CN203890449U - Device for preparing high-purity copper - Google Patents
Device for preparing high-purity copper Download PDFInfo
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- CN203890449U CN203890449U CN201420297345.3U CN201420297345U CN203890449U CN 203890449 U CN203890449 U CN 203890449U CN 201420297345 U CN201420297345 U CN 201420297345U CN 203890449 U CN203890449 U CN 203890449U
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
本实用新型提供一种高纯铜的制备设备，包括有电解槽和导电排，电解槽包括进液口、U型进液管、隔水板和出液口。导电排包括绝缘边、阳极导电排和阴极导电排。电解槽内设置有阴极板和阳极板，电解槽的槽边上设置有导电排，其特征在于，所述电解槽为上进下出平行流循环电解槽，U型进液管的两端与电解槽的槽体焊接在一起，在U型进液管内侧平行分布多个小孔，电解液由进液口流入U型进液管，向电解槽内阴阳极板间输送电解液，整个进液系统位于电解液面上方，进入槽中的电解液由隔水板从下方导出，从出液口流到槽外，完成循环。本实用新型保证了电解槽中离子的均匀分布，确保阴极铜的质量，避免出现槽电压升高的现象。
The utility model provides high-purity copper preparation equipment, which includes an electrolytic tank and a conductive row. The electrolytic tank includes a liquid inlet, a U-shaped liquid inlet pipe, a water baffle and a liquid outlet. The conductive bar includes an insulating edge, an anode conductive bar and a negative conductive bar. A cathode plate and an anode plate are arranged in the electrolytic cell, and a conductive row is arranged on the edge of the electrolytic cell. The tank body of the tank is welded together, and a number of small holes are distributed in parallel on the inside of the U-shaped liquid inlet pipe. The system is located above the electrolyte surface, and the electrolyte entering the tank is led out from below by the water baffle, and flows out of the tank from the liquid outlet to complete the cycle. The utility model ensures the uniform distribution of ions in the electrolytic cell, ensures the quality of cathode copper, and avoids the phenomenon that the voltage of the cell increases.
Description
Technical field
The utility model relates to a kind of preparation facilities of high purity copper, especially relates to a kind of preparation facilities of preparing 6N and the above high purity copper of 6N under nitric acid system with 3N-4N cupric electrolysis.
Background technology
6N superelevation fine copper, contained impurity is considerably less, has minimum grain boundary area, little lattice imperfection, its residual resistance rate is than the high 20 times of left and right of 4N copper.Thereby there is high conductivity and heat conductivility, low softening temperature and good workability.Be widely used in the fields such as microelectronics industry sputtering target material and ion film plating, integrated circuit linkage lead-in wire, HD Audio wire rod, superminiature transformer winding, senior special alloy, there is high economic worth and strategic importance.
High purity copper preparation method mainly contains two classes: a class is chemical purification method, as electrolytic refining process, ion exchange method etc.; One class is physical purification method, as zone melting method, vacuum melting method, electron-beam process etc.The method of purification that general preparation technology all adopts several different methods to combine, technical process is relatively complicated, affects quality factor many, and quality product is wayward.
The patent " preparation method of high purity copper " that on June 19th, 2013, disclosed Chinese patent application notification number was CN103160854A, discloses a kind of method of sulfuric acid system electrolytic preparation 5N high purity copper.It is 10-100 g/L that the method adopts copper ion concentration, be to carry out electrolysis under the condition of 20-80 DEG C in temperature.Easily there is CuSO
45H
2o crystallization and the circulating line that causes stops up, what impact was produced normally carries out.
The patent that October 8, disclosed Chinese patent application notification number was CN101280430A in 2008, disclose a kind of adopt nitric acid system electrolysis, vacuum induction melting or electron beam melting combine preparation ultrapure copper method.The method is taking 4N electrolytic copper as raw material, and electrolytic solution pH controls as 2.0-3.5, adopts the mode electrolysis of circulated in countercurrent to obtain 6N high purity copper.The electrolysis pH that the method control is higher, declines electrical conductivity of solution, and bath voltage is high, and energy consumption increases.Experiment discovery, 25 DEG C is in the electrolytic solution of 54 g/L at copper ion concentration, and its specific conductivity of the electrolytic solution of pH=1.01 is 3.79 mS/cm, and its specific conductivity of the electrolytic solution of pH=2.76 is 2.49 mS/cm, and specific conductivity has declined approximately 35%.
