WO2021233300A1 - 一种自耗阳极电解沉积制备高纯铁的装置和方法 - Google Patents

一种自耗阳极电解沉积制备高纯铁的装置和方法 Download PDF

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WO2021233300A1
WO2021233300A1 PCT/CN2021/094375 CN2021094375W WO2021233300A1 WO 2021233300 A1 WO2021233300 A1 WO 2021233300A1 CN 2021094375 W CN2021094375 W CN 2021094375W WO 2021233300 A1 WO2021233300 A1 WO 2021233300A1
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tank
cathode
electrolyte solution
consumable anode
present
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PCT/CN2021/094375
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English (en)
French (fr)
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邱文涛
盛宇泽
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鄂州汉衍新材料有限公司
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
    • C25C1/06—Electrolytic production, recovery or refining of metals by electrolysis of solutions or iron group metals, refractory metals or manganese
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
    • C25C7/06—Operating or servicing
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

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  • the invention relates to the technical field of electrochemistry, in particular to a device and method for preparing high-purity iron by consumable anode electrodeposition.
  • High-purity iron When the content of impurity elements in iron drops to a very low level (less than one part per million), it is high purity iron.
  • High-purity iron not only has good ductility, but also has good soft magnetic properties, thermal properties, electrical conductivity and corrosion resistance. It is precisely because of these advantages of high-purity iron that it is widely used in aerospace, medical and food, electronic and electrical industries. And the processing of high-tension alloy parts.
  • the purpose of the present invention is to provide a device and method for preparing high-purity iron by consumable anode electrolytic deposition.
  • the device provided by the present invention can recycle the electrolyte solution, save processing costs, and is more environmentally friendly.
  • the miscellaneous tank purifies the electrolyte solution to keep the electrolyte solution in the electrolytic cell in a pure state, ensuring the purity of high-purity iron.
  • the present invention provides a device for preparing high-purity iron by consumable anode electrolytic deposition, which comprises a high-level tank 1, an electrolytic tank 5, a low-level tank 6, and a decontamination tank 8 which are connected in sequence.
  • the water inlet 1-1 of the high-level tank is connected;
  • a consumable anode 4, a cathode 3, and an ion permeable membrane 10 arranged between the consumable anode 4 and the cathode 3 are arranged inside the electrolytic cell 5.
  • the lower surface of the high-level tank 1 is higher than the upper surface of the electrolytic tank 5, and the lower surface of the electrolytic tank 5 is higher than the upper surface of the low-level tank 6.
  • the consumable anode 4 is a pure iron plate;
  • the cathode 3 includes a cathode plate 3-1 and a conductive rod 3-2 fixed on the cathode plate 3-1.
  • the device further includes a filter press 9, the water inlet 9-1 of the filter press is in communication with the water outlet 8-2 of the impurity removal tank, and the water outlet 9-2 of the filter press It is communicated with the water inlet 1-1 of the high-level tank.
  • a stirring device 7 is provided inside the impurity removal tank 8.
  • the present invention also provides a method for preparing high-purity iron based on the device described in the above technical solution, which includes the following steps:
  • the consumable anode 4 and the cathode 3 are placed in an electrolyte solution, and under the action of a direct current power supply, an electrochemical reaction occurs, and iron atoms are deposited on the surface of the cathode 3 to obtain high-purity iron;
  • the electrolyte solution is in a flowing state: the electrolyte solution flows from the electrolytic cell 5 to the lower tank 6, and then enters the impurity removal tank 8 for purification treatment to obtain a purified electrolyte solution;
  • the miscellaneous tank 8 is filled with purification liquid;
  • the purified electrolyte solution is transported into the high-level tank 1, and then flows from the high-level tank 1 to the electrolytic tank 5.
  • the voltage of the DC power supply is 0.7-3V, and the current density is 100-500 A/m 2 .
  • the electrolyte solution is a ferrous sulfate solution or a ferrous chloride solution; the initial concentration of the electrolyte solution is 28-112 g/L.
  • the deposition further includes: sequentially separating, washing and drying the iron deposited on the cathode 3 to obtain high-purity iron.
  • the purification liquid is a sodium sulfide solution.
  • the present invention provides a device for preparing high-purity iron by consumable anode electrolytic deposition, which comprises a high-level tank 1, an electrolytic tank 5, a low-level tank 6, and a decontamination tank 8 which are connected in sequence.
  • the water inlet 1-1 of the high-level tank is connected;
  • the electrolytic cell 5 is provided with a consumable anode 4, a cathode 3, and an ion permeable membrane 10 arranged between the consumable anode 4 and the cathode 3.
  • the electrolyte solution flows from the upper tank 1 to the electrolytic tank 5, and from the electrolytic tank 5 to the lower tank 6, so that the electrolyte solution in the electrolytic tank 5 is kept flowing to facilitate ion migration in the electrolyte solution; 6
  • the electrolyte solution flowing out is purified by the impurity removal tank 8 to remove the non-ferrous metal ions in the electrolyte solution, and then flows back to the electrolytic cell 5 through the high-level tank 1 to keep the electrolyte solution in the electrolytic cell 5 in a pure state, which can improve high-purity iron The purity.
  • the device provided by the invention can recycle the electrolyte solution, reduces the processing cost, avoids environmental pollution, and is more economical and environmentally friendly.
  • the device provided by the present invention has simple operation, control and maintenance, is convenient for transportation and installation, and is suitable for industrial applications.
  • Figure 1 is a schematic diagram of a device for preparing high-purity iron by consumable anode electrolytic deposition according to an embodiment of the present invention, where 1 is a high-level tank, 1-1 is the water inlet of the high-level tank, 2 is an electrolyte solution, 3 is a cathode, and 4 is a self-consumption Anode, 5 is the electrolytic cell, 5-1 is the water inlet of the electrolytic cell, 5-2 is the water outlet of the electrolytic cell, 6 is the low-level tank, 6-2 is the water outlet of the low-level tank, 7 is the stirring device, and 8 is the water inlet of the electrolytic tank.
