CN108505094A - A kind of chemical synthesizing method reducing electrode foil current-leakage - Google Patents

A kind of chemical synthesizing method reducing electrode foil current-leakage Download PDF

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Publication number
CN108505094A
CN108505094A CN201710102991.8A CN201710102991A CN108505094A CN 108505094 A CN108505094 A CN 108505094A CN 201710102991 A CN201710102991 A CN 201710102991A CN 108505094 A CN108505094 A CN 108505094A
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chemical conversion
paillon
solution
mass fraction
chemical
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CN108505094B (en
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余英凤
邓利松
袁姚
何凤荣
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YIDU DONGYANGGUANG FORMED FOIL CO Ltd
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YIDU DONGYANGGUANG FORMED FOIL CO Ltd
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/04Anodisation of aluminium or alloys based thereon
    • C25D11/06Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
    • C25D11/08Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing inorganic acids
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/04Anodisation of aluminium or alloys based thereon
    • C25D11/12Anodising more than once, e.g. in different baths
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G9/00Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/004Details
    • H01G9/04Electrodes or formation of dielectric layers thereon

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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)
  • Inorganic Chemistry (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Secondary Cells (AREA)

Abstract

The invention discloses a kind of chemical synthesizing methods reducing electrode foil current-leakage, including:Pre-treatment, multistage chemical conversion treatment, solution treatment, high-temperature process and phosphoric acid depolarising processing all use solution treatment again after preceding three-level chemical conversion treatment is per coagulation in the multistage chemical conversion treatment.The present invention is modified processing to hydrated alumina, aqua oxidation aluminium film is inhibited excessively to generate by being complexed using the aluminium ion of particular solution (complexometric reagent) processing and aqua oxidation aluminium film after the chemical conversion of preceding three-level;Applying electric current in acid condition simultaneously also promotes aqua oxidation aluminium film to be converted to dense porous pellumina, and the content of hydrated alumina is reduced in terms of two;It is had the following advantages compared with existing forming technology:The leakage current for reducing Waste Acid From Hua Cheng Foil improves the resistance to ripple current ability of electrode foil and extends the service life of capacitor.

Description

A kind of chemical synthesizing method reducing electrode foil current-leakage
Technical field
The invention belongs to electrode foil for aluminum electrolytic capacitors material manufacture technical field, more particularly to a kind of reduction electrode foil The chemical synthesizing method of leakage current.
Technical background
With the development that electronic equipment complete machine minimizes, volume-diminished and specific volume to aluminium electrolutic capacitor propose There is an urgent need to.Foil is anodizing to as the core material in aluminium electrolutic capacitor, decisive work is risen to the various characteristics of capacitor With.The existing chemical synthesis technology for being anodizing to foil is usually high-temperature heat treatment after boiling, level Four chemical conversion, after Pyatyi chemical conversion at phosphoric acid Reason carries out six grades of chemical conversions again, is melted into for seven grades after second of high-temperature heat treatment of progress, impregnation in last ammonium dihydrogen phosphate. The electrode foil being prepared using this chemical synthesis technology, after aluminium electrolutic capacitor is made, leakage current is larger, leads to resistance to ripple current Performance is poor so that capacitor service life is shorter.And one layer thicker of hydration oxygen is contained on the electrode foil surface after chemical conversion Change aluminium film, the leakage current of electrode foil, which is mainly further reacted by aqua oxidation aluminium film with water, generates unformed aluminium oxide or hydrogen Aluminium oxide, caused by oxidation film deterioration.Existing chemical synthesis technology is due to being carried out in aqueous solution, unavoidable aqua oxidation The generation of aluminium film.By high-temperature process, hydrated alumina also only has small part and converts, or passes through at conventional acid dip Reason can only also dissolve a part of hydrated alumina, and processing is too strong to cause specific volume decaying serious.At heat treatment and conventional acid Reason acts on very little to reducing electrode foil current-leakage.
Some to the very high field of capacitor reliability requirement for example flash lamp, energy-saving lamp, alternating current motor, servo motor, Charging pile etc., in addition to Fabrication of High Specific Capacitance, long-life, it is also necessary to have low-leakage current and low-loss characteristic.For such case, need pair Chemical synthesis technology is innovated, and is improved the quality of oxidation film and is reduced the leakage current of Waste Acid From Hua Cheng Foil, to meet corresponding requirements.
Invention content
The purpose of the present invention is being directed to existing issue, a kind of specific volume height is provided, low-loss is substantially reduced leakage current, extends The chemical synthesizing method of the mesohigh positive electrode foil of capacitor service life.
The purpose of the present invention is achieved through the following technical solutions:A kind of chemical synthesizing method reducing electrode foil current-leakage, packet It includes:Pre-treatment, multistage chemical conversion treatment, solution treatment, high-temperature process and phosphoric acid depolarising processing, in the multistage chemical conversion treatment before Solution treatment is all used again after the every coagulation of three-level chemical conversion treatment.
