US20090272651A1 - Method for producing high-purity nickel - Google Patents

Method for producing high-purity nickel Download PDF

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Publication number
US20090272651A1
US20090272651A1 US11/658,626 US65862605A US2009272651A1 US 20090272651 A1 US20090272651 A1 US 20090272651A1 US 65862605 A US65862605 A US 65862605A US 2009272651 A1 US2009272651 A1 US 2009272651A1
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solution
high purity
purity nickel
nickel
impurities
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US11/658,626
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English (en)
Inventor
Yongjun Li
Jun Wu
Wengang Zheng
Zhenhua Chen
Zhongqiang Yan
Yongfeng Ma
Shiqing Qi
Wenying Cao
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Jinchuan Group Co Ltd
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Jinchuan Group Co Ltd
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Assigned to JINCHUAN GROUP LTD. reassignment JINCHUAN GROUP LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: CAO, WENYING, CHEN, ZHENHUA, LI, YONGJUN, MA, YONGFENG, QI, SHIQING, WU, JUN, YAN, ZHONGQIANG, ZHENG, WENGANG
Publication of US20090272651A1 publication Critical patent/US20090272651A1/en
Abandoned legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B23/00—Obtaining nickel or cobalt
    • C22B23/06—Refining
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
    • C25C1/06—Electrolytic production, recovery or refining of metals by electrolysis of solutions or iron group metals, refractory metals or manganese
    • C25C1/08—Electrolytic production, recovery or refining of metals by electrolysis of solutions or iron group metals, refractory metals or manganese of nickel or cobalt
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/42—Treatment or purification of solutions, e.g. obtained by leaching by ion-exchange extraction
    • 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

