CN113061938A - Method for producing high-quality nickel button - Google Patents

Method for producing high-quality nickel button Download PDF

Info

Publication number
CN113061938A
CN113061938A CN202110255727.4A CN202110255727A CN113061938A CN 113061938 A CN113061938 A CN 113061938A CN 202110255727 A CN202110255727 A CN 202110255727A CN 113061938 A CN113061938 A CN 113061938A
Authority
CN
China
Prior art keywords
nickel
button
electrolysis
quality
nickel button
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202110255727.4A
Other languages
Chinese (zh)
Inventor
李化平
张四增
周通
陈涛
张峰瑞
苏兰伍
张本军
卢建波
宛顺磊
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jinchuan Group Nickel Cobalt Co ltd
Original Assignee
Jinchuan Group Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Jinchuan Group Co Ltd filed Critical Jinchuan Group Co Ltd
Priority to CN202110255727.4A priority Critical patent/CN113061938A/en
Publication of CN113061938A publication Critical patent/CN113061938A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25CPROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C1/00Electrolytic production, recovery or refining of metals by electrolysis of solutions
    • C25C1/06Electrolytic production, recovery or refining of metals by electrolysis of solutions or iron group metals, refractory metals or manganese
    • C25C1/08Electrolytic production, recovery or refining of metals by electrolysis of solutions or iron group metals, refractory metals or manganese of nickel or cobalt

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electrolytic Production Of Metals (AREA)

Abstract

The invention discloses a method for producing a high-quality nickel button, which is characterized in that a sulfate-chloride mixed system is taken as electrolyte, Ni9950 electrolytic nickel is cut into small nickel pieces, the small nickel pieces are put into a titanium basket to serve as an anode, a surface-treated composite metal film-coated nickel button plate serves as a cathode, and a high-quality nickel button product is produced through electrolysis. The main grade of nickel and cobalt of the nickel button produced by the method reaches more than 99.98 percent, and impurity elements all meet the requirement of a Ni9997 standard; the nickel button is easy to peel off, has smooth appearance and is free from defects. The electrolyte does not need to be purified and purified, and is simple to operate; relatively low-value Ni9950 is converted into high-value-added Ni9997 high-quality nickel button products, and considerable economic benefits are generated; the electrolytic process has low cell voltage and reduces the electric energy consumption. The invention has good economic benefit and popularization and application prospect.