Specifically, a kind of chemical synthesizing method reducing electrode foil current-leakage, including:
A, etched foil is placed in 90~100 DEG C of pure water and handles;
B, the paillon after Pure water preparation in step A is placed in the boric acid acid solution of mass fraction 8%~15%, temperature control is extremely 70~90 DEG C of progress first order chemical conversions;
C, the paillon after first order chemical conversion in step B is impregnated in solution and carries out solution treatment;
D, the paillon after solution treatment in step C is placed in the boric acid acid solution of mass fraction 8%~15%, temperature control is extremely 70~90 DEG C of progress second level chemical conversions;
E, the paillon after second level chemical conversion in step D is impregnated in solution and carries out solution treatment;
F, the paillon after solution treatment in step E is placed in the boric acid acid solution of mass fraction 8%~15%, temperature control is extremely 70~90 DEG C of progress third level chemical conversions;
G, the paillon foil after third level chemical conversion in step F is impregnated in solution and carries out solution treatment;
H, the paillon after solution treatment in step G is placed in the boric acid acid solution of mass fraction 8%~15%, temperature control is extremely 70~90 DEG C of progress fourth stage chemical conversions;
I, by the paillon after fourth stage chemical conversion in step H, 400~550 DEG C of 1~5min of high-temperature process are placed in;
J, by step I high temperatures, treated that paillon is placed in the boric acid acid solution of mass fraction 8%~15%, and temperature control is extremely 70~90 DEG C of progress level V number chemical conversions;
K, the paillon after level V chemical conversion in step J is placed in 1~5% phosphoric acid solution, temperature control is to 40~60 DEG C, place Manage 2~5min;
L, by phosphoric acid solution in step K, treated that paillon is placed in the boric acid acid solution of mass fraction 8%~15%, control Temperature carries out the 6th grade to 70~90 DEG C and is melted into;
M, the paillon after the 6th grade of chemical conversion in step L is placed in 400~550 DEG C of 1~5min of high-temperature process;
N, by step M high temperatures, treated that paillon is placed in the boric acid acid solution of mass fraction 8%~15% carries out Seven grades of chemical conversions;
O, the paillon after the 7th grade of chemical conversion in step N is placed in ammonium dihydrogen phosphate and is handled.
In some embodiments, processing time is 6~10min in pure water in the step A.
In some embodiments, the first order to the 7th grade be melted into formation voltage range be respectively 100~200V, 300~400V, 400~500V, 500~600V, 500~600V, 500~600V and 500~600V.
In some embodiments, the chemical conversion time that the first order is melted into the 7th grade is 5~15min.
In some embodiments, solution is complexometric reagent solution in the solution treatment;Further, the complexing Reagent solution is selected from nitrilotriacetic acid, nitrilotriacetic acid trisodium salt, 8-hydroxyquinoline, triethanolamine, ethylenediamine tetra-acetic acid, second diammonium tetrem The aqueous solution of one or both of acid disodium.
In some embodiments, the mass fraction of the aqueous solution is 5%~20%.
In some embodiments, the solution treatment time in the step C, step E and step G is 5~15min;Place Reason voltage is 20~100V;Treatment temperature is 40~80 DEG C.
In some embodiments, the mass fraction of ammonium dihydrogen phosphate is 1%~5% in the step O;When processing Between be 2~5min.
The present invention passes through the aluminium using particular solution (complexometric reagent) processing and aqua oxidation aluminium film after the chemical conversion of preceding three-level Ion is complexed, and is modified processing to hydrated alumina, aqua oxidation aluminium film is inhibited excessively to generate;Simultaneously in acid condition Lower application electric current also promotes aqua oxidation aluminium film to be converted to dense porous pellumina, and containing for hydrated alumina is reduced in terms of two Amount;It is had the following advantages compared with existing forming technology:The leakage current for reducing Waste Acid From Hua Cheng Foil improves the resistance to ripple electricity of electrode foil Stream ability and the service life for extending capacitor.
Term defines
The invention is intended to cover all replacement, modification and equivalent technical solutions, they are included in as claim is fixed In the scope of the invention of justice.Those skilled in the art will appreciate that many and similar or equivalent method and material described herein It can be used in the practice present invention.The present invention is not limited to method described herein and material.In document, patent and the class combined One or more or contradict in the case of (include but not limited to defined in term, terms different from the application like material Using, described technology etc.), it is subject to the application.
It will further be appreciated that certain features of the present invention, are clearly visible, are carried out in multiple independent embodiments Description, but can also in combination be provided in single embodiment.Conversely, the various features of the present invention, for brevity, It is described, but can also be provided individually or with any appropriate sub-portfolio in single embodiment.
Unless otherwise stated, all scientific and technical terminologies used in the present invention have with those skilled in the art of the invention's It is generally understood identical meaning.All patents of the present invention and public publication are integrally incorporated this hair by reference It is bright.