  • 1 is a high-level tank
  • 1-1 is the water inlet of the high-level tank
  • 2 is an electrolyte solution
  • 3 is a cathode
  • 4 is a self-consumption Anode
  • 5 is the electrolytic cell
  • 5-1 is the water inlet of the electrolytic cell
  • 5-2 is
  • Miscellaneous tank 8-1 is the water inlet of the impurity removal tank, 8-2 is the water outlet of the impurity removal tank, 9 is the filter press, 9-1 is the water inlet of the filter press, and 9-2 is the filter press At the water outlet, 10 is an ion permeable membrane;
  • 3-1 is a cathode plate
  • 3-2 is a conductive rod.
  • the present invention provides a device for preparing high-purity iron (electrolytic iron) by consumable anode electrodeposition, which comprises a high-level tank 1, an electrolytic cell 5, a low-level tank 6, and a decontamination tank 8, which are connected in sequence, and the water outlet 8 of the deconsumption tank -2 is connected to the water inlet 1-1 of the high-level tank; the electrolytic cell 5 is provided with a consumable anode 4, a cathode 3, and an ion permeable membrane 10 arranged between the consumable anode 4 and the cathode 3 .
  • the device provided by the present invention includes an electrolytic cell 5, which provides a reaction place for electrochemically preparing high-purity iron.
  • an electrolytic cell 5 which provides a reaction place for electrochemically preparing high-purity iron.
  • a consumable anode 4, a cathode 3, and an ion permeable membrane 10 arranged between the consumable anode 4 and the cathode 3 are provided inside the electrolytic cell 5.
  • the consumable anode 4 and the cathode 3 are vertically placed in the electrolytic cell 5, and the horizontal distance between the consumable anode 4 and the cathode 3 is 20-80 mm.
  • the ion permeable membrane 10 is preferably wrapped around the consumable anode; the horizontal distance between the ion permeable membrane 10 and the surface of the consumable anode 4 is preferably 1-10 mm.
  • the consumable anode 4 and the cathode 3 are placed crosswise.
  • the consumable anode 4 is a pure iron plate, and the purity of the pure iron plate is preferably greater than 99%.
  • the consumable anode 4 is a YT01 industrial pure iron plate of Taiyuan Iron and Steel Co., Ltd.
  • the area of the pure iron plate is preferably 0.4 to 0.6 times the cross-sectional area of the electrolytic cell 5.
  • the cathode 3 includes a cathode plate 3-1 and a conductive rod 3-2 fixed on the cathode plate 3-1;
  • the cathode plate 3-1 is preferably a stainless steel plate or a titanium plate , More preferably a 316 stainless steel plate, for attaching the generated high-purity iron;
  • the conductive rod 3-2 is preferably a copper conductive rod 3-2.
  • the conductive rod 3-2 has good conductivity, has low resistance and does not generate heat during use; and has high strength, and can bear the high-purity iron deposited on the cathode plate 3-1.
  • the fixing method of the cathode plate 3-1 and the conductive rod 3-2 is preferably welding.
  • the conductive rod 3-2 is welded to the upper end of the cathode plate 3-1.
  • the area of the cathode plate 3-1 is preferably 0.4 to 0.6 times the cross-sectional area of the electrolytic cell 5; the size of the conductive rod 3-2 is preferably 15*20 mm.
  • the number of the cathode plates 3-1 is 10-100, more preferably 20; when the number of the cathode plates 3-1 is greater than one, a plurality of cathode plates 3-1 Parallel setting.
  • the air permeability of the ion permeable membrane 10 is preferably (30-60) L/m 2 ⁇ s.
  • the ion permeable membrane 10 is preferably Dacron 240, Dacron 740, Dacron 747, Dacron 758 or Dacron 3927, more preferably Dacron 747.
  • the ratio of the cross-sectional area of the ion permeable membrane 10 to the area of the consumable anode 4 is preferably 1.1:1.
  • the present invention uses the ion permeable membrane 10 to filter and remove impurities (specifically C, S, P, Pb, As elements, etc.) brought by the consumable anode 4 during the consumption process.
  • the device provided by the present invention includes a high-level tank 1 connected with the water inlet 5-1 of the electrolytic cell and a low-level tank 6 connected with the water outlet 5-2 of the electrolytic cell.
  • the electrolyte solution flows from the high-level tank 1 to the electrolysis.
  • the tank 5 flows from the electrolytic tank 5 to the low-level tank 6, so that the electrolyte solution in the electrolytic tank 5 is kept flowing, which is beneficial to the migration of ions in the electrolyte solution.
  • the lower surface of the high-level tank 1 is higher than the upper surface of the electrolytic tank 5, and the lower surface of the electrolytic tank 5 is higher than the upper surface of the low-level tank 6, so that the electrolyte solution can Keep flowing under the action of gravity.
  • the height difference between the lower surface of the upper tank 1 and the upper surface of the electrolytic tank 5 is preferably 0.5-2m; the height between the lower surface of the electrolytic tank 5 and the upper surface of the lower tank 6 The difference is preferably 0 to 0.5 m.
  • the present invention does not have special requirements for the specific structures of the high-level tank 1 and the low-level tank 6.
  • the high-level tank 1 and the low-level tank 6 that are well known to those skilled in the art can be used; the materials of the high-level tank 1 and the low-level tank 6 are preferred It is made of acid-resistant corrosion-resistant material.
  • the device provided by the present invention includes a trash removal tank 8 communicating with the water outlet 6-2 of the low-level tank, and the water outlet 8-2 of the trash removal tank is connected with the water inlet 1-1 of the high-level tank, It is used to purify the electrolyte solution, and transport the purified electrolyte solution to the upper tank 1 and then flow to the electrolytic tank 5 to keep the electrolyte solution in the electrolytic tank 5 in a pure state, which can improve the purity of high-purity iron.
  • a stirring device 7 is arranged inside the impurity removal tank 8 to improve the impurity removal efficiency.
  • the present invention does not specifically limit the specific structure and material of the impurity removal tank 8 and the stirring device 7, and the impurity removal tank 8 and the stirring device 7 well known to those skilled in the art may be used.
  • the device provided by the present invention further includes a filter press 9.
  • the water inlet 9-1 of the filter press is communicated with the water outlet 8-2 of the impurity removal tank, and the filter press
  • the water outlet 9-2 of the machine is communicated with the water inlet 1-1 of the high-level tank.