Description

Method for producing high-quality nickel button
Technical Field
The invention relates to a method for producing a high-quality nickel button, belonging to the technical field of hydrometallurgy and electrochemistry.
Background
The electrolytic nickel button as nickel plating material has the advantages of smooth surface, high basket filling smoothness, high density, good electric contact performance, uniform current distribution, uniform reduction in dissolution, no suspension bridging accident and the like. Thus, nickel buttons are increasingly used in the electroplating industry. At present, the nickel buttons used in China mainly depend on imports, and main manufacturers are fresh water valley companies and Norwegian eagle bridge refineries. The electrolytic process that a nickel sulfide soluble anode and a cathode are sleeved with a diaphragm bag is adopted by freshwater valley company to produce the nickel button, the voltage of a tank is 4.0-5.5V, and the cathode plate is sprayed with thermosetting epoxy paint. A process for producing a nickel button by adopting chlorinated medium insoluble anode electrolysis in Norwegian eagle bridge refineries is characterized in that a titanium plate is used as a substrate of a cathode plate, a titanium cylinder is embedded according to specifications, and the surface of the cathode plate is formed by injection molding of epoxy resin; the cell voltage is 3.6-3.8V. The method is characterized in that in a sulfate and hydrochloride mixed system, a nickel sulfide anode plate is taken as a soluble anode, a stainless steel plate is embedded with a stainless steel column as a template, the surface of the stainless steel plate is lined with an insulating material PE and then taken as an electrolytic cathode plate, and new purified liquid is taken as catholyte to carry out diaphragm electrolysis to produce a nickel button product.
The existing production process mainly has the defects of low main grade and high impurity content of the produced nickel buttons; the cell voltage is high and the power consumption is high; the produced nickel button has large internal stress, so that the product has irregular and unattractive appearance; when the nickel button produced by the prior art is used as an electroplating anode, the nickel button is dissolved in a depth direction electrochemical mode, and finally, the shell is left to be insoluble, so that more residues are generated in the use process, and the nickel button is particularly not suitable for a high-end nickel electroplating process. In addition, the production is carried out by adopting a chlorination medium, because the temperature in the production process is higher, chloride ions are volatile, the corrosion to production equipment and auxiliary equipment is larger, and the production environment is poor.
Disclosure of Invention
The invention aims to solve the problems in the existing nickel button production process, improve the nickel button quality, reduce the electric energy consumption and improve the added value of products, and provides a method for producing high-quality nickel buttons, which can produce high-quality nickel button products with high purity, compact crystallization and good electrochemical dissolution activity and can greatly reduce the electric energy consumption in the nickel button production.
The technical scheme of the invention is realized by the following technical scheme:
a method for producing high-quality nickel buttons is completed by the following electrolytic equipment and method:
an electrolysis device: including the electrolysis trough, alternate arrangement multiunit is used for assembling anodal positive pole titanium basket and the negative plate that is used for growing nickel and detains in the electrolysis trough, electrolysis trough upper portion is equipped with positive pole conducting rod and negative pole conducting rod, positive pole conducting rod and negative pole conducting rod are connected respectively to positive pole titanium basket and negative plate, positive pole conducting rod and negative pole conducting rod are connected with DC power supply just, the negative pole respectively, electrolysis trough one side is equipped with the drain pipe, the electrolysis trough top is equipped with a plurality of feed liquor branch pipes and a feed liquor house steward, the storage tank is connected to the drain pipe, the storage tank connects second pipeline and third pipeline respectively through first pipeline, the feed liquor branch pipe is connected to the second pipeline, the third pipeline passes through the filter and connects feed liquor house steward.
The electrolysis method comprises the following steps: the method is characterized in that a sulfate-chloride mixed system is used as electrolyte, Ni9950 is electrolyzed and cut into small nickel blocks (40-60 multiplied by 40-60 mm), the small nickel blocks are placed into a titanium basket to serve as an anode, a surface-treated composite metal film-coated nickel button plate serves as a cathode, and a high-quality nickel button product is produced through electrolysis.