Publication number is the Japanese Patent of " Unexamined Patent 4-365888 ", discloses a kind of method that adopts nitric acid system electrolytic preparation 6N high purity copper.In patent by the impact of the oxynitride anticathode copper mass that adds hydrogen peroxide to eliminate to produce in electrolytic process.In the patent of " Unexamined Patent 4-365888 ", the add-on of hydrogen peroxide is according to preparation when electrolytic solution, determines to the amount that adds nitrous acid in electrolytic solution, and during not according to actual electrolysis, the amount of the nitrous acid producing in electrolytic solution is determined.In addition, in this patent not explanation in the time of long-time electrolysis, hydrogen peroxide add cycle and using method.
Publication number is the Japanese Patent of " Unexamined Patent 6-173063 ", discloses a kind of method that adopts nitric acid system electrolytic preparation 6N high purity copper.In patent, eliminate the impact of oxynitride by hydrogen halide.But it is unstable to generate product NOX, easily decompose, generate nitrous acid and hydrochloric acid.NOX has strong oxidizing property, and in solution, accumulation meeting anticathode copper exerts an influence for a long time.
Japanese Patent " flat 1-152291 " adopts twice membrane electrolysis to prepare high purity copper.Twice diaphragm electrolysis technique is tediously long, and energy consumption is large, complicated operation, and cost is high.
In tradition electrolyzer, the Recycle design of electrolytic solution is vertical current circulation, comprises two kinds of vertical current Recycle design of bottom in and top out and upper entering and lower leaving, and electrolytic solution enters electrolyzer from one end, bottom liquid-inlet pipe, and from top opposite end or two ends spout; Or electrolytic solution flows into electrolyzer from top, flowed out by bottom.The main drawback of this Recycle design is that the flow direction of electrolytic solution is vertical with pole plate direction, hinders ion flowing between anode and cathode, makes part electrolytic solution walk around electrode from electrolyzer both sides and directly flows out electrolyzer, can not play good circulating effect.The parallel-flow circulation of now having applied is bottom in and top out formula, and this Recycle design easily causes groove face flow of electrolyte inequality, occurs the phenomenon of dead groove and electrolytic solution splash.In addition, the sedimentation opposite direction of the circulation of bottom in and top out formula and the anode sludge, easily the disturbance anode sludge, makes the anode sludge adhere at negative electrode, affects negative electrode quality.
Summary of the invention
The purpose of this utility model is to prepare for existing nitric acid system the deficiency existing in high purity copper technology, provides a kind of by the preparation facilities of once electrolytic continuous and stable production high purity copper.The utility model adopts nitric acid system electrolytic preparation high purity copper, is 40-200 g/L at copper ion concentration, and pH is that 0.5-3.0 current density is 100-200 A/m
2temperature is to carry out constant temperature electrolysis under the condition of 20-30 DEG C, reduce energy consumption by the electrolytic solution and the twin contact system that adopt low pH value, by the Recycle design of upper entering and lower leaving parallel-flow, adopt and regularly add hydrogen peroxide to ensure the carrying out that electrolysis can be steady in a long-term, adopt the content that regularly quantitatively adds hydrochloric acid to reduce silver in cathode copper.The high purity copper obtaining by this method electrolytic preparation, analyzes through GDMS, and its purity reaches 6N and more than 6N.
