CN1099907A - Active lead dioxide electrode and preparing method and use - Google Patents
Active lead dioxide electrode and preparing method and use Download PDFInfo
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- CN1099907A CN1099907A CN93116984A CN93116984A CN1099907A CN 1099907 A CN1099907 A CN 1099907A CN 93116984 A CN93116984 A CN 93116984A CN 93116984 A CN93116984 A CN 93116984A CN 1099907 A CN1099907 A CN 1099907A
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- lead dioxide
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- 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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The said lead dioxide electrode uses titanium plate as carrier, and after the titanium plate is acid-etched and coated with the mixed coating liquid of 20% alkoxy tin butanol solution and 20% antimony trichloride-butanol solution, a very thin intermediate layer of tin and antimony oxide is formed by thermo-oxidation under 450 deg.C with a layer thickness of 1-3 micron m, and then it used as anode has a beta-PbO2 layer with a thickness of 0.013-015 mm electrically deposited in electroplating solution system of lead nitrate, nitric acid and sodium fluoride; and the said electrode used as anode is employed in production technology for boric acid by use of diaphragm electrolysis process.
Description
The present invention relates to a kind of active lead dioxide electrode and its production and use.
Lead dioxide electrode has excellent conducting performance, and therefore for a long time, people put forth effort research always, to seek to use it for industrial approach.Brown lead oxide was with β-PbO in the past
2The form electro-deposition on nonmetallic surfaces such as graphite, carbon, pottery or make lead dioxide electrode on the metal surfaces such as platinum, tantalum, but with the electrode of these methods preparations because brown lead oxide electrodeposited coating porous, uneven coating are even, poor adhesive force etc. usually becomes unstable in electrochemical process.Until working out ti-supported lead dioxide electric pole, the electrolysis process that just begins to use it for electrolysis production chlorate and expand oxygenatedchemicalss such as chlorate, perchlorate to is obtained bigger progress.But how to prepare the lead dioxide electrode of tool active intermediate and adopt electrolysis to produce boric acid technology as anode it and still do not have reported in literature.
Purpose of the present invention provides simple, cheap active lead dioxide electrode of a kind of tool active intermediate, preparation method and its production and use, when this electrode was produced anode in the boric acid technology as electrolysis, the anode oxygen evolution potential was low, the electrolytic process working voltage is low, electrode electro Chemical stable performance, anodic current efficiency height.
Purpose of the present invention can realize by following measure:
A kind of active lead dioxide electrode is to be carrier with the titanium plate; At area is 0.1-0.8 square metre, thick in the active tin of one deck, sb oxide intermediate layer are arranged on the titanium plate of 1-2 millimeter, and the thickness in this intermediate layer is the 1-3 micron; Power in the intermediate layer and to deposit β-PbO that thickness is the 0.013-0.15 millimeter
2Layer.
A kind of preparation method of active lead dioxide be with the titanium plate behind acid etching, mixture masking liquid with 20% alkoxyl tin butanols liquid and 20% trichloride antimony butanols liquid applies 1-3 time again, behind hot blast drying, 450 ℃ of following thermal oxidations 1 hour, form the active tin-antimony oxide layer of a thin layer, the water flush away is floating thing, airing, again 450 ℃ of following thermal oxidation half an hour; Then with it as anode, in plumbi nitras, nitric acid, sodium fluoride electroplate liquid system, electro-deposition skim β-PbO
2, promptly made active ti-supported lead dioxide electric pole.
A kind of purposes of active lead dioxide electrode is that this electrode is made anode, is used for diaphragm process and produces boric acid technology; During electrolysis, anodic current density is 250A/m
8-800A/m
8, electrolysis run channel voltage is 3.0-5.5V.
Purpose of the present invention also can realize by following measure:
The masking liquid alkoxyl tin butanols liquid among the preparation method of described active lead dioxide electrode and the volume ratio of trichloride antimony butanols liquid are (2.5~3.5): 1; Plumbi nitras is that 160~200g/l, nitric acid are that 5-15ml/l, sodium fluoride are 0.5-2g/l in the electroplate liquid of preparation lead dioxide electrode, and the anodic current density of electro-deposition is 1-12A/dm
2, electroplating temperature is that 80-90 ℃, electroplating time are that 1-15 minute, cathode material are stainless steel.
The present invention has following advantage compared to existing technology:
1, the present invention provides the ti-supported lead dioxide electric base metal electrode of a kind of tool tin, antimony activating oxide bottom first, and it is used for diaphragm process production boric acid technology first.
2, electrode preparation method of the present invention is simple, electrode is cheap.
3, active lead dioxide electrode of the present invention is produced when making anode in the boric acid technology in electrolysis, and the anode oxygen evolution potential is low, the stable performance of electrode electrode electro Chemical, corrosion resistance and good, can satisfy the requirement in industrial production antianode life-span; And low, the anodic current efficiency of run channel voltage is up to more than 90% in electrolytic process, thereby boron, alkali yield height, boric acid product purity height, energy consumption are low.