In the electrolysis equipment, the outer sleeve of the anode titanium basket is provided with 747#The filter bag has the function of preventing the broken slag dissolved by the anode from falling into the dissolving solution and being adsorbed to the surface of the cathode plate to influence the quality of the nickel button.
Among the electrolysis equipment, be equipped with first control flap, pump and second control flap on the first pipeline in proper order, be equipped with third control flap on the second pipeline, be equipped with fourth control flap on the third pipeline, be equipped with fifth control flap on the feed liquor house steward.
In the electrolysis method, the Ni9950 means that the appearance quality of the electrolytic nickel does not meet the Ni9997 (the main grade Ni + Co is more than or equal to 99.50 percent) standard, and the chemical components can reach the Ni9997 (the main grade Ni + Co is more than or equal to 99.97 percent) standard. The Ni9950 has higher main grade component and low impurity content. Because other impurities are not introduced into the electrolyte, the electrolyte does not need to be purified and purified, the electrolyte flowing out of the electrolytic cell is only returned to the electrolytic cell by a pump, and the electrolyte circularly flows and mainly plays a role in stirring. The electrolyte flows in a closed cycle, and as the current efficiency of the cathode and the anode is basically equal, nickel does not need to be supplemented in the electrolytic process, and only new water accounting for 4.5-5% of the total volume of the electrolyte system is supplemented every day in the electrolyte circulation process, so that the volume balance of the system is maintained.
In the electrolysis method, the main components of an electrolyte sulfate-chloride mixed system are as follows: ni: 65-75 g/l; cu is less than or equal to 0.001 g/l; fe is less than or equal to 0.0004 g/l; pb is less than or equal to 0.00025g/l and Zn is less than or equal to 0.00025 g/l; as is less than or equal to 0.00025 g/l; na (Na)+25~35g/l;Cl-50~70g/l;SO4 2+90~110g/l。
In the electrolysis method, the temperature of the electrolyte is as follows: 60-65 ℃; and the pH of the electrolyte is = 4.5-5.5.
In the electrolysis method, the initial current density of each cathode period is controlled to be 260A/m2The time is 4 h; the current density was then raised to 460A/m2And the time is 140 hours until the nickel is buckled out of the groove. The low current density can reduce the internal stress of the coating, improve the toughness of the coating and avoid the coating from delaminating and turning; the high current density ensures the compactness and smoothness of the later growth of the nickel button, so that the nickel button obtains good appearance and quality.
In the electrolysis method, the cell voltage is 2.8-3.0V, and the cell voltage is only 2/3 of the nickel sulfide soluble anode electrolytic cell, so that the method has the advantage of saving electric energy; the pole pitch was 190 mm.
The main grade of nickel button produced by the method of the invention, namely nickel and cobalt, reaches more than 99.98 percent, and impurity elements all meet the requirements of Ni9997 standard; the nickel button is easy to peel off, has smooth appearance and is free from defects.
Compared with the prior art, the invention has the following beneficial effects:
firstly, because the metal nickel with higher main grade components is adopted as the anode, the impurity content is low, the purity of the produced nickel button product is high, and the chemical quality is improved; secondly, the electrolyte does not need to be purified and purified, and the process is simple; thirdly, as the metal nickel is adopted as the anode and chloride ions exist in the electrolyte, the cell voltage is reduced and the electric energy consumption is reduced; fourthly, the Ni9950 product with lower market price is processed into the high-quality nickel button product with high added value by an electrolysis mode, and considerable economic benefit is generated.
Drawings
FIG. 1 is a schematic view of the connection of an electrolysis apparatus according to the present invention;
FIG. 2 is a physical appearance diagram of a nickel button manufactured by the present invention.
In the figure: 1-electrolytic bath, 2-anode titanium basket; 3-a cathode plate; 4-an anode conductive rod; 5-cathode conductive rod; 6-a liquid outlet pipe; 7-liquid inlet branch pipe; 8-a liquid inlet header pipe; 10-a first conduit; 11-a second conduit; 12-a third conduit; 13-a filter; 14-a first control valve; 15-a pump; 16-a second control valve; 17-a third control valve; 18-a fourth control valve; 19-fifth control valve.
Detailed Description
The method for producing a high-quality nickel button according to the present invention will be further described with reference to the following specific examples.
