EP3181733A1 - Elektrolytreinigungsverfahren und veredler zur anwendung dieses verfahrens (varianten) - Google Patents

Elektrolytreinigungsverfahren und veredler zur anwendung dieses verfahrens (varianten) Download PDF

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Publication number
EP3181733A1
EP3181733A1 EP15200317.4A EP15200317A EP3181733A1 EP 3181733 A1 EP3181733 A1 EP 3181733A1 EP 15200317 A EP15200317 A EP 15200317A EP 3181733 A1 EP3181733 A1 EP 3181733A1
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Prior art keywords
electrolyte
sludge
unit
inputs
outputs
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EP15200317.4A
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English (en)
French (fr)
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Vladimir V. Kazakov
Khamis M. Makhianov
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D21/00—Processes for servicing or operating cells for electrolytic coating
    • C25D21/16—Regeneration of process solutions
    • C25D21/18—Regeneration of process solutions of electrolytes
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D21/00—Processes for servicing or operating cells for electrolytic coating
    • C25D21/06—Filtering particles other than ions

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  • the invention is related to electroplating, namely to methods and devices for continuous renovation, removal of insoluble particles and ultra-pure electrolyte obtaining.
  • electroplating a lot of superpurity metal is required to obtain previously unreachable parameters of devices manufactured with layered ferromagnets and layered electrical conductors of these metals.
  • electroplating of superpurity metals from their aqueous salt solutions are considered as the cheapest and most commercially viable.
  • the quality of metal deposited chemically or electrochemically on solid or liquid surface of its aqueous salt solution depends primarily on the chemical purity of this solution [1].
  • Insoluble sludge particles of the same undesirable property may occur in addition to organic and inorganic colloids in the water as insoluble particles of simple and complex compounds of silicon, aluminum and other chemical elements and their solvates, lyophilic (with high wettability by the liquid phase of the solution), due to the high nucleus charge in these particles, and loose, often having an indistinguishable density compared to contaminated solution, therefore, not nonremovable by sedimentation, centrifugation, filtration and distillation in salt solutions of used metal with components of these salts. Solutions of transition metal salts, changing its valency during air oxidation of these salts with insoluble cementite particles [1], as well as during the process involving these solutions [3] are particularly susceptible to this contamination method.
  • the main disadvantage of the method is current shunting passing through the filtered part of contaminated electrolyte, by a chain of mutually contacting graphite particles, or the loss of electric contact with electrodes due to delamination of the graphite particle concentration and growth of the insulating sludge layer. Due to the mutual screening of the particles, including due to the double electrical layer at the poles of induced electric dipole, which properties are acquired by these isolated particles, an electric potential difference even between two points in this area, one of which is close to cathode, and the second - to anode, becomes smaller ten times compared to the calculated value. Therefore electrophoresis becomes ineffective, and sludge electrical coagulation will only occur near anode and cathode of the device.
  • Another disadvantage of the device is frequent changes of the graphite material, quickly covered with sludge and cedimented. This increases the cost of electrolyte purification.
  • the third disadvantage of the device - the inability to use the method for purification of solutions of salts of iron and other transition metals due to their oxidation by air oxygen incoming with fresh particulate graphite and transition into insoluble sludge particles. This not only further contaminates electrolyte but removes salt from the working solution, making it unsuitable for use.
  • the goal of the invention is to increase efficiency and quality of purification of salt aqueous solutions of iron and other transition metals, to increase compactness and commercial attraction of the electrolyte purification method and of the refiner for its application.
  • the goal is achieved by:
  • the essential difference of the method of removal of analogue and prototype from electrolyte is the addition of the previous electrical machining with high-density current and heating, coupled with the electrolyte electrical machining, being superadditive regarding these processes, as well as the addition of mechanical filtration, and electrolyte measurement before, between, and after electrical machining, automatic calculation and control over electrical machining current, electrolyte temperature and flowrate, automatic sludge removal, signal generation for bath maintenance and on the purification end, supply of a new portion of impure electrolyte, its components, and purified electrolyte discharge, thus the electrolyte is treated fully sealed and unexposed to air;
  • the integrated processes combined this way, providing their superadditive interaction, are applied for the first time, therefore, indicate a novelty of the technical solution.