The Preparation equipment of this high purity copper that the utility model provides, includes electrolyzer and busbar, and electrolyzer comprises fluid inlet, U-shaped liquid-inlet pipe, water-stop sheet and liquid outlet.Busbar comprises insulation limit, anode conducting row and negative electrode busbar.In electrolyzer, be provided with negative plate and positive plate, on the trough rim of electrolyzer, be provided with busbar, it is characterized in that, described electrolyzer is upper entering and lower leaving parallel-flow cyclic electrolysis groove, the two ends of U-shaped liquid-inlet pipe and the cell body of electrolyzer weld together, the multiple apertures of parallel distribution inside U-shaped liquid-inlet pipe, electrolytic solution flows into U-shaped liquid-inlet pipe by fluid inlet, to conveying electrolyte between cathode-anode plate in electrolyzer, whole feed liquor system is positioned at electrolysis liquid surface top, the electrolytic solution entering in groove is derived from below by water-stop sheet, from liquid outlet flows to groove, completes circulation.
Described busbar is the entirety of being made up of insulating material, comprise left, center, right three parts, every part is all interval with groove, and wherein left and right two portions bottom portion of groove of busbar is equipped with copper coin, be anode conducting row, the anode ear of positive plate is placed in anode conducting row and contacts with copper coin; The middle portion bottom portion of groove of busbar is equipped with copper rod, is negative electrode busbar, and cathode bar is put into negative electrode busbar and contacted with copper rod.
Form with twin contact between described negative plate and positive plate and busbar contacts, and negative plate and positive plate two ends all switch on, and avoids the phenomenon that causes bath voltage to raise because an end in contact is bad in electrolytic process.
Adopt the preparation method of high purity copper of the present utility model to be.
(1) preparation copper nitrate solution is as initial electrolysis liquid.
Cupric nitrate initial electrolysis liquid is by 6N level copper and meet the pure nitric acid reaction of GB/T626-2006 top grade and make, it is 18.25 M Ω cm ultrapure waters that water used is resistivity, in the copper nitrate solution of preparation, copper ion concentration is 40-200 g/L, pH value is 0.5-3.0, wherein preferably copper ionic concn is 50-100 g/L
Preferably pH value is 0.5-1.5.
(2) copper nitrate solution of preparation is packed in electrolyzer.
(3) use 4N level copper as anode, stainless steel plate or titanium plate are made negative electrode.
Positive plate is 4N level copper, and negative electrode is stainless steel plate or titanium plate, and in electrolyzer, similar poles distance between plates is 5-30cm.
(4) start electrolysis cycle, carry out DC electrolysis, on negative plate, obtain 6N high purity copper.
In electrolytic solution, add hydrogen peroxide to prevent the impact of oxynitride anticathode copper mass, add hydrochloric acid soln to reduce the content of silver in cathode copper.
Current density is 100-200 A/m
2, preferably 100-150 A/m
2.Avoid too high current density to cause NO in solution
3 -electric discharge, worsens electrolytic environments.
Extract appropriate electrolytic solution every day out, and supplementary ultrapure water and the pure nitric acid of top grade, to ensure that in electrolytic solution, copper ion concentration and pH value are constant, the amount that extracts electrolytic solution every day is calculated by copper ion concentration variable quantity.
Circulation of elecrolyte mode in electrolyzer is the circulation of upper entering and lower leaving parallel-flow, ensures being uniformly distributed of the interior ionic concn of electrolyzer and temperature, ensures the good sedimentation of the anode sludge.
In described electrolytic process, electrolysis temperature is 20-30 DEG C of constant temperature electrolysis.
In the copper nitrate solution of preparation, preferably copper ionic concn is 50-100 g/L, and preferably pH value is 0.5-1.5.
In described electrolytic solution, the amount that adds hydrogen peroxide is 0.5-1.0 mL/L, preferably 0.5-0.8 mL/L, and hydrochloric acid add-on is 100-500 mL/t-Cu.
In electrolytic process, the cycle that adds of hydrogen peroxide is 2-7 days.Add the electrolytic solution of hydrogen peroxide to need before use to leave standstill 1-6 h, excessive decomposing hydrogen dioxide solution is disappeared, avoid its anticathode copper mass in the time of electrolysis to exert an influence, the cycle that adds of hydrochloric acid is 2 h.
Compared with prior art, the beneficial effects of the utility model are.
