal sulfates |
| CN114225465A (en) * | 2021-12-31 | 2022-03-25 | 金川集团镍盐有限公司 | Method for producing electroplated nickel sulfate by continuous crystallization of nickel sulfate solution |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3884644A (en) * | 1969-09-16 | 1975-05-20 | Stamicarbon | Process for recovering ammonium sulphate from aqueous solutions of ammonium sulphate containing organic constituents and heavy metal ions |
| JPS57174102A (en) * | 1981-04-21 | 1982-10-26 | Nippon Synthetic Chem Ind Co Ltd:The | Crystallization method |
| CN1780671A (en) * | 2003-04-29 | 2006-05-31 | 阿克佐诺贝尔股份有限公司 | Processes involving the use of antisolvent crystallisation |
| CN101062793A (en) * | 2007-05-08 | 2007-10-31 | 广东光华化学厂有限公司 | Crystal growth method during alpha-type six hydration nickel sulfate interval crystallization process |
-
2014
- 2014-10-17 CN CN201410551542.8A patent/CN104310496B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3884644A (en) * | 1969-09-16 | 1975-05-20 | Stamicarbon | Process for recovering ammonium sulphate from aqueous solutions of ammonium sulphate containing organic constituents and heavy metal ions |
| JPS57174102A (en) * | 1981-04-21 | 1982-10-26 | Nippon Synthetic Chem Ind Co Ltd:The | Crystallization method |
| CN1780671A (en) * | 2003-04-29 | 2006-05-31 | 阿克佐诺贝尔股份有限公司 | Processes involving the use of antisolvent crystallisation |
| CN101062793A (en) * | 2007-05-08 | 2007-10-31 | 广东光华化学厂有限公司 | Crystal growth method during alpha-type six hydration nickel sulfate interval crystallization process |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10995014B1 (en) | 2020-07-10 | 2021-05-04 | Northvolt Ab | Process for producing crystallized metal sulfates |
| US12054401B2 (en) | 2020-07-10 | 2024-08-06 | Northvolt Ab | Process and method for producing crystallized metal sulfates |
| CN114225465A (en) * | 2021-12-31 | 2022-03-25 | 金川集团镍盐有限公司 | Method for producing electroplated nickel sulfate by continuous crystallization of nickel sulfate solution |
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| Publication number | Publication date |
|---|---|
| CN104310496B (en) | 2016-01-13 |
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Effective date of registration: 20240305 Address after: 737100 No.1 Lanzhou Road, Jinchuan District, Jinchang City, Gansu Province Patentee after: Jinchuan Group Nickel Salt Co.,Ltd. Country or region after: China Address before: 737103 No. 98, Jinchuan Road, Jinchang, Gansu Patentee before: JINCHUAN GROUP Co.,Ltd. Country or region before: China |
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