  • the present invention uses the filter press 9 to transport the electrolyte solution from the impurity removal tank 8 back to the high-level tank 1 to realize the recycling of the electrolyte solution.
  • the present invention does not have special requirements for the filter press 9, and a filter press 9 well known to those skilled in the art can be used.
  • the above-mentioned components are preferably communicated with each other through pipelines.
  • FIG. 1 a schematic diagram of a device for preparing high-purity iron by consumable anode electrolytic deposition provided by the present invention is shown in FIG.
  • the water outlet 6-2 of the lower tank is connected to the water inlet 8-1 of the impurity removal tank, the water outlet 8-2 of the impurity removal tank is connected to the water inlet 9-1 of the filter press, and the filter press
  • the water outlet 9-2 of the machine is communicated with the water inlet 1-1 of the high-level tank; wherein the inside of the electrolytic cell 5 is provided with a consumable anode 4, a cathode 3, and a consumable anode 4 Ion permeable membrane 10; the inside of the electrolytic tank 5 contains an electrolyte solution; the inside of the impurity removal tank 8 is provided with a stirring device 7.
  • the present invention also provides a method for preparing high-purity iron based on the device described in the above technical solution, which includes the following steps:
  • the consumable anode 4 and the cathode 3 are placed in an electrolyte solution, and under the action of a direct current power supply, an electrochemical reaction occurs, and iron atoms are deposited on the surface of the cathode 3 to obtain high-purity iron;
  • the electrolyte solution is in a flowing state: the electrolyte solution flows from the electrolytic cell 5 to the lower tank 6, and then enters the impurity removal tank 8 for purification treatment to obtain a purified electrolyte solution;
  • the miscellaneous tank 8 is filled with purification liquid;
  • the purified electrolyte solution is transported into the high-level tank 1, and then flows from the high-level tank 1 to the electrolytic tank 5.
  • the consumable anode 4 and the cathode 3 are placed in an electrolyte solution, and under the action of a direct current power supply, an electrochemical reaction occurs, and iron atoms are deposited on the surface of the cathode 3 to obtain high-purity iron.
  • the iron atoms on the consumable anode 4 in the electrolytic cell 5 lose electrons and become ferrous ions, and enter the electrolyte solution.
  • the ferrous ions in the electrolyte solution migrate to the cathode 3.
  • the electrons obtained on the cathode 3 become iron atoms and are deposited on the cathode 3 to obtain high-purity iron.
  • the materials of the consumable anode 4 and the cathode 3 have been described in detail above, and will not be repeated here.
  • the voltage of the DC power supply is preferably 0.7 to 3V, more preferably 0.8 to 2.2V; the current density of the DC power supply is preferably 100 to 500A/m 2 , more preferably 200 to 400A/m 2 .
  • the voltage of the DC power supply refers to the voltage drop from the consumable anode 4 to the cathode 3; the current density refers to the total current passing through the conductive part of each cathode 3 divided by the total conductive part of each cathode 3 area.
  • the present invention limits the voltage and current density of the DC power supply within the above range to ensure electrical efficiency.
  • the electrolyte solution is preferably a ferrous sulfate solution or a ferrous chloride solution; the initial concentration of the electrolyte solution is preferably 0.5 to 1.5 mol/L, more preferably 0.5 to 1.0 mol/L.
  • the ratio of the volume of the electrolyte solution to the volume of the electrolytic cell 5 is preferably 1:1.1.
  • the purity of the high-purity iron is preferably 99.9-99.99%.
  • the consumable anode 4 is continuously consumed, and when the conductive area affects the conductive parameter, a new consumable anode 4 is replaced.
  • the area of the consumable anode 4 loses 20%, the conductivity parameter changes, and the consumable anode 4 needs to be replaced.
  • the deposition after the deposition, it preferably further includes: sequentially separating, washing and drying the iron deposited on the cathode 3 to obtain high-purity iron.
  • the iron deposited on the cathode 3 is preferably in the form of flakes, and the method of separation is preferably to knock the cathode 3 to make the iron adhered to the cathode 3 fall off.
  • the washing is preferably physical washing, specifically, it is preferably rinsing with clean water under the condition of material stirring.
  • the invention does not use any chemical detergent to prevent secondary pollution.
  • the present invention removes the electrolyte remaining on the iron surface.
  • the drying is preferably hot air drying, the temperature of the drying is preferably 50-100°C, and the time is preferably 0.5-2h. In the present invention, the residual moisture on the iron surface is removed by drying.
  • the electrolyte solution is in a flowing state: the electrolyte solution flows from the electrolytic cell 5 to the low-level tank 6, and then enters the impurity removal tank 8 for purification treatment to obtain a purified electrolyte solution;
  • the purified electrolyte solution is transported into the high-level tank 1, and then flows from the high-level tank 1 to the electrolytic tank 5.
  • the flow rate of the electrolyte solution is preferably 2-6 L/h.
  • the impurity removal tank 8 is filled with a purification liquid
  • the purification liquid is preferably a sodium sulfide solution
  • the mass concentration of the sodium sulfide solution is preferably 0.5 to 1.5%.
  • the dosage ratio of the sodium sulfide solution and the electrolyte solution is preferably 0.5-2g:1L.
  • the purification treatment preferably includes sequential stirring purification and standing purification; the stirring rate of the stirring purification is preferably 30 to 120 r/min, more preferably 90 r/min; the stirring time is preferably ⁇ 30 minutes, more preferably 1 to 2 hours; the time for standing and purification is preferably 8 to 16 hours.
  • impurities referring to all elements except iron, including solid metal elements, solid acid-insoluble metal elements, and ionic metal elements
  • impurities in the electrolyte solution flowing into the impurity tank 8 are purified by purification treatment. ) Is removed to keep the electrolyte solution flowing back to the electrolytic cell 5 in a pure state.
  • the impurity elements in the impurity removal tank 8 are converted into solid precipitates through impurity removal treatment, and solid-liquid separation is preferably performed by a filter press to remove impurities.