Term "comprising" or " comprising " are open language, that is, include the content specified by the present invention, but it is not precluded Content in terms of him.
Unless explicitly stated otherwise in contrast, otherwise, temperature of the present invention is value range.For example, " 85 DEG C " expressions Ranging from 85 DEG C ± 5 DEG C of temperature.
Specific implementation mode
As described below is the preferred embodiment of the present invention, and what the present invention was protected is not limited to following preferred implementation side Formula.It should be pointed out that for those skilled in the art on the basis of this innovation and creation conceive, several deformations for making with It improves, belongs to protection scope of the present invention.Raw material used in embodiment can be obtained by commercial sources.
Embodiment 1
A, etched foil is placed in 90~100 DEG C of pure water and handles 10min;
B, the paillon after Pure water preparation in step A is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into The row first order is melted into, formation voltage 150V, and the chemical conversion time is 12min;
C, the paillon after first order chemical conversion in step B is impregnated in the nitrilotriacetic acid aqueous solution that mass fraction is 5% Reason, processing voltage are 50V, and processing time 5min, temperature is 40 DEG C;
D, the paillon after solution treatment in step C is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into The row second level is melted into, formation voltage 320V, and the chemical conversion time is 12min;
E, the paillon after second level chemical conversion in step D is impregnated in the nitrilotriacetic acid aqueous solution that mass fraction is 5% Reason, processing voltage are 50V, and processing time 5min, temperature is 40 DEG C;
F, the paillon after solution treatment in step E is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into The row third level is melted into, formation voltage 470V, and the chemical conversion time is 12min;
G, the paillon foil after third level chemical conversion in step F is impregnated in the nitrilotriacetic acid aqueous solution that mass fraction is 5% Processing, processing voltage are 50V, and processing time 5min, temperature is 40 DEG C;
H, the paillon after solution treatment in step G is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into The row fourth stage is melted into, formation voltage 580V, and the chemical conversion time is 12min;
I, by the paillon after fourth stage chemical conversion in step H, 550 DEG C of high-temperature process 2min are placed in;
J, by step I high temperatures, treated that paillon is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into Row level V number is melted into, formation voltage 580V, and the chemical conversion time is 12min;
K, the paillon after level V chemical conversion in step J is placed in 2% phosphoric acid solution, temperature control handles 2min to 50 DEG C;
L, by phosphoric acid solution in step K, treated that paillon is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C carry out level V number chemical conversion, formation voltage 580V, the chemical conversion time be 12min;
M, the paillon after the 6th grade of chemical conversion in step L is placed in 550 DEG C of high-temperature process 2min;
N, by step M high temperatures treated paillon is placed in the boric acid acid solution of mass fraction 8% temperature control to 85 DEG C into Seven series of row is melted into, formation voltage 580V, and the chemical conversion time is 12min;
O, the paillon after the 7th grade of chemical conversion in step N is placed in 2% ammonium dihydrogen phosphate and handles 2min.
Gained Waste Acid From Hua Cheng Foil performance is tested, the results are shown in Table 1.
Embodiment 2
A, etched foil is placed in 90~100 DEG C of pure water and handles 10min;
B, the paillon after Pure water preparation in step A is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into The row first order is melted into, formation voltage 150V, and the chemical conversion time is 12min;
C, the paillon after first order chemical conversion in step B is impregnated in the 8-hydroxyquinoline aqueous solution that mass fraction is 8% Processing, processing voltage are 50V, and processing time 10min, temperature is 60 DEG C;
D, the paillon after solution treatment in step C is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into The row second level is melted into, formation voltage 320V, and the chemical conversion time is 12min;
E, the paillon after second level chemical conversion in step D is impregnated in the 8-hydroxyquinoline aqueous solution that mass fraction is 8% Processing, processing voltage are 50V, and processing time 10min, temperature is 60 DEG C;
F, the paillon after solution treatment in step E is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into The row third level is melted into, formation voltage 470V, and the chemical conversion time is 12min;
G, the paillon foil after third level chemical conversion in step F is impregnated in the 8-hydroxyquinoline aqueous solution that mass fraction is 8% Middle processing, processing voltage are 50V, and processing time 10min, temperature is 60 DEG C;
H, the paillon after solution treatment in step G is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into The row fourth stage is melted into, formation voltage 580V, and the chemical conversion time is 12min;
I, by the paillon after fourth stage chemical conversion in step H, 550 DEG C of high-temperature process 2min are placed in;
J, by step I high temperatures, treated that paillon is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into Row level V number is melted into, formation voltage 580V, and the chemical conversion time is 12min;
K, the paillon after level V chemical conversion in step J is placed in 2% phosphoric acid solution, temperature control handles 2min to 50 DEG C;
L, by phosphoric acid solution in step K, treated that paillon is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C carry out level V number chemical conversion, formation voltage 580V, the chemical conversion time be 12min;
M, the paillon after the 6th grade of chemical conversion in step L is placed in 550 DEG C of high-temperature process 2min;
N, by step M high temperatures treated paillon is placed in the boric acid acid solution of mass fraction 8% temperature control to 85 DEG C into Seven series of row is melted into, formation voltage 580V, and the chemical conversion time is 12min;
O, the paillon after the 7th grade of chemical conversion in step N is placed in 2% ammonium dihydrogen phosphate and handles 2min.
