CN101709489B - Method for producing nickel powder from pure nickel sulfate solution through direct deposition - Google Patents
Method for producing nickel powder from pure nickel sulfate solution through direct deposition Download PDFInfo
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- CN101709489B CN101709489B CN2009103096062A CN200910309606A CN101709489B CN 101709489 B CN101709489 B CN 101709489B CN 2009103096062 A CN2009103096062 A CN 2009103096062A CN 200910309606 A CN200910309606 A CN 200910309606A CN 101709489 B CN101709489 B CN 101709489B
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Abstract
The invention provides a method for producing nickel powder from pure nickel sulfate solution through direct deposition. The method comprises the following steps: adjusting the pH value of the pure nickel sulfate solution at a concentration more than 8g/L to between 2.0 and 7.2; and taking a Pb-Ag-Ca lead base alloy as an anode and a stainless steel plate as a cathode, performing electrolysis to deposit the nickel powder on the negative plate, wherein in the electrolysis, the current density is between 1,000 and 4,000A/M2, and the temperature of electrolyte solution is between 20 and 60DEG C. The granularity of the electrolytic nickel powder prepared by the method is less than 200 meshes, and the oxygen content is lower than 0.35 percent. The method has the advantages of simple process, short process flow, low production cost, energy efficiency and environmental protection, is suitable for directly preparing the electrolytic nickel powder from the pure nickel sulfate solution, is also suitable for directly preparing the electrolytic nickel powder from nickel solution recovered from nickel waste and purified, has realistic significance of recycling materials and protecting the environment, and is particularly suitable for environment-friendly enterprises in which the nickel-containing waste is subjected to various links of impurity removal to obtain nickel-containing solution.
Description
Technical field
The invention discloses a kind of production method of nickel powder, be meant a kind of method especially with producing nickel powder from pure nickel sulfate solution through direct deposition.
Background technology
Nickel powder is a kind of important starting material, is mainly used in nuclear industry, Edison battery, electrical alloy, superalloy, catalyzer and additive for powder metallurgy etc.; Be field important raw and processed materials such as metallurgy, chemical industry, material, light industry, electronics, national defence, nuclear technique, aerospace.
The production method of nickel powder mainly contains electrolytic process, atomization, chemical method.Atomization is to blow out nickel powder again after nickel or the nickelalloy fusing, and the nickel powder pattern that this method is produced is irregular spherical.Easily oxidation in the winding-up process, powder particle is thicker comparatively speaking, and advantage is can the production nickel alloy powder.
The nickel powder of chemical method production is also referred to as reduced nickel powder, and it generally is to adopt oxalic acid, yellow soda ash, carbon ammonium, bicarbonate of ammonia etc. for precipitation agent, is the Ni in the aqueous solution
2+Be precipitated as the carbonate or the oxalate of nickel, calcining reduction is a nickel powder again; Can make the nickel powder of median particle diameter less than 10um, the advantage of this method is the nickel powder fine size purity height of producing; But, environment there is certain pollution owing to adopt chemical raw material production; Particularly adopt oxalic acid as precipitation agent,, cause the nickel powder cost height of being produced because oxalic acid costs an arm and a leg.
Electrolytic process is to adopt sheet nickel as anode, and stainless steel plate is made negative electrode, is containing Ni
2+Water solution system carry out electrolysis, on negative electrode, obtain electrolytic nickel powder.And can reach the GB5247-85 standard.Sheet nickel generally is to obtain high ice nickel with containing nickel ore concentrate through pyrometallurgical smelting, obtains sheet nickel by height ice nickel through electrolysis again, and electrolytic technical qualification are (g/L) Ni60～75; Cu≤0.0003; Fe≤0.004; Co≤0.015; Zn≤0.0003; Pb≤0.0003; Na≤40～50; PH value 2～5; Current density 180～260A/m2; Electrolyte temperature is 60～70 ℃; Homopolarity width between centers 180～200mm; The anode and cathode liquid level differs from 30～50mm.The advantage of the nickel powder that this method is produced is the product purity height, and the nickel powder pattern is dendroid, and specific surface area is big, and suppression performance is good.But this method must be made anode with pure sheet nickel, uses additive, can carry out electrolysis, therefore, complex process, the cost height, and power consumption is big.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art and provide that a kind of processing method is simple, technical process is short, production cost is low, eco-friendly method with producing nickel powder from pure nickel sulfate solution through direct deposition.
