CN110438529A - High purity indium preparation facilities - Google Patents

High purity indium preparation facilities Download PDF

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Publication number
CN110438529A
CN110438529A CN201910837831.7A CN201910837831A CN110438529A CN 110438529 A CN110438529 A CN 110438529A CN 201910837831 A CN201910837831 A CN 201910837831A CN 110438529 A CN110438529 A CN 110438529A
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CN
China
Prior art keywords
electrolytic cell
high purity
power supply
preparation facilities
purity indium
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
CN201910837831.7A
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Chinese (zh)
Inventor
李公权
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.)
Guangxi Yin Tai Science And Technology Ltd
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Guangxi Yin Tai Science And Technology 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 Guangxi Yin Tai Science And Technology Ltd filed Critical Guangxi Yin Tai Science And Technology Ltd
Priority to CN201910837831.7A priority Critical patent/CN110438529A/en
Publication of CN110438529A publication Critical patent/CN110438529A/en
Pending legal-status Critical Current

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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
    • C25C1/22Electrolytic production, recovery or refining of metals by electrolysis of solutions of metals not provided for in groups C25C1/02 - C25C1/20
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25CPROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C7/00Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25CPROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C7/00Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
    • C25C7/06Operating or servicing
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Abstract

The invention discloses a kind of high purity indium preparation facilities, are related to non-ferrous metal metallurgical technology field.Including electrolytic cell bracket, electrolytic cell bracket is equipped with multiple electrolytic cells, is equipped with electrolysis cycle system in one end of electrolytic cell, electrolysis cycle system is connect with electrolytic cell, and electrolysis cycle system is equipped with PH detection sensor;Electrical control and monitoring system and power supply unit are equipped in the other end of electrolytic cell, power supply unit is any of IGBT DC power supply or silicon rectifier DC power supply, have the functions such as the output of constant voltage/constant current double mode and long-distance intelligent control, control and display precision >=0.1V/A;Electrical control and monitoring system and power supply unit are connect with electrolyzer electric, and the top of electrolytic cell is equipped with gas collection unit.The problem of present invention can solve the prior art there are production process technology control difficulty is high, and product quality fluctuation is larger, and production environment is severe, can not produce qualified stable product.