  • the device shown in Figure 1 is used to prepare high-purity iron: including a high-level tank 1, an electrolytic cell 5, and a low-level tank 6, which are connected in turn from high to low, the water outlet 6-2 of the low tank and the water inlet 8-1 of the impurity removal tank
  • the water outlet 8-2 of the impurity removal tank is connected with the water inlet 9-1 of the filter press, and the water outlet 9-2 of the filter press is connected with the water inlet 1-1 of the high-level tank
  • the inside of the electrolytic cell 5 is provided with a consumable anode 4, a cathode 3 and an ion permeable membrane 10 wrapped around the consumable anode 4; the inside of the electrolytic cell 5 contains an electrolyte solution; the A stirring device 7 is provided inside the impurity removal tank 8.
  • the volume of the electrolytic cell 5 is 960L, and 840L of ferrous chloride solution with a concentration of 1mol/L is contained in the electrolytic cell 5.
  • the consumable anode 4 is a YT01 industrial pure iron plate of Taiyuan Iron and Steel, and the cathode 3 is 316 stainless steel. 3-1 and the copper plate welded to the conductive rod 316 of the upper end of the stainless steel plate 3-2, the use of polyester 747 as an ion permeable membrane 10; impurity tank 8 is a volume 12m 3, was filled with 5000g concentration of 1wt%. Sodium sulfide solution.
  • a thyristor DC power supply is set between the consumable anode 4 and the cathode 3 of the electrolytic cell 5, the voltage is 0.9V, and the current density is 150A/m 2.
  • the consumable anode 4 in the electrolytic cell 5 The iron atom loses electrons and becomes ferrous ions, and enters the electrolyte solution.
  • the ferrous ions in the electrolyte solution migrate to the cathode 3.
  • the ferrous ions obtain electrons on the cathode 3 and become iron atoms, which are deposited on the cathode 3 to obtain high purity iron.
  • the electrolyte solution is in a flowing state: the electrolyte solution flows from the electrolytic cell 5 to the low-level tank 6, and then enters the impurity removal tank 8 for purification treatment to obtain a purified electrolyte solution; The purified electrolyte solution is transported to the high-level tank 1 and then flows from the high-level tank 1 to the electrolytic tank 5.
  • the device shown in Figure 1 is used to prepare high-purity iron; among them, the volume of the electrolytic cell 5 is 960L, the electrolytic cell 5 contains 840L of ferrous sulfate solution with a concentration of 40g/L, and the consumable anode 4 is Taigang’s YT01 industrial pure Iron plate, the cathode 3 is a 316 stainless steel plate 3-1 and a copper conductive rod 3-2 welded to the upper end of the 316 stainless steel plate, using polyester 747 as the ion permeable membrane 10; the volume of the impurity removal tank 8 is 12m 3 , containing 5000 g of sodium sulfide solution with a concentration of 1 wt.%.
  • a thyristor DC power supply is set between the consumable anode 4 and the cathode 3 of the electrolytic cell 5, the voltage is 2.3V, and the current density is 300A/m 2.
  • the consumable anode 4 in the electrolytic cell 5 The iron atom loses electrons and becomes ferrous ions, and enters the electrolyte solution.
  • the ferrous ions in the electrolyte solution migrate to the cathode 3.
  • the ferrous ions obtain electrons on the cathode 3 and become iron atoms, which are deposited on the cathode 3 to obtain high purity iron.
  • the electrolyte solution is in a flowing state: the electrolyte solution flows from the electrolytic cell 5 to the low-level tank 6, and then enters the impurity removal tank 8 for purification treatment to obtain a purified electrolyte solution; The purified electrolyte solution is transported to the high-level tank 1 and then flows from the high-level tank 1 to the electrolytic tank 5.
  • the device shown in Figure 1 is used to prepare high-purity iron; among them, the volume of the electrolytic cell 5 is 960L, the electrolytic cell 5 contains 840L of ferrous chloride solution with a concentration of 90g/L, and the consumable anode 4 is YT01 of Taiyuan Iron and Steel Co., Ltd.
  • Industrial pure iron plate the cathode 3 is a 316 stainless steel plate 3-1 and a copper conductive rod 3-2 welded to the upper end of the 316 stainless steel plate, and polyester 240 is used as the ion permeable membrane 10; the volume of the impurity removal tank 8 is 12m 3 , It contains 1000 g of sodium sulfide solution with a concentration of 1 wt.%.
  • a thyristor DC power supply is set between the consumable anode 4 and the cathode 3 of the electrolytic cell 5, the voltage is 1.4V, and the current density is 200A/m 2.
  • the consumable anode 4 in the electrolytic cell 5 The iron atom loses electrons and becomes ferrous ions, and enters the electrolyte solution.
  • the ferrous ions in the electrolyte solution migrate to the cathode 3.
  • the ferrous ions obtain electrons on the cathode 3 and become iron atoms, which are deposited on the cathode 3 to obtain high purity iron.
  • the electrolyte solution is in a flowing state: the electrolyte solution flows from the electrolytic cell 5 to the low-level tank 6, and then enters the impurity removal tank 8 for purification treatment to obtain a purified electrolyte solution; The purified electrolyte solution is transported to the high-level tank 1 and then flows from the high-level tank 1 to the electrolytic tank 5.