The present invention--a kind of method with producing nickel powder from pure nickel sulfate solution through direct deposition comprises the steps:
The first step: electrolytic solution is prepared
Getting concentration is the nickel sulfate solution 20L of 8g/L, contains Cu 0.0003g/L, Fe0.0005g/L, As 0.0001g/L, Sb 0.0001g/L, Bi 0.00035g/L, Zn0.0003g/L, Pb 0.00065g/L, H in the solution
2SO
45～7g/L adds NaOH 10～15 grams, the pH value of solution is adjusted to 2.0 after, in the electrolyzer of packing into, this groove is equipped with turnover conduit, the thermometer of electrolytic solution, and is stand-by;
Second step: electrolysis
Pb-Ag-Ca alloy with argentiferous 0.8% is made anode, and stainless steel plate is made negative electrode, and current density is 1000A/M
2, electrolyte temperature is: 20～30 ℃, the internal circulating load of electrolytic solution is 0.5～1L/ minute, carries out electrolysis, electrolysis time 1.0 hours;
The 3rd step: scrape powder
Gap periods by 30min/ time is scraped powder;
The 4th step: solid-liquid separation, washing
After electrolysis was finished, normal pressure or filtration under diminished pressure obtained electrolytic nickel powder, with the described electrolytic nickel powder of flushing with clean water, used BaCl
2Check is to there not being BaSO
4When white precipitate generates, stop flushing, will be through the electrolytic nickel powder filtration of flushing with clean water, obtain water content less than 8% electrolytic nickel powder;
The 5th step: vacuum-drying
It is the environment of 0～0.1 MPa that the 4th electrolytic nickel powder that obtain of step is placed vacuum tightness, is heated to 80～120 ℃, and vacuum-drying is to constant weight.
Among the present invention, the granularity of described electrolytic nickel powder is less than 200 orders; The oxygen level of described electrolytic nickel powder is lower than 0.34%.
The present invention is owing to adopt above-mentioned processing method, on the one hand, the insoluble anode that employing is made by the Pb-Ag-Ca alloy, bright sulfur acid nickel solution is carried out direct electrolysis, obtain nickel powder, overcome in the prior art the essential pure nickel plate that adopts of electrolysis production nickel powder as the anodic drawback, omitted the production process of electrolysis pure nickel plate, effectively reduce the production cost of electrolytic nickel powder, have and simplify working process, the advantage of energy efficiency; On the other hand, adopt bigger current density, lower electrolyte temperature during electrolysis of the present invention, have the advantage of product fine size; Again on the one hand, the electrolytic nickel powder that adopts processing method of the present invention to produce, granularity reaches 200～300 orders; Oxygen level is lower than 0.35%; Particularly adopt processing method of the present invention, can will contain Ni
2+Solution, as high nickel matte leach liquor, electrolysis waste solution, the galvanized waste material of nickel etc., adopt a series of wet separation to purify means, nickel solution is purified, then, directly electrolysis makes nickel powder, be a large amount of nickeliferous waste liquids and the nickel waste recovery purification enterprise that chemical field produces, a kind of treatment process simple, that easily go is provided.
In sum, processing method of the present invention is simple, technical process is short, production cost is low, energy efficiency, environmental friendliness, both be adapted to adopt bright sulfur acid nickel solution directly to prepare electrolytic nickel powder, the nickel solution that is adapted to the purification of nickel waste recovery again directly prepares electrolytic nickel powder, has the material recycle, eco-friendly realistic meaning; Be adapted to the use of the enviromental protection enterprise of the solution containing nickel that nickle contained discarded material obtains through the removal of impurities of each link especially.