Description

High purity indium preparation facilities
Technical field
The present invention relates to non-ferrous metallurgy technology field, especially a kind of device that high purity indium is prepared for electrolysis method.
Background technique
Indium is a kind of very important strategic dissipated metal, is to prepare ITO, copper indium gallium selenide, indium antimonide, indium phosphide, arsenic The important foundation material of the compound semiconductors such as indium, be widely used in military project, space flight and aviation, plane show, photoelectric information, the sun The fields such as energy battery, belong to one of the rare metal function new material given priority in national " made in China 2025 ".With section The development of skill, product purity requires to be continuously improved, from 5N, the 6N or even 7N or more of initial 4N-4N5 till now, original indium The presence of electrolysis production device is simply equipped, device parameter is extensive, equipment design and material are unsatisfactory for high purity indium production requirement, to life The problems such as environmental disruption is larger are produced, cause high purity indium production process technology control difficulty high, product quality fluctuation is larger, raw Bad environments are produced, qualified stable product can not be produced.
Summary of the invention
The object of the present invention is to provide a kind of high purity indium preparation facilities, it can solve the prior art, and there are production process works The problem of skill controls that difficulty is high, and product quality fluctuation is larger, and production environment is severe, can not produce qualified stable product.
To solve the above-mentioned problems, the technical solution adopted by the present invention is that: this high purity indium preparation facilities, including electrolytic cell Bracket, the electrolytic cell bracket are equipped with multiple electrolytic cells, are equipped with electrolysis cycle system, the electricity in one end of the electrolytic cell The solution circulatory system is connect with the electrolytic cell, and the electrolysis cycle system is equipped with PH detection sensor;In the another of the electrolytic cell One end is equipped with electrical control and monitoring system and power supply unit, and the power supply unit is IGBT DC power supply or silicon rectifier direct current Source it is any, have the output of constant voltage/constant current double mode and the functions such as long-distance intelligent control, control and display precision >=0.1V/ A;The electrical control and monitoring system and power supply unit are connect with the electrolyzer electric, and the top of the electrolytic cell is equipped with gas Body collector unit.
In above-mentioned technical proposal, more specifically scheme may also is that the electrolysis cycle system includes Lower tank and height The side of position slot, the Lower tank is connect by circulating line with the lower part of the electrolytic cell, and the side of the head tank passes through Circulating line is connect with the top of the electrolytic cell, and the other side of the Lower tank passes through the other side of pipeline and the head tank Connection is equipped with circulating pump, at the top of the closely described electrolytic cell of the circulating line at the closely described Lower tank of the pipeline The circulating line is equipped with flow control valve;The PH detection sensor is mounted on the Lower tank;This system is automatic Circulation, endless form are any of upper entering and lower leaving or enterprising upper next-out.
Further: the PH detection sensor is that PH detects needle.
Further, electrical control described in the electrical control and monitoring system and monitoring system include host computer group state layer, The host computer group state layer issues control instruction, the collection to multiple intensive data process block layers respectively by communication switcher layer The control instruction is transmitted to the electrolytic cell by middle data processing block layer, and data of the electrolytic cell in electrolytic process pass through Data collection layer passes back to host computer group state layer, and the data include the bath voltage, electric current, pH value.
Further, the intensive data process block layer is made of PLC controller and external equipment.
Further, the data collection layer is made of voltage sensor, current sensor and PH detection sensor.
Further, the gas collection unit includes gas gathering mask, the gas gathering mask is in broadening formation, and collection port is provided with wind The other end of valve and anti-down flow device, the air-valve and anti-down flow device connects exhaust duct.
Further, the electrolytic cell is provided with overflow port and weif orifice, by the way of in parallel between multiple-grooved series connection plus slot into Row arrangement, slot is interior to place anode and cathode, and anode and cathode is staggered, and anode quantity is n, and cathode quantity is n or n+1, the yin Extremely titanium plate, current-carrying part are titanium copper-clad structure;Busbar material is copper or high purity graphite, and busbar integrally coats insulating corrosion Coating and conductive opening.
By adopting the above-described technical solution, compared with prior art, the present invention having the beneficial effect that due to this hair It is bright to be equipped with power supply unit, electrical control and the monitoring system and gas collection unit for having the output of constant voltage/constant current double mode, institute Can technological parameter precisely be monitored and be controlled in process of production, can be received to the exhaust gas generated in production process Collection processing, therefore, so that stable product quality, the air cleaning of production environment.
Detailed description of the invention
Fig. 1 is structural schematic diagram of the invention.
Fig. 2 is electrical control and monitoring system block diagram of the invention.
Specific embodiment
The invention will be further described with reference to the accompanying drawings and examples:
Embodiment 1:
