CN103864157B - A kind of preparation method of amorphous state nickel sulfide - Google Patents
A kind of preparation method of amorphous state nickel sulfide Download PDFInfo
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- CN103864157B CN103864157B CN201410074075.4A CN201410074075A CN103864157B CN 103864157 B CN103864157 B CN 103864157B CN 201410074075 A CN201410074075 A CN 201410074075A CN 103864157 B CN103864157 B CN 103864157B
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- sulfide
- amorphous state
- dispersant
- nickel sulfide
- liquid
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- WWNBZGLDODTKEM-UHFFFAOYSA-N sulfanylidenenickel Chemical compound [Ni]=S WWNBZGLDODTKEM-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000010949 copper Substances 0.000 claims abstract description 42
- 229910052802 copper Inorganic materials 0.000 claims abstract description 42
- 229910052979 sodium sulfide Inorganic materials 0.000 claims abstract description 38
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000003756 stirring Methods 0.000 claims abstract description 38
- 239000007788 liquid Substances 0.000 claims abstract description 36
- 239000002270 dispersing agent Substances 0.000 claims abstract description 33
- 239000003381 stabilizer Substances 0.000 claims abstract description 19
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 9
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 18
- 239000008399 tap water Substances 0.000 claims description 18
- 235000020679 tap water Nutrition 0.000 claims description 18
- 229940101006 anhydrous sodium sulfite Drugs 0.000 claims description 6
- 229940001482 sodium sulfite Drugs 0.000 claims description 6
- 235000010265 sodium sulphite Nutrition 0.000 claims description 6
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 14
- 238000000034 method Methods 0.000 abstract description 8
- 229920001021 polysulfide Polymers 0.000 abstract description 4
- 239000005077 polysulfide Substances 0.000 abstract description 4
- 150000008117 polysulfides Polymers 0.000 abstract description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 2
- 239000003638 chemical reducing agent Substances 0.000 abstract description 2
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 238000000746 purification Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 229910052717 sulfur Inorganic materials 0.000 abstract description 2
- 239000011593 sulfur Substances 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 229910001431 copper ion Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- YFLLTMUVNFGTIW-UHFFFAOYSA-N nickel;sulfanylidenecopper Chemical compound [Ni].[Cu]=S YFLLTMUVNFGTIW-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000005363 electrowinning Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
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- Removal Of Specific Substances (AREA)
- Catalysts (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The present invention relates to chemical industry purification method, particularly the preparation method of a kind of amorphous state nickel sulfide. The present invention has significantly different from conventional vulcanized method for preparing nickel: sodium sulfide adds stabilizer when dissolving, it is prevented that the oxidation of sodium sulfide, guarantees system reducing simultaneously, adds dispersant, it is prevented that form polysulfide between sodium sulfide. After copper, liquid adds reducing agent so that system prepared by nickel sulfide presents reproducibility. Addition the uniform stirring of sodium sulfide is controlled, it is prevented that sulfur source, local is excessive, forms polysulfide, is simultaneously introduced dispersant, reduces the collision probability between nickel sulfide so that it is can keep activity for a long time during preparation. After nickel sulfide prepared by traditional method places 24 hours in atmosphere, copper removal activity is gradually lowered, and places after more than 48 hours, and activity is down to 15% ~ 20%. The amorphous state nickel sulfide of the present invention is placed 7 days in atmosphere, and copper removal activity still can keep 80% ~ 90%.
Description
Technical field
The present invention relates to chemical industry purification method, particularly the preparation method of a kind of amorphous state nickel sulfide.
Background technology
In traditional nickel sulfide preparation process, directly being dissolved by sodium sulfide, after being then added to copper, in liquid, reaction generates nickel sulfide. When sodium sulfide dissolves, owing to solution containing a small amount of dissolved oxygen, can react after running into the sodium sulfide of reproducibility, oxidized portion sodium sulfide, the consumption of sodium sulfide rises, and utilization rate declines; Sodium sulfide reacts generation nickel sulphide solids particle in liquid after joining copper removal, owing to grain graininess is little, surface atom ratio is big, specific surface area is big, surface can be big, is in energy labile state, and nickel sulphide solids particle all trends towards flocking together, the reunion of nickel sulfide occurs, and production efficiency is low.
Summary of the invention
The preparation method that it is an object of the invention to provide a kind of with low cost, amorphous state nickel sulfide that production efficiency is high.