The invention relates to a method for producing a high-quality nickel button, which is completed by the following electrolytic equipment and method:
as shown in figure 1, the electrolysis equipment comprises an electrolytic bath 1, a plurality of groups of anode titanium baskets 2 used for assembling an anode and cathode plates 3 used for growing a nickel button are alternately arranged in the electrolytic bath 1, an anode conducting rod 4 and a cathode conducting rod 5 are arranged at the upper part of the electrolytic bath 1, the anode titanium baskets 2 and the cathode plates 3 are respectively connected with the anode conducting rod 4 and the cathode conducting rod 5, and the anode conducting rod 4 and the cathode conducting rod 5 are respectively connected with the positive pole and the negative pole of a direct current power supply. 1 one side of electrolysis trough is equipped with drain pipe 6, and 1 top of electrolysis trough is equipped with a plurality of feed liquor branch pipes 7 and a feed liquor house steward 8, and storage tank 9 is connected to drain pipe 6, and storage tank 9 connects second pipeline 11 and third pipeline 12 respectively through first pipeline 10, and feed liquor branch pipe 7 is connected to second pipeline 11, and third pipeline 12 passes through filter 13 (filter fineness 1 mu m), is interrupted to filter electrolyte, keeps electrolyte clean, prevents the influence of foreign matter such as environmental dust. Is connected with the liquid inlet header pipe 8. The first pipeline is sequentially provided with a first control valve 14, a pump 15 and a second control valve 16, the second pipeline 11 is provided with a third control valve 17, the third pipeline 12 is provided with a fourth control valve 18, and the liquid inlet header pipe 8 is provided with a fifth control valve 19.
The electrolyte of the invention is circulated in a closed loop, the electrolyte flows out of the electrolytic tank 1 and then enters the storage tank 9, the electrolyte is filtered every 48 hours, when the filtering is not needed, the fourth control valve 18 and the fifth control valve 19 are closed, the electrolyte enters the electrolytic tank 1 through the plurality of liquid inlet branch pipes 7, and the electrolyte enters the electrolytic tank by adopting multi-point introduction, so that the cathode concentration polarization in the electrolytic tank can be eliminated. When the electrolyte needs to be filtered, the third control valve 17 is closed, the fourth control valve 18 and the fifth control valve 19 are opened, and the electrolyte is filtered by the filter 13 and then is fed into the electrolytic cell 1 through the liquid inlet header pipe 8. The outer sleeve of the anode titanium basket 2 is provided with 747#The filter bag has the function of preventing the broken slag dissolved by the anode from falling into the dissolving solution and being adsorbed to the surface of the cathode plate to influence the quality of the nickel button.
The electrolysis method comprises the following steps: the method is characterized in that a sulfate-chloride mixed system is used as electrolyte, Ni9950 electrolytic nickel is cut into small nickel blocks (50 multiplied by 50 mm), the small nickel blocks are filled into a titanium basket to serve as an anode, a surface-treated composite metal film-coated nickel button plate serves as a cathode, and a high-quality nickel button product is produced through electrolysis. Wherein, the Ni9950 means that the appearance quality of the electrolytic nickel does not meet the Ni9997 standard, and the chemical composition can reach the Ni9997 standard. The main components of the electrolyte sulfate-chloride mixed system are as follows: ni: 65-75 g/l; cu is less than or equal to 0.001 g/l; fe is less than or equal to 0.0004 g/l; pb is less than or equal to 0.00020g/l and Zn is less than or equal to 0.00020 g/l; as is less than or equal to 0.00020 g/l; na (Na)+25~35g/l;Cl-50~70g/l;SO4 2+90~110g/l。
Controlling the temperature of electrolyte in the production process: 60-65 ℃; and the pH of the electrolyte is = 4.8-5.0. Initial current density of 260A/m per cathode period2The time is 4 h; the current density was then raised to 460A/m2And the time is 140h until the nickel is buckled out of the groove. The voltage of the electrolytic bath is 2.8-3.0V; the pole pitch was 190 mm. And (3) supplementing new water accounting for 4.5-5% of the total volume of the electrolyte system every day to maintain the volume balance of the system.
The chemical compositions of high-quality nickel button products produced by the method are randomly extracted from 3 batches of nickel button products and are shown in table 1.
Figure DEST_PATH_IMAGE001
Table 1 shows: the produced nickel button has high main grade content (Ni + Co reaches more than 99.98 percent), low impurity content and chemical components completely meeting the standard of Ni 9997.
The physical appearance of the nickel button produced by the method is shown in figure 2, and the nickel button is crown-shaped, uniform in size, smooth in surface and free of defects.