High purity indium preparation facilities shown in FIG. 1, including electrolytic cell bracket 2, set that there are six electrolytic cells 3 on electrolytic cell bracket 2, in electricity The one end for solving slot 3 is equipped with electrolysis cycle system 4, and electrolysis cycle system 4 is connect with electrolytic cell 3, and electrolysis cycle system 4 is examined equipped with PH Survey sensor 4-7;Electrical control and monitoring system 6 are equipped in the other end of electrolytic cell 3 and power supply unit 1, power supply unit 1 are IGBT DC power supply, has the output of constant voltage/constant current double mode and a functions such as long-distance intelligent control, and control and display precision >= 0.1V/A;Electrical control and monitoring system 6 and power supply unit 1 are electrically connected with the electrolytic cell 3, and the top of electrolytic cell 3 is equipped with Gas collection unit 5.
Electrolysis cycle system 4 includes Lower tank 4-1 and head tank 4-2, and the side of Lower tank 4-1 passes through circulating line 4-4 It is connect with the lower part of electrolytic cell 3, the side of head tank 4-2 is connect by circulating line 4-4 with the top of electrolytic cell 3, Lower tank The other side of 4-1 is connect by pipeline 4-6 with the other side of head tank 4-2, and circulation is equipped at the nearly Lower tank 4-1 of pipeline 4-6 4-3 is pumped, flow control valve 4-5 is equipped on the circulating line 4-4 at the top of the nearly electrolytic cell 3 of circulating line 4-4;PH detection Sensor 4-7 is mounted on Lower tank 4-1;This system is automatic cycle, and endless form is upper entering and lower leaving.
In the present embodiment, PH detection sensor 4-7 is that PH detects needle.
Electrical control and monitoring system 6, as shown in Fig. 2, including host computer group state layer 6-1, host computer group state layer 6-1 passes through Communication switcher layer 6-2 issues control instruction, intensive data process block layer 6-3 to multiple intensive data process block layer 6-3 respectively Control instruction is transmitted to electrolytic cell 3, on electrolytic cell 3 passes back to the data in electrolytic process by data collection layer 6-4 Position unit state layer 6-1, data include bath voltage, electric current, pH value.Data collection layer 4 is by voltage sensor 6-4-1, electric current Sensor 6=4-2 and PH detection sensor is constituted.
In the present embodiment, the voltage signal of 0-500mV is become the current signal of 4-20mA, voltage by data collection layer 6-4 Sensor 6-4-1 is voltage mutual inductor, and 6=4-2 of current sensor is current transformer, and PH detection sensor is PH detection Needle, the intensive data process block layer 6-3 are made of PLC controller and external equipment.
Gas collection unit 5 includes gas gathering mask 5-1, and gas gathering mask 5-1 is in broadening formation, and collection port is provided with air-valve anti-backflow The other end of equipment 5-2, the anti-down flow device 5-2 of air-valve connect exhaust duct.
Electrolytic cell is provided with overflow port and weif orifice, is arranged by the way of in parallel between multiple-grooved series connection plus slot, in slot Anode and cathode is placed, anode and cathode is staggered, and anode quantity is n, and cathode quantity is n or n+1, and cathode is titanium plate, conductive part It is divided into titanium copper-clad structure;Busbar material is copper or high purity graphite, and busbar integrally coats insulating corrosion coating and conductive opening.
The endless form of electrolysis cycle system 4 is upper intake lower outlet type: the sedimentation of the impurity such as electrolyte flow direction and the earth of positive pole Direction is consistent, is conducive to the sedimentation of the earth of positive pole and the earth of positive pole is prevented to be adhered on cathode, and electrolyte temperature distribution is relatively uniform, has Conducive to influence of the suspended impurity to cathode product quality in reduction electrolyte.But electrolyte surface floating material is not easy to be discharged outside slot.
Electrical control and monitoring system 6: data collection layer 6-4 collects the monitoring number such as voltage, electric current, pH value of electrolytic cell It is transferred to host computer group state layer 6-1 after and carries out data processing and record, when monitoring data deviates the numberical range of setting, from The raw alarm of movable property, and control instruction is sent to intensive data process block layer 6-3, intensive data process block layer 6-3 refers to according to control Enable automatic execution abnormal point correction movement.
Gas collection unit 5: electrolysis operational process can generate micro exhaust gas, and electrolyte is influenced also by electrolysis temperature It is escaped from natural evaporation above electrolytic cell 3, when gas collection unit 5 is run, the anti-down flow device 5-2 of air-valve can be automatically turned on, will Workshop is collected by gas gathering mask 5-1 and be discharged to electrolytic waste gas of the loss above electrolytic cell, the wind when present apparatus is out of service The anti-down flow device 5-2 of valve stops, and air-valve is closed, and prevents the extraneous exhaust duct that passes through from being connected to interior, prevents extraneous and air-exhausting duct Road residual thing, which is fallen into electrolytic cell, to be adversely affected.
Embodiment 2:
In the present embodiment, power supply unit 1 is silicon rectifier DC power supply, and 4 endless form of electrolysis cycle system goes out up and down to be enterprising It is consistent that the impurity such as formula, a part of electrolyte flow direction of which and the earth of positive pole settle direction, be conducive to the sedimentation of the earth of positive pole and The earth of positive pole is prevented to be adhered on cathode, electrolyte temperature distribution is relatively uniform, advantageously reduces in electrolyte suspended impurity to yin The influence of pole product quality.A part of electrolyte takes electrolyte surface floating material out of from PARALLEL FLOW above electrolytic cell 3 in time Outside slot, be conducive to electrolyte self-cleaning.Remaining working principle and embodiment 1 are same.