  • Table 1 The chemical composition content (mass content) of the high-purity iron of Examples 1 to 3
  • Example 3 C(%) 0.0017 0.0007 0.0021 Si(%) ⁇ 0.005 0.0022 ⁇ 0.01 Mn(%) ⁇ 0.0005 0.0008 0.0005

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Abstract

本发明涉及电化学技术领域，具体涉及一种自耗阳极电解沉积制备高纯铁的装置和方法。本发明提供的装置，包括依次连通的高位罐、电解槽、低位罐和除杂罐，所述除杂罐的出水口与所述高位罐的进水口相连通；所述电解槽内设置有自耗阳极、阴极以及设置在所述自耗阳极和阴极之间的离子渗透膜。本发明提供的装置能够使电解质溶液循环利用，降低了处理成本，避免了对环境的污染，更加经济环保。另外，本发明提供的装置操作、控制和维护简单，且便于运输、安装，适宜工业化应用。

Description

一种自耗阳极电解沉积制备高纯铁的装置和方法
本申请要求于2020年05月18日提交中国专利局、申请号为CN202010417630.4、发明名称为“一种自耗阳极电解沉积制备高纯铁的装置和方法”的中国专利申请的优先权，其全部内容通过引用结合在本申请中。
技术领域
本发明涉及电化学技术领域，具体涉及一种自耗阳极电解沉积制备高纯铁的装置和方法。
背景技术
当铁中的杂质元素含量降到很低(百万分之一以下)时，即为高纯铁。高纯铁不仅具有良好的延展性，还具有很好的软磁性能、热性能、导电性能和耐腐蚀性能等，正是由于高纯铁的这些优点，因而被广泛应用于宇宙航空、医药食品、电子电器工业以及高抗张力合金零部件的加工等。
目前市场上普遍采用工业副产品硫酸亚铁(FeSO 4)溶液或氯化亚铁(FeCl 2)溶液作为原料，电解沉积得到高纯铁，但采用传统的电解沉积方法制备高纯铁时，工业副产品中其它金属离子也会在阴极板上析出，影响产品的纯度；而且电解残液量大，处理成本高，排放后对环境污染大，系统难以闭环进行。
发明内容
本发明的目的在于提供一种自耗阳极电解沉积制备高纯铁的装置和方法，采用本发明提供的装置能够使电解质溶液循环利用，节省处理成本，更加环保，在电解质溶液循环流动过程中，利用除杂罐对电解质溶液进行净化，使电解槽内的电解质溶液保持纯净状态，保证了高纯铁的纯度。
为了实现上述发明目的，本发明提供以下技术方案：
本发明提供了一种自耗阳极电解沉积制备高纯铁的装置，包括依次连通的高位罐1、电解槽5、低位罐6和除杂罐8，所述除杂罐的出水口8-2与所述高位罐的进水口1-1相连通；
所述电解槽5的内部设置有自耗阳极4、阴极3以及设置在所述自耗阳极4和阴极3之间的离子渗透膜10。
优选地，所述高位罐1的下表面高于所述电解槽5的上表面，所述电解槽5的下表面高于所述低位罐6的上表面。
优选地，所述自耗阳极4为纯铁板；所述阴极3包括阴极板3-1和固定在所述阴极板3-1上的导电杆3-2。
优选地，所述装置还包括压滤机9，所述压滤机的进水口9-1与所述除杂罐的出水口8-2相连通，所述压滤机的出水口9-2与所述高位罐的进水口1-1相连通。
优选地，所述除杂罐8的内部设置有搅拌装置7。
本发明还提供了基于上述技术方案所述装置的高纯铁的制备方法，包括以下步骤：
将自耗阳极4和阴极3置于电解质溶液中，在直流电源的作用下，发生电化学反应，铁原子沉积在阴极3表面，获得高纯铁；
在上述电化学反应过程中，所述电解质溶液处于流动状态：所述电解质溶液由电解槽5流至低位罐6，然后进入除杂罐8内，进行净化处理，得到净化电解质溶液；所述除杂罐8内盛装有净化液；
将所述净化电解质溶液输送至高位罐1内，再由高位罐1流至电解槽5内。
优选地，所述直流电源的电压为0.7～3V，电流密度为100～500A/m 2。
优选地，所述电解质溶液为硫酸亚铁溶液或氯化亚铁溶液；所述电解质溶液的初始浓度为28～112g/L。
优选地，所述沉积后，还包括：将阴极3上沉积的铁依次进行分离、洗涤和干燥，得到高纯铁。
优选地，所述净化液为硫化钠溶液。
本发明提供了一种自耗阳极电解沉积制备高纯铁的装置，包括依次连通的高位罐1、电解槽5、低位罐6和除杂罐8，所述除杂罐的出水口8-2与所述高位罐的进水口1-1相连通；所述电解槽5内设置有自耗阳极4、阴极3以及设置在所述自耗阳极4和阴极3之间的离子渗透膜10。在本发明中，电解质溶液由高位罐1流向电解槽5，由电解槽5流向低位罐6， 让电解槽5内的电解质溶液保持在流动之中，以利于电解质溶液中的离子迁移；低位罐6流出的电解质溶液经过除杂罐8的净化，除去电解质溶液中的非铁金属离子，再经高位罐1流回电解槽5中，保持电解槽5内的电解质溶液处于纯净状态，能够提高高纯铁的纯度。本发明提供的装置能够使电解质溶液循环利用，降低了处理成本，避免了对环境的污染，更加经济环保。另外，本发明提供的装置操作、控制和维护简单，且便于运输、安装，适宜工业化应用。
说明书附图
图1为本发明实施例提供的自耗阳极电解沉积制备高纯铁装置的示意图，其中，1为高位罐，1-1为高位罐的进水口，2为电解质溶液，3为阴极，4为自耗阳极，5为电解槽，5-1为电解槽的进水口，5-2为电解槽的出水口，6为低位罐，6-2为低位罐的出水口，7为搅拌装置，8为除杂罐，8-1为除杂罐的进水口，8-2为除杂罐的出水口，9为压滤机，9-1为压滤机的进水口，9-2为压滤机的出水口，10为离子渗透膜；
图2为本发明实施例中阴极3的结构示意图；其中，3-1为阴极板，3-2为导电杆。
具体实施方式