Claims (9)

1. A method for producing high-quality nickel buttons is completed by the following electrolytic equipment and method:
an electrolysis device: the electrolytic cell comprises an electrolytic cell, wherein a plurality of groups of anode titanium baskets for assembling anodes and cathode plates for growing nickel buttons are alternately arranged in the electrolytic cell, an anode conductive rod and a cathode conductive rod are arranged on the upper part of the electrolytic cell, the anode titanium baskets and the cathode plates are respectively connected with the anode conductive rod and the cathode conductive rod, the anode conductive rod and the cathode conductive rod are respectively connected with the positive pole and the negative pole of a direct-current power supply, a liquid outlet pipe is arranged on one side of the electrolytic cell, a plurality of liquid inlet branch pipes and a liquid inlet header pipe are arranged at the top of the electrolytic cell, the liquid outlet pipe is connected with a storage tank, the storage tank is respectively connected with a second pipeline and a third pipeline through a first pipeline, the second pipeline is connected with the liquid inlet branch pipes, and;
the electrolysis method comprises the following steps: the method is characterized in that a sulfate-chloride mixed system is used as electrolyte, Ni9950 electrolytic nickel is cut into small nickel blocks, the small nickel blocks are loaded into a titanium basket to serve as an anode, a surface-treated composite metal film-coated nickel button plate serves as a cathode, and a high-quality nickel button product is produced through electrolysis.
2. The method for producing a high-quality nickel button as set forth in claim 1, wherein: in the electrolysis equipment, the outer sleeve of the anode titanium basket is provided with 747#And (4) a filter bag.
3. The method for producing a high-quality nickel button as set forth in claim 1, wherein: among the electrolysis equipment, be equipped with first control flap, pump and second control flap on the first pipeline in proper order, be equipped with third control flap on the second pipeline, be equipped with fourth control flap on the third pipeline, be equipped with fifth control flap on the feed liquor house steward.
4. The method for producing a high-quality nickel button as set forth in claim 1, wherein: in the electrolytic method, "Ni 9950" means that the appearance quality of the electrolytic nickel does not meet the "Ni 9997" standard, and the chemical composition can reach the "Ni 9997" standard.
5. The method for producing a high-quality nickel button as set forth in claim 1, wherein: the size of the small nickel blocks is 40-60 multiplied by 40-60 mm.
6. The method of claim 1, wherein the step of forming a high quality nickel button comprises: in the electrolysis method, the main components of an electrolyte sulfate-chloride mixed system are as follows: ni: 65-75 g/l; cu is less than or equal to 0.001 g/l; fe is less than or equal to 0.0004 g/l; pb is less than or equal to 0.00020g/l and Zn is less than or equal to 0.00020 g/l; as is less than or equal to 0.00020 g/l; na (Na)+25~40g/l;Cl-50~70g/l;SO4 2+90~110g/l。
7. A method of producing a high quality nickel button as claimed in claim 1 wherein: in the electrolysis method, the temperature of the electrolyte is as follows: 60-65 ℃; and the pH of the electrolyte is = 4.5-5.5.
8. The method of claim 1, wherein the step of forming a high quality nickel button comprises: controlling the initial current density of 260A/m in each cathode period2The time is 4 hours; the current density was then raised to 460A/m2And the time is 140 hours until the nickel is buckled out of the groove.
9. The method of claim 1, wherein the step of forming a high quality nickel button comprises: in the electrolysis method, the voltage of an electrolysis bath is 2.8-3.0V; the pole pitch was 190 mm.
CN202110255727.4A 2021-03-09 2021-03-09 Method for producing high-quality nickel button Pending CN113061938A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110255727.4A CN113061938A (en) 2021-03-09 2021-03-09 Method for producing high-quality nickel button

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110255727.4A CN113061938A (en) 2021-03-09 2021-03-09 Method for producing high-quality nickel button

Publications (1)

Publication Number Publication Date
CN113061938A true CN113061938A (en) 2021-07-02

Family

ID=76560380

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110255727.4A Pending CN113061938A (en) 2021-03-09 2021-03-09 Method for producing high-quality nickel button

Country Status (1)