Definitions

  • the present invention relates to a method for producing nickel. More particularly, it relates to a method for producing high purity nickel that includes employing 3N-grade electrolytic nickel to electro-deposited in hydrochloric acid solution system.
  • High-purity metals are used in producing semiconductor and VLSI widely. More than 20 types of high purity metal such as Ga, In, As, Sb, Cd, Sn, Te, Bi, S, Zn, Cu, Se, P and their compounds or alloys are used to produce electronic components and PCB.
  • Nickel is generally used in the conventional stainless steel, alloy and other fields. In recent years, demand of high purity nickel increased in several special fields. For example, a superalloy made of high purity nickel sis applied in aeroengines, protective materials for nuclear reactor, biomaterials and low-expansion alloys; Consumption of high purity nickel gradually increases in electronic industry field. For example, a specific Ni—Fe alloy is applied in lead frame, and a Cu—Ni—Sn alloy is applied in wire port; It requires very low content of impurities such as alkali metals, radioelements, transition metals and gases, when high-purity nickel is applied in LSI and thereof line material, magnetic membrane, and special packing materials.
  • impurities such as alkali metals, radioelements, transition metals and gases
  • WO03/014421A1 discloses a method for producing high purity nickel by employing soluble nickel as an anode and bagging the cathode with membrane, removing impurities through depositing them as hydroxide, preliminary electrolyzing or displacing them by displacement reaction by adding nickel foil to the electrolytic solution, purifying electrolytic solution, then electrolyzing to produce high purity nickel of 5N-grade (99.999%).
  • Main impurities of the produced nickel can be follows: O less then 30 ppm, C, N, S, P and F less than 10 ppm each. (the concentrations of other impurities haven't been disclosed.)
  • JP P2000-219988A (title: method for producing high purity nickel and high purity nickel for forming metallization film) discloses a method for producing high purity nickel by performing electrolysis with a soluble anode, and the anode and cathode are partitioned with two-layer membrane, employing anion exchange resin to eliminate the impurities in electrolytic solution, lower the concentration of hydrochloric acid in the electrolytic solution by diffusion dialysis or evaporation drying, purifying the electrolytic solution and then electrolyzing to obtain the high purity nickel.
  • the high purity nickel produced by this method has fewer impurities.
  • Main impurities of the produced nickel can be follows: alkali metals less than 1 ppm, Fe, Co, Cr less than 10 ppm each, U and Th less than 1 ppb each, C less than 50 ppm, and O less than 100 ppm.
  • the object of the present invention is to provide a method for producing high purity nickel to settle effectively high concentration of acid in the electric dissolving stock solution cut down on production cost, dispel pollution, and depurate solution, and prevent the anolyte and catolyte from mixing each other.
  • An object of the present invention is to provide a method for producing high purity nickel. The said method involves the following steps:
  • electrolyzing in hydrochloric acid system are electrolyse to prepare NiCl 2 solution at the current density of about 100 A/m 2 to 200 A/m 2 ; and at the end of electrolysis when the concentration of H + is about 1 g/l to 2 g/l, electrolyzing at the current density of about 30 A/m 2 to 70 A/m 2 to a pH of the solution of about 1 to 3;
  • Main impurities of the prepared solution can be follows: Co and Fe less than 0.001 g/l each, and Cu, Pb and Zn less than 0.0002 g/l each; and
  • a method according to the present invention for producing high purity nickel characterized in that the said electrolytic solution is extracted by 3-stage countercurrent extraction at the extractant phase ratio of 1:2, and back-extract with pure water 10 mins after achieving extraction equilibrium.
  • a method for producing high purity nickel according to the present invention characterized in that anion extractant contains 20 vol. % to 40 vol. % tertiary amine, 20 vol. % to 45 vol. % butylate, and sulphonated kerosene.
  • a method for producing high purity nickel according to the present invention characterized in that it is performed before extracting NiCl2 solution that purifying the organic phase of the anion extractant by washing and sequentially saturating the said organic phase with 4N high purity hydrochloric acid.
  • a method for producing high purity nickel according to the present invention characterized in that a hollow fiber ball is employed to degrease the said solution.
  • a method for producing high purity nickel according to the present invention which employs combined anion exchange resin to form a three dimensional structure to further purify the solution.
  • a method according to the present invention electro-deposit employs high purity solution purified with ion exchange resin to produce high purity nickel of 5N-grade purity and determined by glow discharge mass spectrometry (GDMS) 5N-grade.
  • GDMS glow discharge mass spectrometry
  • reducing the content of acid in the solution by electrolyzing at a low current density at the end of electrolysis procedure overcome the high concentration of acid in the electrolytic solution, removed acid by boil or neutralization, And it cut down the cost and prevent pollution.
  • It employs high purity hydrochloric acid to saturate the purified organic phase, and then extract the high concentration of NiCl 2 solution with the said organic phase to remove Co in order to purify the solution.
  • It also employs combined anion exchange resin forming a three dimensional structure to further purify the solution.
  • Detected impurities in the high purity nickel according to the present invention include 16 impurities as Co, Fe, Cu, Zn, As, Cd, Sn, Sb, Pb, Bi, Al, Mn, Mg, Si, P, and S. Concentration of each impurity element is less than 1 ppm and the concentration of the main element nickel is more than 99.999%.
  • Preparation high purity NiCl 2 solution is the basement of producing high purity nickel. Five impracticable elements, Fe, Co, Cu, Pb and Zn, which have been chosen from 16 impurities, are detected as the main impurities. According to the result estimates the purity of the solution. The experiment shows that choosing the typical impurities as the main objects to remove can improve the determining efficiency.
  • FIG. 1 shows the process flow diagram of the method according to the present invention.
  • a method for producing high purity nickel involves the sequential steps of:
  • the contents of impurities element in prepared NiCl 2 solution by electrolysis are as follows: 0.006 g/l to 0.009 g/l Co, 0.002 g/l Cu, 0.002 g/l Fe, 0.001 g/l Pb, and 0.002 g/l Zn.
  • the said electrolytic solution is extracted by 3-stage countercurrent extraction with anion extractant which contains 20 vol. % to 40 vol. % tertiary amine, 20 vol. % to 45 vol. % butylate, and sulphonated kerosene, at the extractant phase ratio of 1:2, back-extracted with pure water 10 minutes after achieving extraction equilibrium. Since the concentration of Cl ⁇ is increased, the impurities of Fe, Co, Cu, Pb and Zn form complexes anion sufficiently. Fewer impurities exist in the solution after purifying by extracting with anion exctractant, and the main impurities can be follows: Cu and Zn less than 0.0003 g/l each, and Co less than 0.001 g/l.