本发明提供了一种自耗阳极电解沉积制备高纯铁(电解铁)的装置，包括依次连通的高位罐1、电解槽5、低位罐6和除杂罐8，所述除杂罐的出水口8-2与所述高位罐的进水口1-1相连通；所述电解槽5内设置有自耗阳极4、阴极3以及设置在所述自耗阳极4和阴极3之间的离子渗透膜10。
本发明提供的装置包括电解槽5，为电化学制备高纯铁提供反应场所。在本发明中，所述电解槽5的内部设置有自耗阳极4、阴极3以及设置在所述自耗阳极4和阴极3之间的离子渗透膜10。
作为本发明的一个实施例，所述自耗阳极4和阴极3竖直放置在所述电解槽5内，所述自耗阳极4和阴极3之间的水平距离为20～80mm。作为本发明的一个实施例，所述离子渗透膜10优选包裹在所述自耗阳极周 围；所述离子渗透膜10距离所述自耗阳极4表面的水平距离优选为1～10mm。在本发明的具体实施例中，所述自耗阳极4和阴极3交叉放置。
作为本发明的一个实施例，所述自耗阳极4为纯铁板，所述纯铁板的纯度优选为大于99％。在本发明的具体实施例中，所述自耗阳极4为太钢的YT01工业纯铁板。在本发明中，所述纯铁板的面积优选为所述电解槽5截面积的0.4～0.6倍。
作为本发明的一个实施例，所述阴极3包括阴极板3-1和固定在所述阴极板3-1上的导电杆3-2；所述阴极板3-1优选为不锈钢板或钛板，更优选为316不锈钢板，用于附着生成的高纯铁；所述导电杆3-2优选为紫铜导电杆3-2。在本发明中，所述导电杆3-2具有较好的导电性能，在使用过程中电阻小不发热；而且具有较高的强度，能承载阴极板3-1上沉积的高纯铁。在本发明中，所述阴极板3-1和导电杆3-2的固定方式优选为焊接。在本发明的具体实施例中，所述导电杆3-2焊接在阴极板3-1的上端。
作为本发明的一个实施例，所述阴极板3-1的面积优选为所述电解槽5截面积的0.4～0.6倍；所述导电杆3-2的尺寸优选为15*20mm。作为本发明的一个实施例，所述阴极板3-1的个数为10～100个，更优选为20个；当所述阴极板3-1的个数大于1个时，多个阴极板3-1并联设置。
在本发明中，所述离子渗透膜10的透气率优选为(30～60)L/m 2·s。作为本发明的一个实施例，所述离子渗透膜10优选为涤纶240、涤纶740、涤纶747、涤纶758或涤纶3927，更优选为涤纶747。在本发明中，所述离子渗透膜10的截面积与所述自耗阳极4的面积比优选为1.1:1。本发明通过离子渗透膜10过滤去除自耗阳极4在消耗过程中带来的杂质(具体为C、S、P、Pb、As元素等)。
本发明提供的装置包括与所述电解槽的进水口5-1相连通的高位罐1以及与所述电解槽的出水口5-2相连通的低位罐6，电解质溶液由高位罐1流向电解槽5，由电解槽5流向低位罐6，使电解槽5内的电解质溶液保持在流动之中，有利于电解质溶液中离子的迁移。
作为本发明的一个实施例，所述高位罐1的下表面高于所述电解槽5的上表面，所述电解槽5的下表面高于所述低位罐6的上表面，使得电解 质溶液能够在重力的作用下保持流动。在本发明中，所述高位罐1的下表面和电解槽5的上表面之间的高度差优选为0.5～2m；所述电解槽5的下表面和低位罐6的上表面之间的高度差优选为0～0.5m。本发明对所述高位罐1和低位罐6的具体结构没有特殊的要求，采用本领域技术人员所熟知的高位罐1和低位罐6即可；所述高位罐1和低位罐6的材质优选为耐酸腐蚀材质。
本发明提供的装置包括与所述低位罐的出水口6-2相连通的除杂罐8，所述除杂罐的出水口8-2与所述高位罐的进水口1-1相连通，用于净化电解质溶液，并将净化后的电解质溶液输送至高位罐1中，再流至电解槽5中，保持电解槽5内的电解质溶液处于纯净状态，能够提高高纯铁的纯度。
作为本发明的一个实施例，所述除杂罐8的内部设置有搅拌装置7，提高除杂效率。本发明对所述除杂罐8和搅拌装置7的具体结构以及材质没有特殊的限定，采用本领域技术人员所熟知的除杂罐8和搅拌装置7即可。
作为本发明的一个实施例，本发明提供的装置还包括压滤机9，所述压滤机的进水口9-1与所述除杂罐的出水口8-2相连通，所述压滤机的出水口9-2与所述高位罐的进水口1-1相连通，本发明利用压滤机9将除杂罐8流出的电解质溶液输送回高位罐1，实现电解质溶液的循环利用。本发明对所述压滤机9没有特殊的要求，采用本领域技术人员所熟知的压滤机9即可。
在本发明中，上述各部件之间优选通过管路连通。
作为本发明的一个实施例，本发明提供的自耗阳极电解沉积制备高纯铁的装置的示意图如图1所示，包括由高到低依次连通的高位罐1、电解槽5和低位罐6，所述低位罐的出水口6-2与除杂罐的进水口8-1相连通，所述除杂罐的出水口8-2与压滤机的进水口9-1相连通，所述压滤机的出水口9-2与所述高位罐的进水口1-1相连通；其中，所述电解槽5的内部设置有自耗阳极4、阴极3以及包裹在所述自耗阳极4周围的离子渗透膜10；所述电解槽5的内部盛有电解质溶液；所述除杂罐8的内部设置有搅拌装置7。
本发明还提供了基于上述技术方案所述装置的高纯铁的制备方法，包括以下步骤：
将自耗阳极4和阴极3置于电解质溶液中，在直流电源的作用下，发生电化学反应，铁原子沉积在阴极3表面，获得高纯铁；
在上述电化学反应过程中，所述电解质溶液处于流动状态：所述电解质溶液由电解槽5流至低位罐6，然后进入除杂罐8内，进行净化处理，得到净化电解质溶液；所述除杂罐8内盛装有净化液；
将所述净化电解质溶液输送至高位罐1内，再由高位罐1流至电解槽5内。
本发明将自耗阳极4和阴极3置于电解质溶液中，在直流电源的作用下，发生电化学反应，铁原子沉积在阴极3表面，获得高纯铁。在所述电化学反应过程中，电解槽5内自耗阳极4上的铁原子失去电子变成亚铁离子，进入电解质溶液中，电解质溶液中的亚铁离子向阴极3迁移，亚铁离子在阴极3上得到电子成为铁原子，并沉积在阴极3上，获得高纯铁。在本发明中，所述自耗阳极4和阴极3的材质在前文已经进行了详细说明，这里就不再赘述。