(1), in this device, electrolytic solution is flowed between cathode-anode plate by multiple apertures of parallel distribution on liquid-inlet pipe, has ensured being uniformly distributed of electrolyzer intermediate ion.
(2) liquid outlet of this device is all above liquid level, and convenient observation, can on-call maintenance in the time occurring stopping up or damaging phenomenon.
(3) this device adopts upper intake lower outlet type Recycle design, is conducive to the sedimentation of the anode sludge, reduces it in the adhering to of negative electrode, and affects the quality of cathode copper.
(4) cathode-anode plate and busbar adopt the way of contact of twin contact, can avoid the bath voltage rising phenomenon causing because an end in contact is bad.
(5) regularly quantitatively adding of hydrochloric acid soln the content of silver in cathode copper is down to below 1 ppm, can maintains below 0.5 ppm.
(6) eliminate the impact of oxynitride in solution regularly quantitatively adding of hydrogen peroxide, ensured the carrying out of electrolysis long-term stability.
(7) by present method, can produce purity at 6N and high purity copper more than 6N by once electrolytic.
Brief description of the drawings
Fig. 1 is cell construction schematic diagram.
Fig. 2 is busbar structural representation (vertical view).
Fig. 3 is busbar structural representation (side-view).
Mark in figure: 1-electrolyzer, 2-fluid inlet, 3-busbar, 4-water-stop sheet, 5-liquid-inlet pipe, 6-liquid outlet, 7-anode conducting row, 8-insulation limit, 9-negative electrode busbar, 10-insulation limit.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the technical solution of the utility model is described further.
As shown in FIG. 1 to 3, the Preparation equipment of this high purity copper, include electrolyzer 1 and busbar 3, in electrolyzer 1, be provided with negative plate and positive plate, be provided with busbar 3 on the trough rim of electrolyzer 1, wherein electrolyzer 1 is upper entering and lower leaving parallel-flow cyclic electrolysis groove, at the two ends of this electrolyzer 1, parallel laid is provided with liquid-inlet pipe 5, liquid-inlet pipe 5 welds together with the cell body of electrolyzer 1, at the multiple inlet openings of the liquid-inlet pipe 5 parallel distribution in inner side, to conveying electrolyte in electrolyzer.
Described busbar 3 is the entirety of being made up of insulating material, comprise left, center, right three parts, every part is all interval with groove, and wherein left and right two portions bottom portion of groove of busbar 3 is equipped with copper coin, for anode conducting row 7, the anode ear of positive plate is placed in anode conducting row 7 and contacts with copper coin; The middle portion bottom portion of groove of busbar 3 is equipped with copper rod, is negative electrode busbar 9, and cathode bar is put into negative electrode busbar 9 and contacted with copper rod.
Between described negative plate and positive plate and busbar 3, contact with the form of twin contact, negative plate and positive plate two ends all switch on, and avoid the phenomenon that causes bath voltage to raise because an end in contact is bad in electrolytic process.
Embodiment 1.
Using 6N copper and the pure preparation of nitric acid copper ion concentration of top grade is 55 g/L, the Cu (NO that pH value is 0.5
3)
2initial electrolysis liquid adds H according to the ratio of 0.6 mL/L in initial electrolysis liquid
2o
2, the ratio of 200 mL/t-Cu adds HCl, and the copper nitrate solution preparing is packed in electrolyzer.Adopt 4N level copper as anode, titanium plate or stainless steel plate are negative electrode, are 150 A/m in current density
2, temperature is under 30 DEG C of conditions, to carry out bottom in and top out parallel-flow cyclic electrolysis.Electrolysis obtain cathode copper through GDMS analytical results in table 1.
Table 1 cathode copper glow discharge mass spectrometry GDMS analytical results.
Embodiment 2.