  • the essential difference of the refiner to apply the proposed electrolyte purification method is addition of a mechanical filtration unit 2 and a control unit 3; thus the sludge pretreatment unit 1 and the mechanical filtration unit 2 are series-connected; the first input of the sludge pretreatment unit 1 is connected to the source 5 for supply of impure electrolyte and its components through the first solenoid valve 4, the output of the mechanical filtration unit 2 is connected through the second solenoid valve 6 to the drain 7 of corrected purified electrolyte and to the second input of the pretreatment unit 1, which inputs also serve as the refiner inputs, a group of the sludge removal lines from the preliminary unit 1 is connected through the first group 8 of solenoid valves to the sludge drain 9, to which the group of sludge removal lines from the mechanical filtration unit 2 is connected through the second group 10 of solenoid valves; the signal outputs of both units are connected to the inputs of the control units 3, and the control inputs of both units and the control inputs of the first sole
  • the sludge pretreatment unit 1 is additionally equipped with an electric heater 20 ( R 1 ), adherent to the entire outer surface of its bottom 13, with a compartment 21 of high-current electrophoresis, located between the inputs of the pretreatment unit 1 and its low-voltage electrophoresis compartment 11, containing over two pairs of soluble electrodes 22 made of metal, which salt serves as the base for the electrolyte purified of fine sludge; thus each soluble electrode 22 is placed into the bigger case 23
  • the essential difference of the second method of removal of analogue and prototype from electrolyte is an additional coarsening of fine sludge particles by salt crystallization during electrolyte cooling.
  • the integrated operation and its interconnection with the others are applied for the first time, therefore, indicate a novelty of the technical solution.
  • the essential difference of the refiner to apply the second proposed method of removal of analogue and prototype from electrolyte is an additional crystallizer 40, thus the crystallizer 40 consists of a body 41 with an upwards expanding inner cavity, passing into a gasholder 42 at the top, and at the bottom - into a sludge compactor 43, which side walls are adhered by the second electric heater 44 ( R 2 ); a silicone dispenser 45 of cold nitrogen, spaced at a h cr distance from the upper edge of the body 41, thus the dispenser 45 input is connected to the source 46 for cooled nitrogen supply, the gasholder 42 output is connected through the upper hole in it to a drain 47 for warm nitrogen disposal, the crystallizer 40 output is located on the line of the upper edge of its body 41 and connected to the inputs of the sludge pretreatment unit 1, the first and second inputs of the crystallizer 40 are located below the cooled nitrogen dispenser 45 and serve as new inputs of the refiner, thus the first input is connected to the source 5 for impure electrolyte supply and its
  • the first option of the proposed method of electrolyte purification includes the electrical machining with high-density current and low-voltage electrical machining with electrolyte flow transmittance through mesh cathode and anode and associated heating, superadditive regarding these processes, mechanical filtration, and electrolyte measurement before, between, and after electrical machining, automatic calculation and control over electrical machining current, electrolyte temperature and flowrate, sludge removal, signal generation for bath maintenance and on the purification end, supply of a new portion of impure electrolyte, its components, and purified electrolyte discharge, thus the electrolyte is treated fully sealed and unexposed to air;
  • FIG. 1 A block diagram of the refiner for the first method of electrolyte purifification is shown in Fig. 1 and comprises a unit 1 for sludge pretreatment acting as a sediment basin and a low-voltage electrophoresis block, a mechanical filtration unit 2 and a control unit 3; thus the pretreatment unit 1 and the mechanical filtration unit 2 are series-connected; the first input of the sludge pretreatment unit 1 is connected to the source 5 for supply of impure electrolyte and its components through the first solenoid valve 4, the output of the mechanical filtration unit 2 is connected through the second solenoid valve 6 to the drain 7 of corrected purified electrolyte and to the second input of the sludge pretreatment unit 1, which inputs also serve as the refiner inputs, a group of the sludge removal lines from the preliminary unit 1 is connected through the first group 8 of solenoid valves to the sludge drain 9, to which the group of sludge removal lines from the mechanical filtration unit 2 is connected through the second group 10 of