Gained Waste Acid From Hua Cheng Foil performance is tested, the results are shown in Table 1.
Embodiment 3
A, etched foil is placed in 90~100 DEG C of pure water and handles 10min;
B, the paillon after Pure water preparation in step A is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into The row first order is melted into, formation voltage 150V, and the chemical conversion time is 12min;
C, the paillon after first order chemical conversion in step B is impregnated in the edta solution that mass fraction is 10% Middle processing, processing voltage are 60V, and processing time 10min, temperature is 80 DEG C;
D, the paillon after solution treatment in step C is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into The row second level is melted into, formation voltage 320V, and the chemical conversion time is 12min;
E, the paillon after second level chemical conversion in step D is impregnated in the edta solution that mass fraction is 10% Middle processing, processing voltage are 60V, and processing time 10min, temperature is 80 DEG C;
F, the paillon after solution treatment in step E is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into The row third level is melted into, formation voltage 470V, and the chemical conversion time is 12min;
G, it is water-soluble that the paillon foil after being melted into the third level in step F is impregnated in the ethylenediamine tetra-acetic acid that mass fraction is 10% It is handled in liquid, processing voltage is 60V, and processing time 10min, temperature is 80 DEG C;
H, the paillon after solution treatment in step G is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into The row fourth stage is melted into, formation voltage 580V, and the chemical conversion time is 12min;
I, by the paillon after fourth stage chemical conversion in step H, 550 DEG C of high-temperature process 2min are placed in;
J, by step I high temperatures, treated that paillon is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into Row level V number is melted into, formation voltage 580V, and the chemical conversion time is 12min;
K, the paillon after level V chemical conversion in step J is placed in 2% phosphoric acid solution, temperature control handles 2min to 50 DEG C;
L, by phosphoric acid solution in step K, treated that paillon is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C carry out level V number chemical conversion, formation voltage 580V, the chemical conversion time be 12min;
M, the paillon after the 6th grade of chemical conversion in step L is placed in 550 DEG C of high-temperature process 2min;
N, by step M high temperatures treated paillon is placed in the boric acid acid solution of mass fraction 8% temperature control to 85 DEG C into Seven series of row is melted into, formation voltage 580V, and the chemical conversion time is 12min;
O, the paillon after the 7th grade of chemical conversion in step N is placed in 2% ammonium dihydrogen phosphate and handles 2min.
Gained Waste Acid From Hua Cheng Foil performance is tested, the results are shown in Table 1.
Embodiment 4
A, etched foil is placed in 90~100 DEG C of pure water and handles 10min;
B, the paillon after Pure water preparation in step A is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into The row first order is melted into, formation voltage 150V, and the chemical conversion time is 12min;
C, it is 5% nitrilotriacetic acid and 5% ammonia three paillon after first order chemical conversion in step B to be impregnated in mass fraction It is handled in the mixed solution of acetic acid trisodium, processing voltage is 60V, and processing time 10min, temperature is 80 DEG C;
D, the paillon after solution treatment in step C is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into The row second level is melted into, formation voltage 320V, and the chemical conversion time is 12min;
E, it is 5% nitrilotriacetic acid and 5% ammonia three paillon after second level chemical conversion in step D to be impregnated in mass fraction It is handled in the mixed solution of acetic acid trisodium, processing voltage is 60V, and processing time 10min, temperature is 80 DEG C;
F, the paillon after solution treatment in step E is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into The row third level is melted into, formation voltage 470V, and the chemical conversion time is 12min;
G, it is 5% nitrilotriacetic acid and 5% ammonia the paillon foil after third level chemical conversion in step F to be impregnated in mass fraction It is handled in the mixed solution of triacetic acid trisodium, processing voltage is 60V, and processing time 10min, temperature is 80 DEG C;
H, the paillon after solution treatment in step G is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into The row fourth stage is melted into, formation voltage 580V, and the chemical conversion time is 12min;
I, by the paillon after fourth stage chemical conversion in step H, 550 DEG C of high-temperature process 2min are placed in;
J, by step I high temperatures, treated that paillon is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into Row level V number is melted into, formation voltage 580V, and the chemical conversion time is 12min;
K, the paillon after level V chemical conversion in step J is placed in 2% phosphoric acid solution, temperature control handles 2min to 50 DEG C;
L, by phosphoric acid solution in step K, treated that paillon is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C carry out level V number chemical conversion, formation voltage 580V, the chemical conversion time be 12min;
M, the paillon after the 6th grade of chemical conversion in step L is placed in 550 DEG C of high-temperature process 2min;
N, by step M high temperatures treated paillon is placed in the boric acid acid solution of mass fraction 8% temperature control to 85 DEG C into Seven series of row is melted into, formation voltage 580V, and the chemical conversion time is 12min;
O, the paillon after the 7th grade of chemical conversion in step N is placed in 2% ammonium dihydrogen phosphate and handles 2min.