  • the extracted solution is degreased through the activated carbon column, and further purified the said solution through anion exchange resin 331, 717, D301 and D401 mixed ion-exchange resin sequentially at the exchange follow rate no more than 2 BV/h.
  • the purified solution contains Co and Fe are both less than 0.001 g/l, Cu, Pb and Zn are all less than 0.0002 g/. Since the design principle of ion exchange system is to ensure that no impurities from the system pollute the solution, the pure materials is used to make ion exchange column main body as well as system.
  • the antipollution metering pump is used to transport and control the follow of ion exchange solution quantitatively, and the specific anion exchange resin is used to further purify.
  • Extracting residue is degreased, adjusted acidity, purified by ion exchange resin at the flow rate of about 1 BV/h to 2 BV/h. Impurities could not be removed efficiently at the too fast flow, and on the contrary, it will deduce the economic efficiency at the too slow flow.
  • the impurities such as Pb, Zn, Cu, Fe, and Co in the solution are reduced after ion exchange and the solution contains 0.006 g/l to 0.009 g/l Co, 0.002 g/l Cu, 0.00 g/l Pb, and 0.002 g/l Zn.
  • the solution purified by ion exchange resin is electro-deposited in electrolytic cell at a pH of about 1 to 3, a current density of about 100 A/m 2 to 200 A/m 2 and a temperature of 40 to 60°, draw out the electro-deposited solution simultaneously to keep a constant circulating to obtain high purity nickel, which is analyzed by glow discharge mass spectrometry (GDMS) to achieves 5N-grade purity high purity nickel.
  • GDMS glow discharge mass spectrometry
  • the electrolytic cell is airproofed and has a dustproof head cover which is connect with the cell with water seal. Cathode plate and anode plate assembled with conductive rods are hung on the head cover. Electrode plates and conductive rods are made of pure anticorrosive material to prevent acid corrosion and pollution in solution. Circuit junctions are fastened with screws and high precision silicon rectifier power is employed in order to keep constant electrobath voltage and current and eliminate junction resistance.
  • 3N-grade electrolytic nickel was electrolyzed in hydrochloric acid system to prepare NiCl 2 solution at a current density of 100 A/m 2 .
  • the concentration of H + was 1 g/l
  • the current density was changed to 30 A/m 2 and electrolyzed till the pH of the solution to 3, wherein the concentration of Cl ⁇ was 6 mol/L and the impurities were shown in the table 1.
  • Anion extractant contained 25 vol. % tertiary amine, 45 vol. % butylate, and 30 vol. % sulphonated kerosene was washed by high purity water, saturated with 4 mol/l high purity hydrochloric acid.
  • the concentration of Co was decreased from 0.009 g/l to 0.001 g/l.
  • the back-extracted solution was degreased through activated carbon column, further purified through ion exchange column mixed ion exchange resin from anion exchange resin 331, 717, D301 and D401 at the exchange follow rate of 2 BV/h. Ingredients in solution further purified by ion change were shown in table 3.
  • Eletrowinning conditions current density was 100 A/m 2 , pH of NiCl 2 solution was 3, Eletrowinning temperature was 50°.
  • An insoluble anode was employed to electro-deposit the solution further purified by ion exchange to produce 5N-grade high purity nickel.
  • Main impurities of the produced high purity nickel were as follows: alkali metals less than 0.1 ppm, Fe, Co and Cr less than 1 ppm each, U and Th less than 0.1 ppb each, C less than 60 ppm, and O less than 100 ppm. Contents of some impurities in high purity nickel were shown in table 4.
  • 3N-grade electrolytic nickel was electrolyzed in hydrochloric acid system to prepare NiCl 2 solution at a current density of 150 A/m 2 .
  • the concentration of H + was 1.5 g/l
  • the current density was changed to 50 A/m 2 and electrolyzed till the pH of the solution to 3, wherein the concentration of Cl ⁇ was 6 mol/L and the impurities were shown in the table 5.
  • Anion extractant contained 40 vol. % tertiary amine, 20 vol. % butylate, and 40 vol. % sulphonated kerosene was washed by high purity water, saturated with 4 mol/l high purity hydrochloric acid.
  • the concentration of Co was decreased from 0.008 g/l to 0.001 g/l.
  • the back-extracted solution was degreased through activated carbon column, further purified through ion exchange column mixed ion exchange resin from anion exchange resin 331, 717, D301 and D401 at the exchange follow rate of 1.5 BV/h. Ingredients in solution further purified by ion change were shown in table 7.
  • An insoluble anode was employed to electro-deposit NiCl 2 solution. Eletrowinning conditions were as follows: current density was 100 A/m 2 , pH of NiCl 2 solution was 3, Eletrowinning temperature was 50°. An insoluble anode was employed to electro-deposit in the solution further purified by ion exchange to produce 5N-grade high purity nickel. Main impurities of the produced high purity nickel were as follows: alkali metals less than 0.1 ppm, Fe, Co, and Cr less than 1 ppm each, U and Th less than 0.1 ppb each, C less than 60 ppm, and O less than 100 ppm. Contents of some impurities in high purity nickel were shown in table 7.
  • An insoluble anode was employed to electro-deposit in NiCI 2 solution. Electro-deposition conditions were as follows: current density was 200 Am 2 , pH of NiCl 2 solution was 2. Electro-deposition temperature was 60°. An insoluble anode was employed to electro-deposit the solution further purified by ion exchange to produce 5N-grade high purity nickel. Main impurities of the produced high purity nickel were as follows: alkali metals less than 0.1 ppm, Fe, Co and Cr less than 1 ppm each, U and Th less than 0.1 ppb each, C less than 60 ppm, and O less than 100 ppm. Contents of main impurities in high purity nickel were shown in table 9.
  • 3N-grade electrolytic nickel was electrolyzed in hydrochloric acid system to prepare NiCl 2 solution at a current density of 200 A/m 2 .
  • the concentration of H + was 2 g/l
  • the current density was changed to 70 A/m 2 and electrolyzed till the pH of the solution to 1, wherein the concentration of Cl ⁇ was 6 mol/L and the impurities were shown in the table 10.
  • An insoluble anode was employed to electro-deposit in the high purity NiCl 2 solution. Electro-deposition conditions were as follows: current density was 160 A/m 2 , pH of NiCl 2 solution was 1, Electro-deposition temperature was 50°. An insoluble anode was employed to electro-deposit in the solution and further was purified by ion exchange to produce 5N-grade high purity nickel. Main impurities of the produced high purity nickel were as follows: alkali metals less than 0.1 ppm, Fe, Co and Cr less than 1 ppm each, U and Th less than 0.1 ppb each, C less than 60 ppm, and O less than 100 ppm. Contents of main impurities in high purity nickel were shown in table 12.