Using 6N copper and the pure preparation of nitric acid copper ion concentration of top grade is 85 g/L, the Cu (NO that pH value is 0.8
3)
2initial electrolysis liquid adds H according to the ratio of 0.6 mL/L in initial electrolysis liquid
2o
2, the ratio of 150 mL/t-Cu adds HCl, and the copper nitrate solution preparing is packed in electrolyzer.Adopt 4N level copper as anode, titanium plate or stainless steel plate are negative electrode, are 100 A/m in current density
2, temperature is under 24 DEG C of conditions, to carry out bottom in and top out parallel-flow cyclic electrolysis.Electrolysis obtain cathode copper through GDMS analytical results in table 2.
Table 2 cathode copper glow discharge mass spectrometry GDMS analytical results.
Embodiment 3.
Using 6N copper and the pure preparation of nitric acid copper ion concentration of top grade is 60 g/L, the Cu (NO that pH value is 1.2
3)
2initial electrolysis liquid adds H according to the ratio of 0.75 mL/L in initial electrolysis liquid
2o
2, the ratio of 350 mL/t-Cu adds HCl, and the copper nitrate solution preparing is packed in electrolyzer.Adopt 4N level copper as anode, titanium plate or stainless steel plate are negative electrode, are 150 A/m in current density
2, temperature is under 22 DEG C of conditions, to carry out bottom in and top out parallel-flow cyclic electrolysis.Electrolysis obtain cathode copper through GDMS analytical results in table 3.
Table 3 cathode copper glow discharge mass spectrometry GDMS analytical results.
Embodiment 4.
Using 6N copper and the pure preparation of nitric acid copper ion concentration of top grade is 90 g/L, the Cu (NO that pH value is 0.9
3)
2initial electrolysis liquid adds H according to the ratio of 0.5 mL/L in initial electrolysis liquid
2o
2, the ratio of 100 mL/t-Cu adds HCl, and the copper nitrate solution preparing is packed in electrolyzer.Adopt 4N level copper as anode, titanium plate is or stainless steel plate negative electrode, is 150 A/m in current density
2, temperature is under 25 DEG C of conditions, to carry out bottom in and top out parallel-flow cyclic electrolysis.Electrolysis obtain cathode copper through GDMS analytical results in table 4.
Table 4 cathode copper glow discharge mass spectrometry GDMS analytical results.
Embodiment 5.
Using 6N copper and the pure preparation of nitric acid copper ion concentration of top grade is 100 g/L, the Cu (NO that pH value is 0.8
3)
2initial electrolysis liquid adds H according to the ratio of 0.5 mL/L in initial electrolysis liquid
2o
2, the ratio of 300 mL/t-Cu adds HCl, and the copper nitrate solution preparing is packed in electrolyzer.Adopt 4N level copper as anode, titanium plate or stainless steel plate are negative electrode, are 120 A/m in current density
2, temperature is under 24 DEG C of conditions, to carry out bottom in and top out parallel-flow cyclic electrolysis.Electrolysis obtain cathode copper through GDMS analytical results in table 5.
Table 5 cathode copper glow discharge mass spectrometry GDMS analytical results.
Embodiment 6.
Using 6N copper and the pure preparation of nitric acid copper ion concentration of top grade is 65 g/L, the Cu (NO that pH value is 0.7
3)
2initial electrolysis liquid adds H according to the ratio of 0.8 mL/L in initial electrolysis liquid
2o
2, the ratio of 150 mL/t-Cu adds HCl, and the copper nitrate solution preparing is packed in electrolyzer.Adopt 4N level copper as anode, titanium plate or stainless steel plate are negative electrode, are 100 A/m in current density
2, temperature is under 25 DEG C of conditions, to carry out bottom in and top out parallel-flow cyclic electrolysis.Electrolysis obtain cathode copper through GDMS analytical results in table 6.
Table 6 cathode copper glow discharge mass spectrometry GDMS analytical results.
Embodiment 7.
Using 6N copper and the pure preparation of nitric acid copper ion concentration of top grade is 75 g/L, the Cu (NO that pH value is 1.0
3)
2initial electrolysis liquid adds H according to the ratio of 0.65 mL/L in initial electrolysis liquid
2o
2, the ratio of 400 mL/t-Cu adds HCl, and the copper nitrate solution preparing is packed in electrolyzer.Adopt 4N level copper as anode, titanium plate or stainless steel plate or stainless steel plate are negative electrode, are 150 A/m in current density
2, temperature is under 26 DEG C of conditions, to carry out bottom in and top out parallel-flow cyclic electrolysis.Electrolysis obtain cathode copper through GDMS analytical results in table 7.