Claims (8)

1. a kind of high purity indium preparation facilities, including electrolytic cell bracket, the electrolytic cell bracket is equipped with multiple electrolytic cells, feature It is: is equipped with electrolysis cycle system in one end of the electrolytic cell, the electrolysis cycle system is connect with the electrolytic cell, described Electrolysis cycle system is equipped with PH detection sensor;Electrical control and monitoring system and power supply are equipped in the other end of the electrolytic cell Unit, the power supply unit are any of IGBT DC power supply or silicon rectifier DC power supply, and it is defeated to have constant voltage/constant current double mode Out and the functions such as long-distance intelligent control, control and display precision >=0.1V/A;The electrical control and monitoring system and power supply list Member is connect with the electrolyzer electric, and the top of the electrolytic cell is equipped with gas collection unit.
2. high purity indium preparation facilities according to claim 1, it is characterised in that: the electrolysis cycle system includes Lower tank And head tank, the side of the Lower tank are connect by circulating line with the lower part of the electrolytic cell, the side of the head tank It is connect by circulating line with the top of the electrolytic cell, the other side of the Lower tank is another by pipeline and the head tank Side connection, is equipped with circulating pump, on the top of the closely described electrolytic cell of the circulating line at the closely described Lower tank of the pipeline The circulating line at place is equipped with flow control valve;The PH detection sensor is mounted on the Lower tank;This system is Automatic cycle, endless form are any of upper entering and lower leaving or enterprising upper next-out.
3. high purity indium preparation facilities according to claim 1 or 2, it is characterised in that: the PH detection sensor is PH spy Stylus.
4. high purity indium preparation facilities according to claim 1 or 2, it is characterised in that: the electrical control and monitoring system Including host computer group state layer, the host computer group state layer is sent out to multiple intensive data process block layers respectively by communication switcher layer The control instruction is transmitted to the electrolytic cell by control instruction out, the intensive data process block layer, and the electrolytic cell is in electricity Data in solution preocess pass back to host computer group state layer by data collection layer, and the data include the bath voltage, electricity Stream, pH value.
5. high purity indium preparation facilities according to claim 4, it is characterised in that: the intensive data process block layer is by PLC Controller and external equipment are constituted.
6. high purity indium preparation facilities according to claim 4, it is characterised in that: the data collection layer is by voltage sensor Device, current sensor and PH detection sensor are constituted.
7. high purity indium preparation facilities according to claim 1 or 2, it is characterised in that: the gas collection unit includes collection Gas hood, the gas gathering mask are in broadening formation, and collection port is provided with air-valve and anti-down flow device, the air-valve and anti-down flow device The other end connects exhaust duct.
8. high purity indium preparation facilities according to claim 1 or 2, it is characterised in that: the electrolytic cell is provided with overflow port And weif orifice, it is arranged by the way of in parallel between multiple-grooved series connection plus slot, anode and cathode, anode and cathode staggered row is placed in slot Column, anode quantity are n, and cathode quantity is n or n+1, and the cathode is titanium plate, and current-carrying part is titanium copper-clad structure;Busbar material Matter is copper or high purity graphite, and busbar integrally coats insulating corrosion coating and conductive opening.
CN201910837831.7A 2019-09-05 2019-09-05 High purity indium preparation facilities Pending CN110438529A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910837831.7A CN110438529A (en) 2019-09-05 2019-09-05 High purity indium preparation facilities