在本发明中，所述直流电源的电压优选为0.7～3V，更优选为0.8～2.2V；所述直流电源的电流密度优选为100～500A/m 2，更优选为200～400A/m 2。在本发明中，所述直流电源的电压是指自耗阳极4到阴极3的压降；所述电流密度是指通过每个阴极3导电部分的总电流除以每个阴极3导电部分的总面积。本发明限定直流电源的电压和电流密度在上述范围能够保证电效率。当电流密度过大时(比如大于500A/m 2)，易出现树枝状生长，导致刺破离子渗透膜10或者造成阴阳极短路，当电流密度过小或者电压过小时，反应速度较慢，电效率低，产量低，当电压过高(比如大于3V)时，会出现析氢现象。
在本发明中，所述电解质溶液优选为硫酸亚铁溶液或氯化亚铁溶液；所述电解质溶液的初始浓度优选为0.5～1.5mol/L，更优选为0.5～1.0mol/L。在本发明中，所述电解质溶液的体积与所述电解槽5的体积比优选为1:1.1。
在本发明中，所述高纯铁的纯度优选为99.9～99.99％。
本发明在上述电化学反应过程中，自耗阳极4不断消耗，至导电面积影响导电参数时，更换新的自耗阳极4。在本发明的具体实施例中，当所述自耗阳极4的面积损失20％时，导电参数发生变化，需要更换自耗阳极4。
在本发明中，所述沉积后，优选还包括：将阴极3上沉积的铁依次进行分离、洗涤和干燥，得到高纯铁。在本发明中，所述阴极3上沉积的铁优选为片状，所述分离的方式优选为敲打阴极3，使附着在所述阴极3的铁脱落。在本发明中，所述洗涤优选为物理清洗，具体优选为物料搅拌条件下清水漂洗。本发明不采用任何化学洗涤剂，防止二次污染。本发明通过除去铁表面残留的电解质。在本发明中，所述干燥优选为热空气干燥，所述干燥的温度优选为50～100℃，时间优选为0.5～2h。本发明通过干燥除去铁表面残留的水分。
本发明在上述电化学反应过程中，所述电解质溶液处于流动状态：所述电解质溶液由电解槽5流至低位罐6，然后进入除杂罐8内，进行净化处理，得到净化电解质溶液；
将所述净化电解质溶液输送至高位罐1内，再由高位罐1流至电解槽5内。
在本发明中，所述电解质溶液的流速优选为2～6L/h。
在本发明中，所述除杂罐8内盛装有净化液，所述净化液优选为硫化钠溶液，所述硫化钠溶液的质量浓度优选为0.5～1.5％。在本发明中，所述硫化钠溶液和电解质溶液的用量比优选为0.5～2g：1L。在本发明中，所述净化处理优选包括依次进行的搅拌净化和静置净化；所述搅拌净化的搅拌速率优选为30～120r/min，更优选为90r/min；所述搅拌的时间优选≥30min，更优选为1～2h；所述静置净化的时间优选为8～16h。本发明通过净化处理将流入除杂罐8内的电解质溶液中的杂质(指除铁以外的所有元素，具体包括固体态的金属元素、固体态的不溶于酸的金属元素和离子态的金属元素)去除，使流回电解槽5的电解质溶液保持纯净状态。在本发明中，所述除杂罐8中杂质元素通过除杂处理成为固体沉淀物，优选通过压滤机进行固液分离，除去杂质。
下面将结合本发明中的实施例，对本发明中的技术方案进行清楚、完 整地描述。显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1
采用图1所示的装置制备高纯铁：包括由高到低依次连通的高位罐1、电解槽5和低位罐6，所述低位罐的出水口6-2与除杂罐的进水口8-1相连通，所述除杂罐的出水口8-2与压滤机的进水口9-1相连通，所述压滤机的出水口9-2与所述高位罐的进水口1-1相连通；其中，所述电解槽5的内部设置有自耗阳极4、阴极3以及包裹在所述自耗阳极4周围的离子渗透膜10；所述电解槽5的内部盛有电解质溶液；所述除杂罐8的内部设置有搅拌装置7。
其中，电解槽5的体积为960L，在电解槽5内盛有840L的浓度为1mol/L的氯化亚铁溶液，自耗阳极4为太钢的YT01工业纯铁板，阴极3为316不锈钢板3-1和焊接在所述316不锈钢板上端的紫铜导电杆3-2，采用涤纶747作为离子渗透膜10；除杂罐8的体积为12m 3，盛有5000g的浓度为1wt.％的硫化钠溶液。
在电解槽5的自耗阳极4和阴极3之间设置可控硅直流电源，电压为0.9V，电流密度为150A/m 2，在直流电源的作用下，电解槽5内自耗阳极4上的铁原子失去电子变成亚铁离子，进入电解质溶液中，电解质溶液中的亚铁离子向阴极3迁移，亚铁离子在阴极3上得到电子成为铁原子，并沉积在阴极3上，获得高纯铁；在上述电化学反应过程中，所述电解质溶液处于流动状态：所述电解质溶液由电解槽5流至低位罐6，然后进入除杂罐8内，进行净化处理，得到净化电解质溶液；将所述净化电解质溶液输送至高位罐1内，再由高位罐1流至电解槽5内。
实施例2
采用图1所示的装置制备高纯铁；其中，电解槽5的体积为960L，在电解槽5内盛有840L浓度为40g/L的硫酸亚铁溶液，自耗阳极4为太钢的YT01工业纯铁板，阴极3为316不锈钢板3-1和焊接在所述316不锈钢板上端的紫铜导电杆3-2，采用涤纶747作为离子渗透膜10；除杂罐8的体积为12m 3，盛有5000g的浓度为1wt.％的硫化钠溶液。
在电解槽5的自耗阳极4和阴极3之间设置可控硅直流电源，电压为2.3V，电流密度为300A/m 2，在直流电源的作用下，电解槽5内自耗阳极4上的铁原子失去电子变成亚铁离子，进入电解质溶液中，电解质溶液中的亚铁离子向阴极3迁移，亚铁离子在阴极3上得到电子成为铁原子，并沉积在阴极3上，获得高纯铁；在上述电化学反应过程中，所述电解质溶液处于流动状态：所述电解质溶液由电解槽5流至低位罐6，然后进入除杂罐8内，进行净化处理，得到净化电解质溶液；将所述净化电解质溶液输送至高位罐1内，再由高位罐1流至电解槽5内。
实施例3