  • the refiner comprises a sludge pretreatment unit 1, acting as a sediment basin and a low-voltage electrophoresis block, a mechanical filtration unit 2 and a control unit 3; thus the pretreatment unit 1 and the mechanical filtration unit 2 are series-connected; the first input of the sludge pretreatment unit 1 is connected to the source 5 for supply of impure electrolyte and its components through the first solenoid valve 4, the output of the mechanical filtration unit 2 is connected through the second solenoid valve 6 to the drain 7 of corrected purified electrolyte and to the second input of the sludge pretreatment unit 1, which inputs also serve as the refiner inputs; sections of the low-voltage electrophoresis compartment 11 in the pretreatment unit 1, transversal to the electrolyte flow direction, are completely blocked with a stack 12 of insoluble mesh electrodes, tightly adjacent to the inner walls of the unit 1 and making the clearance ⁇ with its bottom 13 for sludge drain into the mechanical filtration unit 2, thus ⁇
  • the sludge pretreatment unit 1 also comprises an electric heater 20 ( R 1 ), adherent to the entire outer surface of its bottom 13, with a compartment 21 of high-current electrophoresis, located between the inputs of the pretreatment unit 1 and its low-voltage electrophoresis compartment 11, containing over two pairs of soluble electrodes 22 made of metal, which salt serves as the base for the electrolyte purified of fine sludge; thus each soluble electrode 22 is placed into the bigger case 23 of acidproof di
  • the second method of electrolyte purification includes coarsening of fine sludge particles by salt crystallization during electrolyte cooling, high-density current electrical machining, low-voltage electrical machining with electrolyte transmittance through mesh cathode and anode and associated heating, superadditive relating to these electrical machining processes, mechanical filtration and electrolyte measurement before, between, and after electrical machining, automatic calculation and control over electrical machining current, electrolyte temperature and flowrate, sludge removal, signal generation for bath maintenance and on the purification end, supply of a new portion of impure electrolyte, its components, and purified electrolyte discharge, thus the electrolyte is treated fully sealed and unexposed to air.
  • the refiner comprises a sludge pretreatment unit 1, acting as a sediment basin and a low-voltage electrophoresis block, the mechanical filtration unit 2 and the control unit 3, and the crystallizer 40, thus the sludge pretreatment unit 1 and the mechanical filtration unit 2 are series-connected and connected to the crystallizer 40 output, two inputs of which are new outputs of the refiner, thus the first input of the crystallizer 40 is connected to the source 5 for impure electrolyte supply and its components through the first solenoid valve 4, and the second input is connected to the output of the mechanical filtration unit 2, which is connected through the second solenoid valve 6 to the drain 7 of corrected purified electrolyte, a group of the sludge removal lines from the preliminary unit 1 is connected through the first group 8 of solenoid valves to the sludge drain 9, to which the group of sludge removal lines from the mechanical
  • the refiner function algorithm for the first electrolyte purification method which block diagram is shown in Fig. 4 , is carried out as follows.
  • the fine sludge is considered as the most difficult to be removed from electrolytes, based on transition metal salts, quickly oxidized while exposed to air, contained in these insoluble colloidal particles.
  • a saturated aqueous solution of ferric chloride FeCl 2 is a typical representative of these imbalance electrolytes, with ultra purity to be achieved is believed to be the most commercially attractive and of the greatest practical significance [26].
  • the method is provided by simultaneous physical-chemical processes, i.e. electrolyte heating, high-current electrophoresis, low-voltage electrophoresis, and mechanical filtration.
  • electrolyte temperature of above 75 °C
  • the frequency and energy of collision of fine sludge particles are sufficient for adhesion of particles of greater than 200 nm. This is evident even visually by quick turbidity of impure electrolyte [28].