Country Link
CN (1) CN113061938A (en)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101008088A (en) * 2006-12-29 2007-08-01 金川集团有限公司 Process for preparing nickel button
CN101403124A (en) * 2007-12-20 2009-04-08 金川集团有限公司 Cathode plate used for producing nickel buckle and its production method
US20090272651A1 (en) * 2004-07-28 2009-11-05 Jinchuan Group Ltd. Method for producing high-purity nickel
CN110820034A (en) * 2018-08-08 2020-02-21 上海睿福有色金属有限公司 Nickel button production method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090272651A1 (en) * 2004-07-28 2009-11-05 Jinchuan Group Ltd. Method for producing high-purity nickel
CN101008088A (en) * 2006-12-29 2007-08-01 金川集团有限公司 Process for preparing nickel button
CN101403124A (en) * 2007-12-20 2009-04-08 金川集团有限公司 Cathode plate used for producing nickel buckle and its production method
CN110820034A (en) * 2018-08-08 2020-02-21 上海睿福有色金属有限公司 Nickel button production method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
C.M.WHITTINGTON等: "精炼镍阳极──通往工业最佳实践应用的途径", 《电镀与涂饰》, vol. 32, no. 05, pages 6 - 12 *

Similar Documents

Publication Publication Date Title
AU2016338328B2 (en) Filter press device for electroplating metal from solutions, which is formed by separating elements formed by ion-exchange membranes, forming a plurality of anolyte and catholyte chambers, the electrodes being connected in series with automatic detachment of the metallic product
CN101928957A (en) Method for electrolyzing refined copper at room temperature
CN109112569A (en) A kind of ion-exchange film method prepares the production method of manganese metal and manganese dioxide simultaneously
CN109485023A (en) A method of recycling tellurium from cupric tellurium waste liquid
CN106757149A (en) It is a kind of that manganese, lead, the method for silver are reclaimed from electrolytic zinc anode mud
CN102677062A (en) Method for electrolyzing and regenerating alkaline etching liquid
CN106676578B (en) A kind of new and effective joint additive of Zinc electrolysis
CN110616327A (en) Method and device for recovering elemental nickel from nickel-containing wastewater
CN107815540A (en) A kind of method of hydrometallurgy metal nickel cobalt and its salt product
CN106757116A (en) A kind of ABS plates the method that metal charge produces spherical basic nickel carbonate
CN113061938A (en) Method for producing high-quality nickel button
CN113293408A (en) Method for electrolytic deposition of high-purity manganese from manganese chloride electrolyte
CN101008088A (en) Process for preparing nickel button
CN105040032A (en) Method of preparing transition metal and alloy thereof through low temperature molten salt electro-deposition
CN101560677A (en) Method for preparing solution of tin methane sulfonate
CN111304694A (en) Method for directly electrolyzing scrap copper
CN204779889U (en) Flexible electrolytic device
CN100590230C (en) Method for synchronously electrolyzing metal lead and manganese dioxide in chloride medium
CN109809502A (en) A method of nickel sulfate is produced using electro deposited nickel anolyte
CN100585014C (en) A kind of ceramic diaphragm electrolytic cells and its production and application
CN104975328B (en) A kind of flexible electrolysis unit
CN111378991A (en) Production method of 5N high-purity copper
CN102888624A (en) Method for producing superfine zinc powder by performing cyclone electrolyzing on zinc-containing alkali liquor
CN106929875A (en) A kind of method that ferrate is prepared based on carbon plate plating iron
CN111197171A (en) Wet copper extraction process

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
TA01 Transfer of patent application right

Effective date of registration: 20240417

Address after: 737104 No. 2 Lanzhou Road, Beijing Road Street, Jinchuan District, Jinchang City, Gansu Province

Applicant after: Jinchuan Group Nickel Cobalt Co.,Ltd.

Country or region after: China

Address before: No.98, Jinchuan Road, Jinchuan District, Jinchang City, Gansu Province 737100

Applicant before: JINCHUAN GROUP Co.,Ltd.

Country or region before: China

TA01 Transfer of patent application right