Gained Waste Acid From Hua Cheng Foil performance is tested, the results are shown in Table 1.
Embodiment 5
A, etched foil is placed in 90~100 DEG C of pure water and handles 10min;
B, the paillon after Pure water preparation in step A is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into The row first order is melted into, formation voltage 150V, and the chemical conversion time is 12min;
C, the paillon after first order chemical conversion in step B is impregnated in the triethanolamine aqueous solution that mass fraction is 15% Reason, processing voltage are 80V, and processing time 10min, temperature is 40 DEG C;
D, the paillon after solution treatment in step C is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into The row second level is melted into, formation voltage 320V, and the chemical conversion time is 12min;
E, the paillon after second level chemical conversion in step D is impregnated in the triethanolamine aqueous solution that mass fraction is 15% Reason, processing voltage are 80V, and processing time 10min, temperature is 40 DEG C;
F, the paillon after solution treatment in step E is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into The row third level is melted into, formation voltage 470V, and the chemical conversion time is 12min;
G, the paillon foil after third level chemical conversion in step F is impregnated in the triethanolamine aqueous solution that mass fraction is 15% Processing, processing voltage are 80V, and processing time 10min, temperature is 40 DEG C;
H, the paillon after solution treatment in step G is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into The row fourth stage is melted into, formation voltage 580V, and the chemical conversion time is 12min;
I, by the paillon after fourth stage chemical conversion in step H, 550 DEG C of high-temperature process 2min are placed in;
J, by step I high temperatures, treated that paillon is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into Row level V number is melted into, formation voltage 580V, and the chemical conversion time is 12min;
K, the paillon after level V chemical conversion in step J is placed in 2% phosphoric acid solution, temperature control handles 2min to 50 DEG C;
L, by phosphoric acid solution in step K, treated that paillon is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C carry out level V number chemical conversion, formation voltage 580V, the chemical conversion time be 12min;
M, the paillon after the 6th grade of chemical conversion in step L is placed in 550 DEG C of high-temperature process 2min;
N, by step M high temperatures treated paillon is placed in the boric acid acid solution of mass fraction 8% temperature control to 85 DEG C into Seven series of row is melted into, formation voltage 580V, and the chemical conversion time is 12min;
O, the paillon after the 7th grade of chemical conversion in step N is placed in 2% ammonium dihydrogen phosphate and handles 2min.
Gained Waste Acid From Hua Cheng Foil performance is tested, the results are shown in Table 1.
Embodiment 6
A, etched foil is placed in 90~100 DEG C of pure water and handles 10min;
B, the paillon after Pure water preparation in step A is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into The row first order is melted into, formation voltage 150V, and the chemical conversion time is 12min;
C, the paillon after first order chemical conversion in step B is impregnated in the ethylenediamine tetra-acetic acid and 5% that mass fraction is 15% Disodium ethylene diamine tetraacetate mixed solution in handle, processing voltage be 80V, processing time 15min, temperature be 50 DEG C;
D, the paillon after solution treatment in step C is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into The row second level is melted into, formation voltage 320V, and the chemical conversion time is 12min;
E, the paillon after second level chemical conversion in step D is impregnated in the ethylenediamine tetra-acetic acid and 5% that mass fraction is 15% Disodium ethylene diamine tetraacetate mixed solution in handle, processing voltage be 80V, processing time 15min, temperature be 50 DEG C;
F, the paillon after solution treatment in step E is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into The row third level is melted into, formation voltage 470V, and the chemical conversion time is 12min;
G, by step F the third level chemical conversion after paillon foil be impregnated in mass fraction be 15% ethylenediamine tetra-acetic acid and It is handled in 5% disodium ethylene diamine tetraacetate mixed solution, processing voltage is 80V, and processing time 15min, temperature is 50 DEG C;
H, the paillon after solution treatment in step G is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into The row fourth stage is melted into, formation voltage 580V, and the chemical conversion time is 12min;
I, by the paillon after fourth stage chemical conversion in step H, 550 DEG C of high-temperature process 2min are placed in;
J, by step I high temperatures, treated that paillon is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into Row level V number is melted into, formation voltage 580V, and the chemical conversion time is 12min;
K, the paillon after level V chemical conversion in step J is placed in 2% phosphoric acid solution, temperature control handles 2min to 50 DEG C;
L, by phosphoric acid solution in step K, treated that paillon is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C carry out level V number chemical conversion, formation voltage 580V, the chemical conversion time be 12min;
M, the paillon after the 6th grade of chemical conversion in step L is placed in 550 DEG C of high-temperature process 2min;
N, by step M high temperatures treated paillon is placed in the boric acid acid solution of mass fraction 8% temperature control to 85 DEG C into Seven series of row is melted into, formation voltage 580V, and the chemical conversion time is 12min;
O, the paillon after the 7th grade of chemical conversion in step N is placed in 2% ammonium dihydrogen phosphate and handles 2min.