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Application Number Priority Date Filing Date Title
CN201910837831.7A CN110438529A (en) 2019-09-05 2019-09-05 High purity indium preparation facilities

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Publication Number Publication Date
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113219217A (en) * 2021-04-23 2021-08-06 先导薄膜材料(广东)有限公司 On-line monitoring device and method for electrolytic cell and computer readable storage medium
CN113668017A (en) * 2021-08-11 2021-11-19 广东长信精密设备有限公司 High-purity indium apparatus for producing

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1314500A (en) * 2000-03-22 2001-09-26 中南工业大学 Automatic controller for fully distributed aluminum electrolyzing bath
CN2786158Y (en) * 2005-05-17 2006-06-07 四川鑫炬矿业资源开发股份有限公司 Electrolytic refining device for extracting high purity metal
CN2791070Y (en) * 2005-05-19 2006-06-28 大连科思特固态化学材料有限公司 Automatic controller for closed loop electrolytic silver recovery
CN202164364U (en) * 2011-06-17 2012-03-14 贵研铂业股份有限公司 Electrochemical dissolving device for precious metals and alloys
CN103108997A (en) * 2010-08-11 2013-05-15 奥图泰有限公司 Apparatus for use in electrorefining and electrowinning
CN103103575A (en) * 2012-12-13 2013-05-15 苏州新区化工节能设备厂 Electrolyser applicable to titanium cathode plates
CN205676541U (en) * 2016-04-01 2016-11-09 福建师范大学福清分校 A kind of intelligent wireless electrolytic silver control system based on ARM
CN208472197U (en) * 2018-07-09 2019-02-05 江西龙天勇有色金属有限公司 Thick indium impurity removing equipment
CN109930173A (en) * 2019-04-12 2019-06-25 深圳市祺鑫天正环保科技有限公司 Electrolysis proposes copper equipment and its monitoring method

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1314500A (en) * 2000-03-22 2001-09-26 中南工业大学 Automatic controller for fully distributed aluminum electrolyzing bath
CN2786158Y (en) * 2005-05-17 2006-06-07 四川鑫炬矿业资源开发股份有限公司 Electrolytic refining device for extracting high purity metal
CN2791070Y (en) * 2005-05-19 2006-06-28 大连科思特固态化学材料有限公司 Automatic controller for closed loop electrolytic silver recovery
CN103108997A (en) * 2010-08-11 2013-05-15 奥图泰有限公司 Apparatus for use in electrorefining and electrowinning
CN202164364U (en) * 2011-06-17 2012-03-14 贵研铂业股份有限公司 Electrochemical dissolving device for precious metals and alloys
CN103103575A (en) * 2012-12-13 2013-05-15 苏州新区化工节能设备厂 Electrolyser applicable to titanium cathode plates
CN205676541U (en) * 2016-04-01 2016-11-09 福建师范大学福清分校 A kind of intelligent wireless electrolytic silver control system based on ARM
CN208472197U (en) * 2018-07-09 2019-02-05 江西龙天勇有色金属有限公司 Thick indium impurity removing equipment
CN109930173A (en) * 2019-04-12 2019-06-25 深圳市祺鑫天正环保科技有限公司 Electrolysis proposes copper equipment and its monitoring method

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
王鲁杨等: "《工业用电设备》", 30 September 2006, 中国电力出版社 *
程永红等: "《铜电解精炼工(铜电解工、硫酸盐工)》", 31 July 2013, 冶金工业出版社 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113219217A (en) * 2021-04-23 2021-08-06 先导薄膜材料(广东)有限公司 On-line monitoring device and method for electrolytic cell and computer readable storage medium
CN113668017A (en) * 2021-08-11 2021-11-19 广东长信精密设备有限公司 High-purity indium apparatus for producing

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