CN104310496B - A kind of method for crystallising of nickel sulfate solution - Google Patents
A kind of method for crystallising of nickel sulfate solution Download PDFInfo
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- CN104310496B CN104310496B CN201410551542.8A CN201410551542A CN104310496B CN 104310496 B CN104310496 B CN 104310496B CN 201410551542 A CN201410551542 A CN 201410551542A CN 104310496 B CN104310496 B CN 104310496B
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- nickel sulfate
- crystal
- sulfate solution
- crystallization
- crystallising
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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 claims abstract description 28
- 239000013078 crystal Substances 0.000 claims abstract description 45
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229940053662 nickel sulfate Drugs 0.000 claims abstract description 31
- 238000002425 crystallisation Methods 0.000 claims abstract description 29
- 230000008025 crystallization Effects 0.000 claims abstract description 27
- 229940116202 nickel sulfate hexahydrate Drugs 0.000 claims abstract description 27
- 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 26
- 229960000583 acetic acid Drugs 0.000 claims abstract description 14
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 10
- 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 31
- 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
- 239000000126 substance Substances 0.000 abstract description 7
- 239000002245 particle Substances 0.000 abstract description 5
- 238000001556 precipitation Methods 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000002904 solvent Substances 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 abstract description 2
- 238000001640 fractional crystallisation Methods 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 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
- 229910052793 cadmium Inorganic materials 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 238000001914 filtration Methods 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
- 239000000203 mixture Substances 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000009713 electroplating Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000007614 solvation Methods 0.000 description 2
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-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
- 229930003268 Vitamin C Natural products 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
- OJIJEKBXJYRIBZ-UHFFFAOYSA-N cadmium nickel Chemical compound [Ni].[Cd] OJIJEKBXJYRIBZ-UHFFFAOYSA-N 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
- 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
- 150000002815 nickel Chemical class 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
- 239000000346 nonvolatile oil Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000007254 oxidation reaction Methods 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
- 235000019154 vitamin C Nutrition 0.000 description 1
- 239000011718 vitamin C Substances 0.000 description 1
Abstract
The invention provides a kind of method for crystallising of nickel sulfate solution, the temperature of nickel sulfate solution is adjusted to 35 DEG C ~ 40 DEG C; Add the glacial acetic acid that volume is nickel sulfate solution volume 50% ~ 60%, crystallize out; Stir, under the constant temperature of 34 ± 1 DEG C, crystallization makes crystal grow up in 12 ~ 16 hours, obtains magma; Filter magma, fractional crystallization mother liquor and crystal, after the drying of gained crystal, obtain α-type nickel sulfate hexahydrate crystal.This method for crystallising obtains crystal formation rule by measures such as temperature adjustment, solubilizer precipitation, thermostatical crystallizations, uniform particle sizes, glossiness are good, not easily agglomerate, and chemical quality is better than the α-type nickel sulfate hexahydrate crystal of applicable industry nickelous sulfate standard; Can significantly reduce crystallization energy consumption and crystallization temperature, method is simple, reliable, and workable, percent crystallization in massecuite more than 95%, can not introduce other impurity; Having good economic worth, is a kind of new method of nickel sulfate solution crystallization.
Description
Technical field
The invention belongs to crystallization technique field, relate to a kind of method for crystallising 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 catalyst of oil hydrogenation in fixed oil is produced, medical industry is for the production of the catalyst of vitamin C oxidation reaction, the primary raw material of ammonium nickel 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 reducing dye in printing and dyeing industry, also can be used for producing nickel-cadmium cell etc.
The method of nickel sulfate solution evaporation and concentration, crystallisation by cooling is generally adopted to produce nickel sulfate hexahydrate product in industrial production.There is following shortcoming in the 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 outlet 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 final products 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 method for crystallising of the nickel sulfate solution that a kind of crystallization process is gentle, crystallizing cycle is short, reduce energy resource consumption, improve percent crystallization in massecuite.
For achieving the above object, the technical solution adopted in the present invention is: a kind of method for crystallising of nickel sulfate solution, is characterized in that, this method for crystallising 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.
Method for crystallising of the present invention prepares nickel sulfate hexahydrate crystal by measures such as temperature adjustment, solubilizer 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 nickelous sulfate standard (HG/T2824-2009); And can significantly reduce crystallization energy consumption and crystallization temperature, having good economic worth, is a kind of new method of nickel sulfate solution crystallization.
Detailed description of the invention
Below in conjunction with detailed description of the invention, 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 crystallization 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 method for crystallising of the present invention: in the water that polarity is stronger, hydrone can with Ni
2+and SO
4 2-solvation and be accumulated in Ni
2+and SO
4 2-form hydrated sheath 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 hydrone, weakens hydrone to Ni
2+and SO
4 2-solvation, make the portion of water in hydrated sheath seized by molecular acid, hydrone and Ni
2+and SO
4 2-form supersaturated solution, separate out nickel sulfate hexahydrate crystal.Because the quantity of nickelous sulfate 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 isolated by filtration, 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 composition 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 professional 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 isolated by filtration, 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 composition 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 professional 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 isolated by filtration, 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 composition 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 professional standard (HG/T2824-2009) requires.
Claims (4)
1. a method for crystallising for nickel sulfate solution, is characterized in that, this method for crystallising 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 12 ~ 16 hours, makes crystal grow up, obtain magma under the constant temperature of 34 ± 1 DEG C;
Step 4: filtered by step 3 magma, is separated mother liquor and crystal, namely obtains α-type nickel sulfate hexahydrate crystal after the drying of gained crystal.
2. the method for crystallising 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 method for crystallising of nickel sulfate solution according to claim 1, is characterized in that, the speed of agitator in described step 3 is 110 ± 10r/min.
4. the method for crystallising 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.
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| 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 (3)
| 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 |
| 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 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57174102A (en) * | 1981-04-21 | 1982-10-26 | Nippon Synthetic Chem Ind Co Ltd:The | Crystallization method |
-
2014
- 2014-10-17 CN CN201410551542.8A patent/CN104310496B/en active Active
Patent Citations (3)
| 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 |
| 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 |
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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 |