Gained Waste Acid From Hua Cheng Foil performance is tested, the results are shown in Table 1.
Comparative example 1
A, etched foil is placed in 90~100 DEG C of pure water and handles 10min;
B, the paillon after Pure water preparation in step A is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into The row first order is melted into, formation voltage 150V, and the chemical conversion time is 12min;
C, the paillon after first order chemical conversion in step B is impregnated in the nitrilotriacetic acid aqueous solution that mass fraction is 5% Reason, processing voltage are 50V, and processing time 5min, temperature is 40 DEG C;
D, the paillon after solution treatment in step C is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into The row second level is melted into, formation voltage 320V, and the chemical conversion time is 12min;
E, the paillon after second level chemical conversion treatment in step D is placed in the boric acid acid solution of mass fraction 8%, temperature control is extremely 85 DEG C of progress third level chemical conversions, formation voltage 470V, chemical conversion time are 12min;
F, the paillon after third level chemical conversion in step E is placed in the boric acid acid solution of mass fraction 8%, temperature control is to 85 DEG C Fourth stage chemical conversion, formation voltage 580V are carried out, the chemical conversion time is 12min;
G, by the paillon after fourth stage chemical conversion in step F, 550 DEG C of high-temperature process 2min are placed in;
H, by step G high temperatures, treated that paillon is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into Row level V number is melted into, formation voltage 580V, and the chemical conversion time is 12min;
I, the paillon after level V chemical conversion in step H is placed in 2% phosphoric acid solution, temperature control handles 2min to 50 DEG C;
J, by phosphoric acid solution in step I, treated that paillon is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C carry out level V number chemical conversion, formation voltage 580V, the chemical conversion time be 12min;
K, the paillon after the 6th grade of chemical conversion in step J is placed in 550 DEG C of high-temperature process 2min;
L, by step K high temperatures treated paillon is placed in the boric acid acid solution of mass fraction 8% temperature control to 85 DEG C into Seven series of row is melted into, formation voltage 580V, and the chemical conversion time is 12min;
M, the paillon after the 7th grade of chemical conversion in step L is placed in 2% ammonium dihydrogen phosphate and handles 2min.
Gained Waste Acid From Hua Cheng Foil performance is tested, the results are shown in Table 1.
Comparative example 2
A, etched foil is placed in 90~100 DEG C of pure water and handles 10min;
B, the paillon after Pure water preparation in step A is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into The row first order is melted into, formation voltage 150V, and the chemical conversion time is 12min;
C, it is 5% nitrilotriacetic acid and 5% ammonia three paillon after first order chemical conversion in step B to be impregnated in mass fraction It is handled in acetic acid trisodium mixed solution, processing voltage is 60V, and processing time 10min, temperature is 80 DEG C;
D, the paillon after solution treatment in step C is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into The row second level is melted into, formation voltage 320V, and the chemical conversion time is 12min;
E, it is 5% nitrilotriacetic acid and 5% ammonia three paillon after second level chemical conversion in step D to be impregnated in mass fraction It is handled in acetic acid trisodium mixed solution, processing voltage is 60V, and processing time 10min, temperature is 80 DEG C;
F, the paillon after solution treatment in step E is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into The row third level is melted into, formation voltage 470V, and the chemical conversion time is 12min;
G, the paillon after third level chemical conversion treatment in step F is placed in the boric acid acid solution of mass fraction 8%, temperature control is extremely 85 DEG C of progress fourth stage chemical conversions, formation voltage 580V, chemical conversion time are 12min;
H, by the paillon after fourth stage chemical conversion in step G, 550 DEG C of high-temperature process 2min are placed in;
I, by step H high temperatures, treated that paillon is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into Row level V number is melted into, formation voltage 580V, and the chemical conversion time is 12min;
J, the paillon after level V chemical conversion in step I is placed in 2% phosphoric acid solution, temperature control handles 2min to 50 DEG C;
K, by phosphoric acid solution in step J, treated that paillon is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C carry out level V number chemical conversion, formation voltage 580V, the chemical conversion time be 12min;
L, the paillon after the 6th grade of chemical conversion in step K is placed in 550 DEG C of high-temperature process 2min;
M, by step L high temperatures treated paillon is placed in the boric acid acid solution of mass fraction 8% temperature control to 85 DEG C into Seven series of row is melted into, formation voltage 580V, and the chemical conversion time is 12min;
N, the paillon after the 7th grade of chemical conversion in step M is placed in 2% ammonium dihydrogen phosphate and handles 2min.