The technical solution adopted for the present invention to solve the technical problems is:
The preparation method of a kind of amorphous state nickel sulfide, specifically comprises the following steps that
A, sodium sulfide dissolve
The tap water that temperature is 5 ~ 25 DEG C is joined in sodium sulfide dissolving tank, add stabilizer, stabilizer and tap water volume ratio are 0.18 ~ 0.25:100, stir 10 ~ 20 minutes, add purity 60% industrial sodium sulfide, dissolve after cure na concn and control at 90 ~ 120g/l, stir 1 ~ 1.5 hour, adding dispersant, dispersant and tap water volume ratio are 0.15 ~ 0.2:100, stir 0.5 ~ 1 hour;
Prepared by b, amorphous state nickel sulfide
Liquid after another extracting container addition copper removal, nickel concentration 75 ~ 85g/l in liquid after copper removal, temperature is 20 ~ 40 DEG C, pH value is 3.2 ~ 3.6, adds anhydrous sodium sulfite, stirs 0.5 ~ 1 hour, after sodium sulfite dissolves, concentration is 0.8 ~ 1g/l, adding dispersant, after dispersant and copper, liquid volume ratio is 0.2 ~ 0.25:100, stirs 15 ~ 30 minutes; The sodium sulfide solution of step a is mixed with above-mentioned solution 1.0 ~ 1.3:1 by volume, stirs and within 0.5 ~ 1 hour, make amorphous state nickel sulfide pulp liquid.
Described step b adds dispersant and stabilizer, its copper removal activity can be kept for a long time.
Described dispersant is the Polyethylene Glycol of purity 99%, stabilizer is the hydrazine hydrate of mass fraction 80%.
The present invention has significantly different from conventional vulcanized method for preparing nickel: sodium sulfide adds stabilizer when dissolving, it is prevented that the oxidation of sodium sulfide, guarantees system reducing simultaneously, adds dispersant, it is prevented that form polysulfide between sodium sulfide. After copper, liquid adds reducing agent so that system prepared by nickel sulfide presents reproducibility. Addition the uniform stirring of sodium sulfide is controlled, it is prevented that sulfur source, local is excessive, forms polysulfide, is simultaneously introduced dispersant, reduces the collision probability between nickel sulfide so that it is can keep activity for a long time during preparation. After nickel sulfide prepared by traditional method places 24 hours in atmosphere, copper removal activity is gradually lowered, and places after more than 48 hours, and activity is down to 15% ~ 20%. The amorphous state nickel sulfide of the present invention is placed 7 days in atmosphere, and copper removal activity still can keep 80% ~ 90%.
Accompanying drawing explanation
Fig. 1 is the process chart of the present invention.
Detailed description of the invention
The preparation method of a kind of amorphous state nickel sulfide, specifically comprises the following steps that
A, sodium sulfide dissolve
The tap water that temperature is 5 ~ 25 DEG C is joined in sodium sulfide dissolving tank, add stabilizer, stabilizer and tap water volume ratio are 0.18 ~ 0.25:100, stir 10 ~ 20 minutes, add purity 60% industrial sodium sulfide, dissolve after cure na concn and control at 90 ~ 120g/l, stir 1 ~ 1.5 hour, adding dispersant, dispersant and tap water volume ratio are 0.15 ~ 0.2:100, stir 0.5 ~ 1 hour;
Prepared by b, amorphous state nickel sulfide
Liquid after another extracting container addition copper removal, nickel concentration 75 ~ 85g/l in liquid after copper removal, temperature is 20 ~ 40 DEG C, pH value is 3.2 ~ 3.6, adds anhydrous sodium sulfite, stirs 0.5 ~ 1 hour, after sodium sulfite dissolves, concentration is 0.8 ~ 1g/l, adding dispersant, after dispersant and copper, liquid volume ratio is 0.2 ~ 0.25:100, stirs 15 ~ 30 minutes; The sodium sulfide solution of step a is mixed with above-mentioned solution 1.0 ~ 1.3:1 by volume, stirs and within 0.5 ~ 1 hour, make amorphous state nickel sulfide pulp liquid.
Described step b adds dispersant and stabilizer, its copper removal activity can be kept for a long time.
Described dispersant is the Polyethylene Glycol of purity 99%, stabilizer is the hydrazine hydrate of mass fraction 80%.