Table 7 cathode copper glow discharge mass spectrometry GDMS analytical results.
Embodiment 8.
Using 6N copper and the pure preparation of nitric acid copper ion concentration of top grade is 80 g/L, the Cu (NO that pH value is 0.8
3)
2initial electrolysis liquid adds H according to the ratio of 0.7 mL/L in initial electrolysis liquid
2o
2, the ratio of 250 mL/t-Cu adds HCl, and the copper nitrate solution preparing is packed in electrolyzer.Adopt 4N level copper as anode, titanium plate or stainless steel plate are negative electrode, are 120 A/m in current density
2, temperature is under 23 DEG C of conditions, to carry out bottom in and top out parallel-flow cyclic electrolysis.Electrolysis obtain cathode copper through GDMS analytical results in table 8.
Table 8 cathode copper glow discharge mass spectrometry GDMS analytical results
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| Application Number | Priority Date | Filing Date | Title |
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| CN201420297345.3U CN203890449U (en) | 2014-06-06 | 2014-06-06 | Device for preparing high-purity copper |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104775132A (en) * | 2015-03-27 | 2015-07-15 | 张家港联合铜业有限公司 | Trapezoidal flow electrodeposition apparatus |
| CN105132944A (en) * | 2014-06-06 | 2015-12-09 | 东北大学 | High pure copper producing method and device |
| CN106835196A (en) * | 2017-03-20 | 2017-06-13 | 铜陵有色金属集团股份有限公司金冠铜业分公司 | Produce the mixing electrolysis system of tough cathode |
| CN112553656A (en) * | 2020-11-08 | 2021-03-26 | 株洲冶炼集团股份有限公司 | Clamping groove type zinc electrolytic tank |
| CN113279023A (en) * | 2021-05-28 | 2021-08-20 | 金川集团股份有限公司 | Circular purification impurity removal kettle for metal solution purification and impurity removal method |
| CN114196993A (en) * | 2021-12-16 | 2022-03-18 | 虹华科技股份有限公司 | Preparation method of high-purity copper for transmission cable |
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2014
- 2014-06-06 CN CN201420297345.3U patent/CN203890449U/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105132944A (en) * | 2014-06-06 | 2015-12-09 | 东北大学 | High pure copper producing method and device |
| CN105132944B (en) * | 2014-06-06 | 2017-08-11 | 东北大学 | A kind of method and device for preparing high purity copper |
| CN104775132A (en) * | 2015-03-27 | 2015-07-15 | 张家港联合铜业有限公司 | Trapezoidal flow electrodeposition apparatus |
| CN106835196A (en) * | 2017-03-20 | 2017-06-13 | 铜陵有色金属集团股份有限公司金冠铜业分公司 | Produce the mixing electrolysis system of tough cathode |
| CN106835196B (en) * | 2017-03-20 | 2018-10-30 | 铜陵有色金属集团股份有限公司金冠铜业分公司 | Produce the mixing electrolysis system of tough cathode |
| CN112553656A (en) * | 2020-11-08 | 2021-03-26 | 株洲冶炼集团股份有限公司 | Clamping groove type zinc electrolytic tank |
| CN113279023A (en) * | 2021-05-28 | 2021-08-20 | 金川集团股份有限公司 | Circular purification impurity removal kettle for metal solution purification and impurity removal method |
| CN113279023B (en) * | 2021-05-28 | 2023-05-26 | 金川集团股份有限公司 | Circulation purifying and impurity removing kettle for purifying metal solution and impurity removing method |
| CN114196993A (en) * | 2021-12-16 | 2022-03-18 | 虹华科技股份有限公司 | Preparation method of high-purity copper for transmission cable |
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| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20141022 Termination date: 20170606 |
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| CF01 | Termination of patent right due to non-payment of annual fee |