Gained Waste Acid From Hua Cheng Foil performance is tested, the results are shown in Table 1.
Comparative example 3
A, etched foil is placed in 90~100 DEG C of pure water and handles 10min;
B, the paillon after Pure water preparation in step A is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into The row first order is melted into, formation voltage 150V, and the chemical conversion time is 12min;
C, the paillon after first order chemical conversion in step B is impregnated in the ethylenediamine tetra-acetic acid and 5% that mass fraction is 15% Disodium ethylene diamine tetraacetate mixed solution in handle, processing voltage be 80V, processing time 10min, temperature be 40 DEG C;
D, the paillon after solution treatment in step C is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into The row second level is melted into, formation voltage 320V, and the chemical conversion time is 12min;
E, the paillon after second level chemical conversion treatment in step D is placed in the boric acid acid solution of mass fraction 8%, temperature control is extremely 85 DEG C of progress third level chemical conversions, formation voltage 470V, chemical conversion time are 12min;
F, by step E the third level chemical conversion after paillon foil be impregnated in mass fraction be 15% ethylenediamine tetra-acetic acid and It is handled in 5% disodium ethylene diamine tetraacetate mixed solution, processing voltage is 80V, and processing time 10min, temperature is 40 DEG C;
G, the paillon after solution treatment in step F is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into The row fourth stage is melted into, formation voltage 580V, and the chemical conversion time is 12min;
H, by the paillon after fourth stage chemical conversion in step G, 550 DEG C of high-temperature process 2min are placed in;
I, by step H high temperatures, treated that paillon is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into Row level V number is melted into, formation voltage 580V, and the chemical conversion time is 12min;
J, the paillon after level V chemical conversion in step I is placed in 2% phosphoric acid solution, temperature control handles 2min to 50 DEG C;
K, by phosphoric acid solution in step J, treated that paillon is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C carry out level V number chemical conversion, formation voltage 580V, the chemical conversion time be 12min;
L, the paillon after the 6th grade of chemical conversion in step K is placed in 550 DEG C of high-temperature process 2min;
M, by step L high temperatures treated paillon is placed in the boric acid acid solution of mass fraction 8% temperature control to 85 DEG C into Seven series of row is melted into, formation voltage 580V, and the chemical conversion time is 12min;
N, the paillon after the 7th grade of chemical conversion in step M is placed in 2% ammonium dihydrogen phosphate and handles 2min.
Gained Waste Acid From Hua Cheng Foil performance is tested, the results are shown in Table 1.
Comparative example 4
A, etched foil is placed in 90~100 DEG C of pure water and handles 10min;
B, the paillon after Pure water preparation in step A is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into The row first order is melted into, formation voltage 150V, and the chemical conversion time is 12min;
C, the paillon after first order chemical conversion treatment in step B is placed in the boric acid acid solution of mass fraction 8%, temperature control is extremely 85 DEG C of progress second level chemical conversions, formation voltage 320V, chemical conversion time are 12min;
D, the paillon after second level chemical conversion treatment in step C is placed in the boric acid acid solution of mass fraction 8%, temperature control is extremely 85 DEG C of progress third level chemical conversions, formation voltage 470V, chemical conversion time are 12min;
E, the paillon after third level chemical conversion treatment in step D is placed in the boric acid acid solution of mass fraction 8%, temperature control is extremely 85 DEG C of progress fourth stage chemical conversions, formation voltage 580V, chemical conversion time are 12min;
F, by the paillon after fourth stage chemical conversion in step E, 550 DEG C of high-temperature process 2min are placed in;
G, by step F high temperatures, treated that paillon is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C into Row level V number is melted into, formation voltage 580V, and the chemical conversion time is 12min;
H, the paillon after level V chemical conversion in step G is placed in 2% phosphoric acid solution, temperature control handles 2min to 50 DEG C;
I, by phosphoric acid solution in step H, treated that paillon is placed in the boric acid acid solution of mass fraction 8%, temperature control to 85 DEG C carry out level V number chemical conversion, formation voltage 580V, the chemical conversion time be 12min;
J, the paillon after the 6th grade of chemical conversion in step I is placed in 550 DEG C of high-temperature process 2min;
K, by step J high temperatures treated paillon is placed in the boric acid acid solution of mass fraction 8% temperature control to 85 DEG C into Seven series of row is melted into, formation voltage 580V, and the chemical conversion time is 12min;
L, the paillon after the 7th grade of chemical conversion in step K is placed in 2% ammonium dihydrogen phosphate and handles 2min.
Gained Waste Acid From Hua Cheng Foil performance is tested, the results are shown in Table 1.