Embodiment
Embodiment 1:
Getting concentration is the nickel sulfate solution 20L of 8g/L, contains Cu 0.0003g/L, Fe0.0005g/L, As 0.0001g/L, Sb 0.0001g/L, Bi 0.00035g/L, Zn0.0003g/L, Pb 0.00065g/L, H in the solution
2SO
45～7g/L adds NaOH 10～15 grams, the pH value of solution is adjusted to 2.0 after, in the electrolyzer of packing into, this groove is equipped with turnover conduit, the thermometer of electrolytic solution; It is stainless steel plate that anode adopts Pb-Ag-Ca alloy, the negative electrode of argentiferous 0.8%.Solution temperature is adjusted to 20～30 ℃; Current density 1000A/M
2, circulation of elecrolyte speed 0.5～1L/min, electrolysis time 1.0 hours is scraped powder by 30min/ time gap periods; After electrolysis was finished, normal pressure or filtration under diminished pressure obtained electrolytic nickel powder, with the described electrolytic nickel powder of flushing with clean water, used BaCl
2Check is to there not being BaSO
4When white precipitate generates, stop flushing, will be through the electrolytic nickel powder filtration of flushing with clean water, obtain water content less than 8% electrolytic nickel powder.It is the vacuum of 0～0.1 MPa that described electrolytic nickel powder is placed vacuum tightness, is heated to 80～120 ℃, is dried to constant weight; Obtain electrolytic nickel powder, be dark gray powder, chemical ingredients is a pure nickel powder, and the granularity of product is less than 200 orders, and the pattern of product is irregular dendroid.The oxygen level measurement result is less than 0.34%.
Embodiment 2:
Getting concentration is the nickel sulfate solution 20L of 25g/L, contain Cu 0.0006g/L, Fe 0.0003g/L, Pb 0.00028g/L, Zn 0.0002g/L, As 0.0002g/L, Sb 0.0003g/L, Bi 0.0005g/L in the solution, add NaOH 25～35 grams, after the pH value of solution is adjusted to 4.0, pack in the electrolyzer, this groove is equipped with turnover conduit, the thermometer of electrolytic solution; It is stainless steel plate that anode adopts Pb-Ag-Ca alloy, the negative electrode of argentiferous 1.2%.Solution temperature is adjusted to 35～45 ℃; Current density 2500A/m
2, circulation of elecrolyte speed 2～3L/min, electrolysis time 1.0 hours is scraped powder by 30min/ time gap periods; After electrolysis was finished, normal pressure or filtration under diminished pressure obtained electrolytic nickel powder, with the described electrolytic nickel powder of flushing with clean water, used BaCl
2Check is to there not being BaSO
4When white precipitate generated, stopping to wash will be through the electrolytic nickel powder filtration of flushing with clean water, obtained water content less than 8% electrolytic nickel powder.It is the vacuum of 0～0.1 MPa that described electrolytic nickel powder is placed vacuum tightness, is heated to 80～120 ℃, is dried to constant weight; Obtain electrolytic nickel powder, be dark gray powder, chemical ingredients is a pure nickel powder, and the granularity of product is less than 250 orders, and the pattern of product is irregular dendroid.The oxygen level measurement result is less than 0.33%.
Embodiment 3
Getting concentration is the nickel sulfate solution 20L of 50g/L, contains Cu 0.0006g/L, Fe 0.0003g/L, Pb 0.00028g/L, Zn 0.0002g/L, As 0.0002g/L, Sb 0.0003g/L, Bi 0.0005g/L in the solution, adds NaOH and Na
2CO
3Mixture 40～50 gram, the pH value of solution is adjusted to 7.2 after, in the electrolyzer of packing into, this groove is equipped with turnover conduit, the thermometer of electrolytic solution; It is stainless steel plate that anode adopts Pb-Ag-Ca alloy, the negative electrode of argentiferous 1.5%.Solution temperature is adjusted to 35～45 ℃; Current density 4000A/m
2, circulation of elecrolyte speed 4～5L/min, electrolysis time 1.0 hours is scraped powder by 30min/ time gap periods; After electrolysis was finished, normal pressure or filtration under diminished pressure obtained electrolytic nickel powder, with the described electrolytic nickel powder of flushing with clean water, used BaCl
2Check is to there not being BaSO
4When white precipitate generated, stopping to wash will be through the electrolytic nickel powder filtration of flushing with clean water, obtained water content less than 8% electrolytic nickel powder.It is the vacuum of 0～0.1 MPa that described electrolytic nickel powder is placed vacuum tightness, is heated to 80～120 ℃, is dried to constant weight; Obtain electrolytic nickel powder, be dark gray powder, chemical ingredients is a pure nickel powder, and the granularity of product is less than 300 orders, and the pattern of product is irregular dendroid, and the oxygen level measurement result is less than 0.32%.