  • Simultaneous electrophoresis processes lead to increased colloidal sludge concentration near the electrodes, and the particle coarsening by the electrolyte heating is accelerated more than 10 ... 100 times.
  • the coarsening involves a big part of all insoluble particles, i.e. particles of greater than 1 nm.
  • the low-voltage electrophoresis functions in the low-voltage electrophoresis compartment 11 is similar. Even the usual combination of several functions of one unit capacity allows to reduce its dimensions and to increase its productivity and efficiency, including the quality of the device functions. Superadditive improves the device parameters by k sa times.
  • the combination of two types of electrophoresis is required to improve the refiner performance, to reduce energy costs for electrolyte treatment by automatic optimization of the schedule of the use of capabilities of these types of electrophoresis.
  • the high-current electrophoresis is especially effective at an initial stage of sludge removal and correction of the electrolyte composition, since it allows not only to coarsen the sludge quickly, but also to restore the ion concentration of the working metal in the electrolyte, decreased as a result of its use in chemical and metal electroplating, as well as of oxidation when exposed to air.
  • Traditional electroplating technology is limited only by this kind of electrolyte treatment, its duration in hours is approximately determined from the empirical relation T ⁇ (12 ...
  • V - the treated electrolyte volume in liters, I - electric current flowing through the electrolyte volume V [29], [3], [30], [13].
  • the effectiveness of this type of electrical-machining decreases 6 times in 3 hours, and electric energy will be mainly spent for the electrolyte ohmic heating, even though the colloidal sludge concentration in electrolyte is decreased only by 50 %.
  • the density J H ph of current near cathode and anode surfaces can be selected from a range of 20 ... 350 A/dm 2 .
  • anodes from the electrode 22 group almost completely dissolve and become unsuitable for further use.
  • an automatic change of the output polarity in the high power source 25 is provided at regular intervals ⁇ T ⁇ 5 ... 30 minutes.
  • the electrodes 22 metal in this case is consumed insignificantly - only to restore the ion concentration in the electrolyte, which typically decreases by less 2 %. Since the necessity to restore the metal ion concentration in the electrolyte disappears in 3 ... 4 hours, then only low-voltage electrophoresis is advisable to be used in the future to save energy.
  • the low voltage is required between the fabric electrodes 15 and 17 of the electrode stack 12 because the metal deposition is unacceptable since it could cause not only their short circuit, but also the loss of electrode porosity and electrolyte clog in the compartment 11 volume. Since transition metals in aqueous solutions are mainly electronegative, i.e. are located to the left of hydrogen in electrochemical series, the voltage on the electrodes 15 and 17 can be reduced to values when the metal isolation on cathode becomes impossible.
  • the obtained coarsen sludge can be removed from the electrolyte using available highly-efficient mechanical filters periodically cleaned of accumulated sludge, having an inexpensive structure based on cartridges with pores of 1 ... 5 ⁇ m.
  • the electrolyte returns to repeat the treatment and purification cycles, after the first treatment cycle, through the connected output of the mechanical filtration unit 2 and the input of the sludge pretreatment unit 1. This allows to remove the sludge, more stable due to its decreased concentration and concentration of particles tended to coagulate. Therefore, the used superadditive processes of sludge coagulation are non-selective, affecting all kinds of fine sludge, irrespective of dispersion, structure and chemical composition.
  • Ultra-pure electrolyte with high performance and cost minimization is available thanks to the automatic control of the electrolyte parameters and the timely automatic switching of sludge treatment and filtration modes, correction of electrolyte composition.
  • This function is performed by the refiner control unit 3 operating as follows.
  • the 3 control unit is initialized, and the signals are continuously sampled from outputs of the photodetector 28 to measure the turbidity, color, and light polarization, and the thermal relay 32 during alternating pulse switching on of the front LED and laser modules 27, and alternating sequential pulsed switchings on of the upper LED and laser modules 27.