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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Electrolytic Production Of Metals (AREA)
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US11/658,626 2004-07-28 2005-04-13 Method for producing high-purity nickel Abandoned US20090272651A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
CN200410070648.2 2004-07-28
CNB2004100706482A CN1276129C (zh) 2004-07-28 2004-07-28 一种制备高纯镍的方法
PCT/CN2005/000488 WO2006010305A1 (fr) 2004-07-28 2005-04-13 Procede d'obtention d'un nickel de grande purete

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JP (1) JP4659829B2 (fr)
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CN113061938A (zh) * 2021-03-09 2021-07-02 金川集团股份有限公司 一种生产高品质镍扣的方法
CN115573003A (zh) * 2022-10-12 2023-01-06 金川集团股份有限公司 一种6n超纯镍的制备方法

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CN102268691B (zh) * 2011-08-04 2012-12-05 苏州晶纯新材料有限公司 一种高纯镍的生产方法
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CN105441974B (zh) * 2015-11-20 2017-12-01 金川集团股份有限公司 一种生产电积镍的方法
CN106283108B (zh) * 2016-08-31 2018-04-03 中南大学 一种用离子交换树脂从镍电解阳极液中深度除铜的方法
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CN110129572B (zh) * 2019-06-18 2021-01-05 中国科学院兰州化学物理研究所 一种利用废旧镍基高温合金制备高纯铼酸铵的方法
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113061938A (zh) * 2021-03-09 2021-07-02 金川集团股份有限公司 一种生产高品质镍扣的方法
CN115573003A (zh) * 2022-10-12 2023-01-06 金川集团股份有限公司 一种6n超纯镍的制备方法

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JP4659829B2 (ja) 2011-03-30
CN1587441A (zh) 2005-03-02
JP2008507628A (ja) 2008-03-13
WO2006010305A1 (fr) 2006-02-02

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