Embodiment 1
The preparation method of a kind of amorphous state nickel sulfide, specifically comprises the following steps that
A, sodium sulfide dissolve
The tap water that temperature is 5 ~ 25 DEG C is joined in sodium sulfide dissolving tank, add stabilizer, stabilizer and tap water volume ratio are 0.18:100, stir 10 ~ 20 minutes, add purity 60% industrial sodium sulfide, dissolve after cure na concn and control at 90g/l, stir 1 ~ 1.5 hour, adding dispersant, dispersant and tap water volume ratio are 0.15:100, stir 0.5 ~ 1 hour;
Prepared by b, amorphous state nickel sulfide
Liquid after another extracting container addition copper removal, nickel concentration 75g/l in liquid after copper removal, temperature is 20 ~ 40 DEG C, pH value is 3.2 ~ 3.6, adds anhydrous sodium sulfite, stirs 0.5 ~ 1 hour, after sodium sulfite dissolves, concentration is 0.8g/l, adding dispersant, after dispersant and copper, liquid volume ratio is 0.2:100, stirs 15 ~ 30 minutes; The sodium sulfide solution of step a is mixed with above-mentioned solution 1.0:1 by volume, stirs and within 0.5 ~ 1 hour, make amorphous state nickel sulfide pulp liquid.
Embodiment 2
The preparation method of a kind of amorphous state nickel sulfide, specifically comprises the following steps that
A, sodium sulfide dissolve
The tap water that temperature is 5 ~ 25 DEG C is joined in sodium sulfide dissolving tank, add stabilizer, stabilizer and tap water volume ratio are 0.25:100, stir 10 ~ 20 minutes, add purity 60% industrial sodium sulfide, dissolve after cure na concn and control at 120g/l, stir 1 ~ 1.5 hour, adding dispersant, dispersant and tap water volume ratio are 0.2:100, stir 0.5 ~ 1 hour;
Prepared by b, amorphous state nickel sulfide
Liquid after another extracting container addition copper removal, nickel concentration 85g/l in liquid after copper removal, temperature is 20 ~ 40 DEG C, pH value is 3.2 ~ 3.6, adds anhydrous sodium sulfite, stirs 0.5 ~ 1 hour, after sodium sulfite dissolves, concentration is 1g/l, adding dispersant, after dispersant and copper, liquid volume ratio is 0.25:100, stirs 15 ~ 30 minutes; The sodium sulfide solution of step a is mixed with above-mentioned solution 1.3:1 by volume, stirs and within 0.5 ~ 1 hour, make amorphous state nickel sulfide pulp liquid.
Embodiment 3
The preparation method of a kind of amorphous state nickel sulfide, specifically comprises the following steps that
A, sodium sulfide dissolve
The tap water that temperature is 5 ~ 25 DEG C is joined in sodium sulfide dissolving tank, add stabilizer, stabilizer and tap water volume ratio are 0.2:100, stir 10 ~ 20 minutes, add purity 60% industrial sodium sulfide, dissolve after cure na concn and control at 100g/l, stir 1 ~ 1.5 hour, adding dispersant, dispersant and tap water volume ratio are 0.16:100, stir 0.5 ~ 1 hour;
Prepared by b, amorphous state nickel sulfide
Liquid after another extracting container addition copper removal, nickel concentration 75 ~ 85g/l in liquid after copper removal, temperature is 20 ~ 40 DEG C, pH value is 3.2 ~ 3.6, adds anhydrous sodium sulfite, stirs 0.5 ~ 1 hour, after sodium sulfite dissolves, concentration is 0.9g/l, adding dispersant, after dispersant and copper, liquid volume ratio is 0.21:100, stirs 15 ~ 30 minutes; The sodium sulfide solution of step a is mixed with above-mentioned solution 1.1:1 by volume, stirs and within 0.5 ~ 1 hour, make amorphous state nickel sulfide pulp liquid.
The amorphous state nickel sulfide embodiment 1 prepared places 7 days, the amorphous state nickel sulfide prepared of embodiment 2 places 14 days, the amorphous state nickel sulfide prepared of embodiment 3 places 20 days, carry out copper-stripping reaction and check its copper removal activity, amorphous state nickel sulfide addition is after ferrum the 0.7% of liquid, after copper removal, liquid is containing copper number all in 0.8 ~ 2.5ppm value range, and amorphous state nickel sulfide copper removal activity keeps better.
Amorphous state nickel sulfide changes over copper removal active testing tables of data 1. As it can be seen from table 1 amorphous state nickel sulfide is after placing 7 days, 14 days and 20 days respectively, carry out copper removal test, hydroful foot nickel electrowinning requirement after copper removal, illustrate that amorphous state nickel sulfide copper removal activity keeps better.