  • the signal at the photodetectors 28 outputs is maximal for a horizontal beam from the laser modules 27 with vertical light polarization, and is absent at the photodetector 28 outputs for a scattered beam from the upper laser modules 27 with polarization by normal to the angle of the beam, no color signal and perpendicular components of the light polarization appear at the photodetector 28 outputs.
  • the controller 37 sends to the indication and annunciator panel 39 a command to display signs to fill electrolyte, sets a command to open the first solenoid valve 4 and continues the mode of initial sample of the photodetector 28.
  • the control unit 3 monitors the electrolyte level in the refiner. In this mode, its commands for the rest of the controlled refiner components are not active.
  • the same low signal is set at the photodetector 28 outputs. Then signals to turn on these power sources are set at the control unit 3 outputs, connected to the control inputs of the low-voltage source 19 and the high-current source 25, the signal to open the valve 4 is switched off. At the same time the control unit 3 constantly checks the thermal relay 32 output state, and if the contacts are not closed or an electrolyte temperature signal is below a predetermined value of 75 ° ...
  • the control unit 3 sends a command to switch the first electric heater 20 ( R 1 , TC) on; later when the thermal relay 32 contacts are closed or a temperature signal is higher than predetermined, this command is always switched off and on, when the thermal relays 32 outputs return into the initial state. If the electrolyte temperature is not decreased over time T cool > 1 min at the switched off electric heater 20, then the high-current source 25 can be switched off to reduce the electrolyte temperature, however after achieved electrolyte temperature decrease below predetermined of 75 ...°90°°C, a program jump of the control unit 3 occurs not to enable the electric heater 20, but to switch off the high-current source 25.
  • the control unit 3 sends a command to switch the pump 33 on and the valve of the third group of valves 35, relating to the first input line I of the filters 34.
  • Output signals of photodetectors 28 are changed during the sludge treatment in the sludge pretreatment unit 1 and its removal in the mechanical filtration unit 2, allowing to measure the sludge concentration at different stages of removal of sludge:
  • the correction of electrolyte concentration and composition, changed at its sludging-up, is followed by the procedure of the last electrolyte purification phase in the control unit 3 program.
  • the control unit 3 polls signals at the outputs of the conductivity meter 29, the densitometer 30, the pH -meter 31 and the thermometer (thermo-relay) 32, and, calculating the procedure parameters, sets information on the number of missing electrolyte components, i.e. acid or alkali, at the indication and annunciator panel 39, sets a signal to open the solenoid valve 4.
  • the true sludge-free solution of metal salt is provided by the refiner operation.
  • the invention goal is achieved by the proposed method of electrolyte purification and the refiner to apply it - to increase efficiency and quality of purification of salt aqueous solutions of iron and other transition metals, to increase compactness and commercial attraction of the electrolyte purification method and the refiner to apply it.
  • the refiner function algorithm for the second electrolyte purification method which block diagram is shown in Fig. 5 , is supplemented with a procedure of fine sludge particle coarsening by salt crystallization during supersaturated electrolyte cooling, and this procedure starts the first phase of repetitive cycles of sludge treatment and electrolyte filtration. Thanks to this operation, electrolyte is quickly purified of fine particles, not tended to coagulation due to the absence of ionization, electrical polarity or the possibility of its induction, unpaired magnetic moments, hidden by an energy penetrable double electric or shielding layer in the coagulated particles.
  • the particles formed by non-hydratable oxides, fluorides, oxychlorides, allotropic graphite modifications, hydrocarbons, and other organic compounds are characterized by the highest concentration among fine particles not tended to coagulation. These particles as well as colloidal ones are considered to be the salt crystallization centers during cooling of supersaturated aqueous solution of FeCl 2 and of salts of other transition metals.
  • the resulting turbidity of fine crystals is precipitated, takes the sludge from the solution, and increases the sludge concentration to values at which coagulation is possible for the particles unable to coagulate because of their insufficient concentration in solution. Collision of sedimented crystals and remaining fine sludge particles is similar to the sorbent action, i.e.