Claims (2)
1. the method with producing nickel powder from pure nickel sulfate solution through direct deposition comprises the steps:
The first step: electrolytic solution is prepared
Getting concentration is the nickel sulfate solution 20L of 8g/L, contains Cu 0.0003g/L, Fe0.0005g/L, As 0.0001g/L, Sb 0.0001g/L, Bi 0.00035g/L, Zn0.0003g/L, Pb 0.00065g/L, H in the solution
2SO
45～7g/L adds NaOH 10～15 grams, the pH value of solution is adjusted to 2.0 after, in the electrolyzer of packing into, this groove is equipped with turnover conduit, the thermometer of electrolytic solution, and is stand-by;
Second step: electrolysis
Pb-Ag-Ca alloy with argentiferous 0.8% is made anode, and stainless steel plate is made negative electrode, and current density is 1000A/M
2, electrolyte temperature is: 20～30 ℃, the internal circulating load of electrolytic solution is 0.5～1L/ minute, carries out electrolysis, electrolysis time 1.0 hours;
The 3rd step: scrape powder
Gap periods by 30min/ time is scraped powder;
The 4th step: solid-liquid separation, washing
After electrolysis was finished, normal pressure or filtration under diminished pressure obtained electrolytic nickel powder, with the described electrolytic nickel powder of flushing with clean water, used BaCl
2Check is to there not being BaSO
4When white precipitate generates, stop flushing, will be through the electrolytic nickel powder filtration of flushing with clean water, obtain water content less than 8% electrolytic nickel powder;
The 5th step: vacuum-drying
It is the environment of 0～0.1 MPa that the 4th electrolytic nickel powder that obtain of step is placed vacuum tightness, is heated to 80～120 ℃, and vacuum-drying is to constant weight.
2. a kind of method according to claim 1 with producing nickel powder from pure nickel sulfate solution through direct deposition, it is characterized in that: the granularity of described electrolytic nickel powder is less than 200 orders; The oxygen level of described electrolytic nickel powder is lower than 0.34%.
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| CN2009103096062A CN101709489B (en) | 2009-11-12 | 2009-11-12 | Method for producing nickel powder from pure nickel sulfate solution through direct deposition |
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| CN101709489B true CN101709489B (en) | 2011-03-23 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101962787B (en) * | 2010-11-08 | 2011-12-07 | 重庆市机电设计研究院 | Automatic powder-scraping device |
| CN102628172B (en) * | 2012-04-24 | 2015-07-22 | 天华化工机械及自动化研究设计院有限公司 | Device for scraping sponge copper |
| CN114411205B (en) * | 2022-01-21 | 2023-10-27 | 中国人民解放军陆军勤务学院 | Preparation method of graphene-loaded nickel particle composite powder |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1257120A1 (en) * | 1985-04-15 | 1986-09-15 | Уральский политехнический институт им.С.М.Кирова | Method of production of nickel powder by electrolysis from aqueous solution of sulfate-chloride electrolyte |
| CN1827266A (en) * | 2006-04-10 | 2006-09-06 | 李小毛 | Process for preparing nano nickel powder |
| CN101265589A (en) * | 2007-03-12 | 2008-09-17 | 张建玲 | Method for producing electrolytic nickel using various nickel-containing raw material |
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2009
- 2009-11-12 CN CN2009103096062A patent/CN101709489B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1257120A1 (en) * | 1985-04-15 | 1986-09-15 | Уральский политехнический институт им.С.М.Кирова | Method of production of nickel powder by electrolysis from aqueous solution of sulfate-chloride electrolyte |
| CN1827266A (en) * | 2006-04-10 | 2006-09-06 | 李小毛 | Process for preparing nano nickel powder |
| CN101265589A (en) * | 2007-03-12 | 2008-09-17 | 张建玲 | Method for producing electrolytic nickel using various nickel-containing raw material |
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Assignee: Changzhou KTK-Bofan Energy New Material Co., Ltd. Assignor: Central South University Contract record no.: 2011320000875 Denomination of invention: Method for producing nickel powder from pure nickel sulfate solution through direct deposition Granted publication date: 20110323 License type: Exclusive License Open date: 20100519 Record date: 20110622 |
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