The performance test results
1 the performance test results of table
As can be seen from the table, the paillon performance for implementing solution treatment three times in preceding three-level chemical conversion is superior to implementation one Secondary and solution treatment twice paillon.In the case where 600V reaches voltage, Waste Acid From Hua Cheng Foil prepared by the embodiment of the present invention is than common chemical conversion work The Waste Acid From Hua Cheng Foil specific volume that skill is prepared is higher by 4% or more, and leakage current reduces by 8% or more, and loss and boiling pressure rising time are superior to Common Waste Acid From Hua Cheng Foil.

Claims (10)

1. a kind of chemical synthesizing method reducing electrode foil current-leakage, including:Pre-treatment, multistage chemical conversion treatment, solution treatment, at high temperature Reason and phosphoric acid depolarising processing, which is characterized in that after preceding three-level chemical conversion treatment is per coagulation in the multistage chemical conversion treatment all Solution treatment is used again.
2. the chemical synthesizing method according to claim 1 for reducing electrode foil current-leakage, which is characterized in that including:
A, etched foil is placed in 90~100 DEG C of pure water and handles;
B, the paillon after Pure water preparation in step A is placed in the boric acid acid solution of mass fraction 8%~15%, temperature control to 70~ 90 DEG C of progress first order chemical conversions;
C, the paillon after first order chemical conversion in step B is impregnated in solution and carries out solution treatment;
D, the paillon after solution treatment in step C is placed in the boric acid acid solution of mass fraction 8%~15%, temperature control to 70~ 90 DEG C of progress second level chemical conversions;
E, the paillon after second level chemical conversion in step D is impregnated in solution and carries out solution treatment;
F, the paillon after solution treatment in step E is placed in the boric acid acid solution of mass fraction 8%~15%, temperature control to 70~ 90 DEG C of progress third level chemical conversions;
G, the paillon foil after third level chemical conversion in step F is impregnated in solution and carries out solution treatment;
H, the paillon after solution treatment in step G is placed in the boric acid acid solution of mass fraction 8%~15%, temperature control to 70~ 90 DEG C of progress fourth stage chemical conversions;
I, by the paillon after fourth stage chemical conversion in step H, 400~550 DEG C of 1~5min of high-temperature process are placed in;
J, by step I high temperatures, treated that paillon is placed in the boric acid acid solution of mass fraction 8%~15%, and temperature control to 70~ 90 DEG C of progress level V number chemical conversions;
K, the paillon after level V chemical conversion in step J is placed in 1~5% phosphoric acid solution, temperature control is to 40~60 DEG C, processing 2 ~5min;
L, by phosphoric acid solution in step K, treated that paillon is placed in the boric acid acid solution of mass fraction 8%~15%, and temperature control is extremely 70~90 DEG C carry out the 6th grade of chemical conversion;
M, the paillon after the 6th grade of chemical conversion in step L is placed in 400~550 DEG C of 1~5min of high-temperature process;
N, by step M high temperatures, treated that paillon is placed in that the 7th grade is carried out in the boric acid acid solution of mass fraction 8%~15% Chemical conversion;
O, the paillon after the 7th grade of chemical conversion in step N is placed in ammonium dihydrogen phosphate and is handled.
3. the chemical synthesizing method according to claim 2 for reducing electrode foil current-leakage, which is characterized in that pure in the step A Processing time is 6~10min in water.
4. the chemical synthesizing method according to claim 2 for reducing electrode foil current-leakage, which is characterized in that the first order to the Seven grades chemical conversion formation voltage ranges be respectively 100~200V, 300~400V, 400~500V, 500~600V, 500~ 600V, 500~600V and 500~600V.
5. the chemical synthesizing method according to claim 2 for reducing electrode foil current-leakage, which is characterized in that the first order to the The chemical conversion time of seven grades of chemical conversions is 5~15min.
6. the chemical synthesizing method according to claim 1 or 2 for reducing electrode foil current-leakage, which is characterized in that at the solution The solution of reason is complexometric reagent solution.
7. the chemical synthesizing method according to claim 6 for reducing electrode foil current-leakage, which is characterized in that the complexometric reagent is molten Liquid is selected from nitrilotriacetic acid, nitrilotriacetic acid trisodium salt, 8-hydroxyquinoline, triethanolamine, ethylenediamine tetra-acetic acid, b diammonium disodium edta One or both of aqueous solution.
8. the chemical synthesizing method according to claim 7 for reducing electrode foil current-leakage, which is characterized in that the complexometric reagent is molten The mass fraction of solute is 5%~20% in liquid.
9. the chemical synthesizing method according to claim 2 for reducing electrode foil current-leakage, which is characterized in that the step C, step The solution treatment time in E and step G is 5~15min;Processing voltage is 20~100V;Treatment temperature is 40~80 DEG C.
10. the chemical synthesizing method according to claim 2 for reducing electrode foil current-leakage, which is characterized in that phosphorus in the step O The mass fraction of acid dihydride ammonium salt solution is 1%~5%;Processing time is 2~5min.
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