采用图1所示的装置制备高纯铁；其中，电解槽5的体积为960L，在电解槽5内盛有840L的浓度为90g/L的氯化亚铁溶液，自耗阳极4为太钢的YT01工业纯铁板，阴极3为316不锈钢板3-1和焊接在所述316不锈钢板上端的紫铜导电杆3-2，采用涤纶240作为离子渗透膜10；除杂罐8的体积为12m 3，盛有1000g的浓度为1wt.％的硫化钠溶液。
在电解槽5的自耗阳极4和阴极3之间设置可控硅直流电源，电压为1.4V，电流密度为200A/m 2，在直流电源的作用下，电解槽5内自耗阳极4上的铁原子失去电子变成亚铁离子，进入电解质溶液中，电解质溶液中的亚铁离子向阴极3迁移，亚铁离子在阴极3上得到电子成为铁原子，并沉积在阴极3上，获得高纯铁；在上述电化学反应过程中，所述电解质溶液处于流动状态：所述电解质溶液由电解槽5流至低位罐6，然后进入除杂罐8内，进行净化处理，得到净化电解质溶液；将所述净化电解质溶液输送至高位罐1内，再由高位罐1流至电解槽5内。
测试例
实施例1～3制备得到高纯铁的化学成分如表1所示；
表1实施例1～3的高纯铁的化学成分含量(质量含量)
  实施例1 实施例2 实施例3
C(％) 0.0017 0.0007 0.0021
Si(％) <0.005 0.0022 <0.01
Mn(％) <0.0005 0.0008 0.0005
P(％) <0.001 0.0008 <0.001
S(％) 0.0002 0.0069 0.0007
Cu(％) <0.0005 0.0005 0.0023
Cr(％) <0.0005 0.0012 0.0012
Ni(％) <0.005 0.0038 0.0048
Al(％) 0.0023 0.0074 0.0048
As(％) <0.00005 <0.0005 <0.0005
Co(％) 0.0015 0.0012 0.0005
Pb(％) <0.0001 0.0001 <0.0001
Zn(％) <0.0001 <0.0001 <0.0005
Fe(％) 99.992 99.956 99.985
实施例结果表明，采用本发明提供的装置能够得到纯度较高的高纯铁。
以上实施例的说明只是用于帮助理解本发明的方法及其核心思想。应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以对本发明进行若干改进和修饰，这些改进和修饰也落入本发明权利要求的保护范围内。对这些实施例的多种修改对本领域的专业技术人员来说是显而易见的，本文中所定义的一般原理可以在不脱离本发明的精神或范围的情况下在其它实施例中实现。因此，本发明将不会被限制于本文所示的这些实施例，而是要符合与本文所公开的原理和新颖特点相一致的最宽的范围。

Claims (14)

  1. 一种自耗阳极电解沉积制备高纯铁的装置，包括依次连通的高位罐(1)、电解槽(5)、低位罐(6)和除杂罐(8)，所述除杂罐的出水口(8-2)与所述高位罐的进水口(1-1)相连通；
    所述电解槽(5)的内部设置有自耗阳极(4)、阴极(3)以及设置在所述自耗阳极(4)和阴极(3)之间的离子渗透膜(10)。
  2. 根据权利要求1所述的装置，其特征在于，所述高位罐(1)的下表面高于所述电解槽(5)的上表面，所述电解槽(5)的下表面高于所述低位罐(6)的上表面。
  3. 根据权利要求1所述的装置，其特征在于，所述自耗阳极(4)为纯铁板；所述阴极(3)包括阴极板(3-1)和固定在所述阴极板(3-1)上的导电杆(3-2)。
  4. 根据权利要求1所述的装置，其特征在于，所述离子渗透膜(10)包裹在所述自耗阳极(4)周围；所述离子渗透膜(10)距离所述自耗阳极(4)表面的水平距离为1～10mm。
  5. 根据权利要求1或4所述的装置，其特征在于，所述离子渗透膜(10)的透气率为(30～60)L/m 2·s。
  6. 根据权利要求1所述的装置，其特征在于，还包括压滤机(9)，所述压滤机的进水口(9-1)与所述除杂罐的出水口(8-2)相连通，所述压滤机的出水口(9-2)与所述高位罐的进水口(1-1)相连通。
  7. 根据权利要求1所述的装置，其特征在于，所述除杂罐(8)的内部设置有搅拌装置(7)。
  8. 基于权利要求1～7任一项所述装置的高纯铁的制备方法，包括以下步骤：
    将自耗阳极(4)和阴极(3)置于电解质溶液中，在直流电源的作用下，发生电化学反应，铁原子沉积在阴极(3)表面，获得高纯铁；
    在上述电化学反应过程中，所述电解质溶液处于流动状态：所述电解质溶液由电解槽(5)流至低位罐(6)，然后进入除杂罐(8)内，进行净化处理，得到净化电解质溶液；所述除杂罐(8)内盛装有净化液；
    将所述净化电解质溶液输送至高位罐(1)内，再由高位罐(1)流至电解槽(5)内。
  9. 根据权利要求8所述的制备方法，其特征在于，所述直流电源的电压为0.7～3.0V，电流密度为100～500A/m 2。
  10. 根据权利要求8所述的制备方法，其特征在于，所述电解质溶液为硫酸亚铁溶液或氯化亚铁溶液；所述电解质溶液的初始浓度为28～112g/L。
  11. 根据权利要求8所述的制备方法，其特征在于，所述沉积后，还包括：将阴极(3)上沉积的铁依次进行分离、洗涤和干燥，得到高纯铁。
  12. 根据权利要求8所述的制备方法，其特征在于，所述净化液为硫化钠溶液。
  13. 根据权利要求12所述的制备方法，其特征在于，所述硫化钠溶液的质量浓度为0.5～1.5％。
  14. 根据权利要求8或12所述的制备方法，其特征在于，所述净化处理包括依次进行的搅拌净化和静置净化；所述搅拌净化的搅拌速率为30～120r/min，所述搅拌净化的时间≥30min；所述静置净化的时间为8～16h。
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