  • the control unit 3 is initialized, and similarly the signals from outputs of the turbidity, color and light polarization photodetector 28 and the thermal relay 32 are continuously polled during alternating pulse switching on of the front LED and laser modules 27 and alternating sequential pulsed switchings on of the upper LED and laser module 27. If the electrolyte amount in the refiner, i.e.
  • the controller 37 of the unit 3 displays a command on the panel 39 to fill electrolyte, sets a command to open the first solenoid valve 4 of the crystallizer 40, and continues the mode of the initial poll of the photodetectors 28, constantly monitoring the electrolyte level in the refiner.
  • the commands is for the rest controlled components of the refiner remain inactive.
  • the algorithm of the control unit 3 based on a comparison of the measured electrolyte parameters with its tabulated values, is similar to the unit operation in the first option of the refiner except that a command to switch on the solenoid valve 43, of similar designation, of the crystallizer 40, is set with the short-term signal to switch on the solenoid valves of the group 8 of the sludge drain from the pockets 24 of the sludge pretreatment unit 1.
  • the electric heater 44 ( R 2 ) operates synchroniously with the electric heater 20 of the sludge pretreatment unit 1.
  • the refiner self-stabilization achieved thanks to the control unit 3, excludes the need for time-consuming manual calculations and the refiner mode control, arising from differences of contamination in different electrolyte batches, to provide determined electrolyte ultra-purity with minimal energy consumption.
  • the electrolyte flow in the case 43 of the crystallizer 40 is directed upwardly from its inlet to its outlet.
  • Fine sludge particles, to be removed from electrolyte are considered to be crystallization nucleation arising in this case.
  • the electrolyte becomes unsaturated in and on the compactor, up to the of the distributor 45 level, so the salt crystals, collected in the sludge compactor 43, are dissolved in the electrolyte, turning it into saturated state, and the heated sludge compacted and coagulates by force.
  • the nitrogen, heated in the electrolyte, collected in the gasholder 42 of the refiner 40, is coming through the disposal drain 47 and after cooling to the cold nitrogen source 46.
  • An initial solution to be purified obtained by dissolving of available salt FeCl 2 ( FeCl 2 ⁇ 4H 2 O crystalline) or iron etching with hydrochloric acid, has pale green color.
  • the proposed methods of electrolyte purification and the refiners provide achievement of the invention goal - to improve efficiency and quality of purification of salt aqueous solutions of iron and other transition metals, to increase compactness and commercial attraction of the electrolyte purification process and the refiner to apply it.
  • the great decrease in the electrolyte cost is achieved not by reducing the electrolyte purification quality but by using automatic refiners applying the proposed treatments and purification.
  • the claimed methods of electrolyte purification and the refiners to apply it are believed to be universal and can be used in the production of high-pure commercial salts of transition and other metals, as well as in removal of fine sludge from mineral and fresh water without losing their healthful mineral composition, in the preparation of high-pure solutions for medical application.
  • the refiners Due to deep purification, the refiners can be used to produce commercially attractive coatings and foils of very extensive range of pure metals not only by electroplating, but chemical deposition.
  • An ability to customize the refiners for purification and correction of salt solutions of different metals allows their use in the production of high-quality polymetallic, coatings of alternating layers of different metals, highly corrosion resistance coatings.
  • the refiners can also be used in the production of high-pure chemicals.
  • the distributor 45 of the crystallizer 40 is made in the form of a net of silicone pipes with small holes.
  • the pretreatment unit 1 case and the crystallizer 40 are manufactured of pure titanium coated with titanium oxide or other chemically resistant material.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Filtration Of Liquid (AREA)
EP15200317.4A 2015-12-16 2015-12-16 Elektrolytreinigungsverfahren und veredler zur anwendung dieses verfahrens (varianten) Withdrawn EP3181733A1 (de)

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Cited By (2)

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CN108358387A (zh) * 2018-03-07 2018-08-03 武汉东川自来水科技开发有限公司 一种电镀废水处理***及方法
CN112144100A (zh) * 2020-09-24 2020-12-29 芜湖时烁电子科技有限公司 一种电镀槽中电镀液的回收***

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