In table, refer to " standing time " the amorphous state nickel sulfide aerial standing time of preparation, " before copper removal liquid cupric " is to place 7 days at amorphous state nickel sulfide, liquid copper content after the ferrum taken at the scene when 14 days and 20 days, " nickel sulfide and copper additional proportion " refers to that amorphous state nickel sulfide adds 0.7% that after volume is ferrum, liquid is long-pending in test amorphous state nickel sulfide activity test process, " after copper removal liquid cupric " refers to that amorphous state nickel sulfide is placed 7 days, after 14 days and 20 days, " before copper removal liquid " is carried out liquid copper content after the copper removal that copper removal obtains, " copper ion removal efficiency " refers to that the copper ion of removing accounts for the total amount of total ion.
Claims (1)
1. the preparation method of an amorphous state nickel sulfide, it is characterised in that specifically comprise the following steps that
A, sodium sulfide dissolve
The tap water that temperature is 5 ~ 25 DEG C is joined in sodium sulfide dissolving tank, add stabilizer, stabilizer and tap water volume ratio are 0.18 ~ 0.25:100, stir 10 ~ 20 minutes, add purity 60% industrial sodium sulfide, dissolve after cure na concn and control at 90 ~ 120g/L, stir 1 ~ 1.5 hour, adding dispersant, dispersant and tap water volume ratio are 0.15 ~ 0.2:100, stir 0.5 ~ 1 hour;
Prepared by b, amorphous state nickel sulfide
Liquid after another extracting container addition copper removal, nickel concentration 75 ~ 85g/L in liquid after copper removal, temperature is 20 ~ 40 DEG C, pH value is 3.2 ~ 3.6, adds anhydrous sodium sulfite, stirs 0.5 ~ 1 hour, after sodium sulfite dissolves, concentration is 0.8 ~ 1g/L, adding dispersant, after dispersant and copper, liquid volume ratio is 0.2 ~ 0.25:100, stirs 15 ~ 30 minutes; The sodium sulfide solution of step a is mixed with above-mentioned solution 1.0 ~ 1.3:1 by volume, stirs and within 0.5 ~ 1 hour, make amorphous state nickel sulfide pulp liquid;
Described dispersant is the Polyethylene Glycol of purity 99%, stabilizer is the hydrazine hydrate of mass fraction 80%.
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| CN201410074075.4A CN103864157B (en) | 2014-02-28 | 2014-02-28 | A kind of preparation method of amorphous state nickel sulfide |
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| CN110156093B (en) * | 2019-05-30 | 2022-03-11 | 重庆交通大学 | Method for efficiently preparing nickel sulfide ultrafine particles under mild condition |
| CN113151863A (en) * | 2021-03-18 | 2021-07-23 | 金川集团股份有限公司 | Method for removing copper ions in nickel production process by electrodeposition |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1459663A (en) * | 2002-05-21 | 2003-12-03 | 中国科学院理化技术研究所 | Nickel sulfide nano particle sensitizing agent and its preparation method |
| CN101186346A (en) * | 2007-12-19 | 2008-05-28 | 扬州大学 | Low-temperature solid-phase synthesizing method for hexagonal-phase nickel sulfide submicron crystal |
| CN102633309A (en) * | 2012-01-13 | 2012-08-15 | 沈阳理工大学 | Hydrothermal preparation method for NiS2 with controllable shape |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3250451B2 (en) * | 1996-03-14 | 2002-01-28 | 大平洋金属株式会社 | Method for removing water from mixed sulfides of nickel and cobalt |
| US20130252798A1 (en) * | 2012-03-21 | 2013-09-26 | National Tsing Hua University | Metallic sulfide photocatalyst for carbon dioxide reduction and the preparation for the same |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1459663A (en) * | 2002-05-21 | 2003-12-03 | 中国科学院理化技术研究所 | Nickel sulfide nano particle sensitizing agent and its preparation method |
| CN101186346A (en) * | 2007-12-19 | 2008-05-28 | 扬州大学 | Low-temperature solid-phase synthesizing method for hexagonal-phase nickel sulfide submicron crystal |
| CN102633309A (en) * | 2012-01-13 | 2012-08-15 | 沈阳理工大学 | Hydrothermal preparation method for NiS2 with controllable shape |
Non-Patent Citations (3)
| Title |
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| "水热微乳液法制备低维硫化镍纳米晶";陈德良等;《高等学校化学学报》;20040831;第25卷(第8期);第1407-1412页 * |
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Effective date of registration: 20240204 Address after: 737100 No. 2 Lanzhou Road, Beijing Road Street, Jinchuan District, Jinchang City, Gansu Province Patentee after: Jinchuan Group Nickel Cobalt Co.,Ltd. Country or region after: China Patentee after: Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences Address before: 737103 No. 98, Jinchuan Road, Jinchang, Gansu Patentee before: JINCHUAN GROUP Co.,Ltd. Country or region before: China Patentee before: Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences |
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