The present invention also will be described in further detail in conjunction with the embodiments:
Embodiment one:
A kind of active lead dioxide electrode is to be carrier with the titanium plate; Area be 0.1 square metre, thick be that the active tin of one deck, sb oxide intermediate layer are arranged on 1 millimeter the titanium plate, the thickness in this intermediate layer is 1 micron; Powering in the intermediate layer and depositing thickness is β-PbO of 0.15 millimeter
2Layer.
The preparation method of active lead dioxide electrode be with the titanium plate behind acid etching, mixture masking liquid with 20% alkoxyl tin butanols liquid and 20% trichloride antimony butanols liquid applies 1 time again, behind hot blast drying, 450 ℃ of following thermal oxidations 1 hour, form the active tin-antimony oxide layer of a thin layer, the water flush away is floating thing, airing, again 450 ℃ of following thermal oxidation half an hour; Then with it as anode, in plumbi nitras, nitric acid, sodium fluoride electroplate liquid system, electro-deposition skim β-PbO
2, promptly made active ti-supported lead dioxide electric pole; The volume ratio of described masking liquid alkoxyl tin butanols liquid and trichloride antimony butanols liquid is 2.5: 1; Plumbi nitras is that 160g/l, nitric acid are that 5ml/l, sodium fluoride are 0.5g/l in the electroplate liquid of preparation lead dioxide electrode, and the anodic current density of electro-deposition is 12A/dm
2, electroplating temperature is that 80 ℃, electroplating time are that 15 minutes, cathode material are stainless steel.
The purposes of described active lead dioxide electrode is that this electrode is made anode, is used for diaphragm process and produces boric acid technology; During electrolysis, anodic current density is 250A/m
2, electrolysis run channel voltage is 3.0V.
Embodiment two:
A kind of active lead dioxide electrode is to be carrier with the titanium plate; Area be 0.8 square metre, thick be that the active tin of one deck, sb oxide intermediate layer are arranged on 2 millimeters the titanium plate, the thickness in this intermediate layer is 3 microns; Powering in the intermediate layer and depositing thickness is β-PbO of 0.04 millimeter
2Layer.
Its preparation method be with the titanium plate behind acid etching, mixture masking liquid with 20% alkoxyl tin butanols liquid and 20% trichloride antimony butanols liquid applies 3 times again, behind hot blast drying, 450 ℃ of following thermal oxidations 1 hour, form the active tin-antimony oxide layer of a thin layer, the water flush away is floating thing, airing, again 450 ℃ of following thermal oxidation half an hour; Then with it as anode, in plumbi nitras, nitric acid, sodium fluoride electroplate liquid system, electro-deposition skim β-PbO
2, promptly made active ti-supported lead dioxide electric pole; The volume ratio of described masking liquid alkoxyl tin butanols liquid and trichloride antimony butanols liquid is 3.5: 1; Plumbi nitras is 200g/l, nitric acid 15ml/l, sodium fluoride 2g/l in the electroplate liquid of preparation lead dioxide electrode, and the anodic current density of electro-deposition is 6A/dm
2, electroplating temperature is that 90 ℃, electroplating time are that 8 minutes, cathode material are stainless steel.
Its purposes and example are together.
Embodiment three:
A kind of active lead dioxide electrode is to be carrier with the titanium plate; Area be 0.5 square metre, thick be that the active tin of one deck, sb oxide intermediate layer are arranged on 1.5 millimeters the titanium plate, the thickness in this intermediate layer is 2 microns; Powering in the intermediate layer and depositing thickness is β-PbO of 0.013 millimeter
2Layer.
Its preparation method be with the titanium plate behind acid etching, mixture masking liquid with 20% alkoxyl tin butanols liquid and 20% trichloride antimony butanols liquid applies 2 times again, behind hot blast drying, 450 ℃ of following thermal oxidations 1 hour, form the active tin-antimony oxide layer of a thin layer, the water flush away is floating thing, airing, again 450 ℃ of following thermal oxidation half an hour; Then with it as anode, in plumbi nitras, nitric acid, sodium fluoride electroplate liquid system, electro-deposition skim β-PbO
2, promptly made active ti-supported lead dioxide electric pole; The volume ratio of described masking liquid alkoxyl tin butanols liquid and trichloride antimony butanols liquid is 3: 1; Plumbi nitras is 180g/l, nitric acid 10ml/l, sodium fluoride 1g/l in the electroplate liquid of preparation lead dioxide electrode, and the anodic current density of electro-deposition is 2A/dm
2, electroplating temperature is that 85 ℃, electroplating time are that 3 minutes, cathode material are stainless steel.
Its purposes and example are together.
Claims (5)
1, a kind of active lead dioxide electrode is to be carrier with the titanium plate; It is characterized in that at area be 0.1-0.8 square metre, thick in the active tin of one deck, sb oxide intermediate layer are arranged on the titanium plate of 1-2 millimeter, the thickness in this intermediate layer is the 1-3 micron; Power in the intermediate layer and to deposit β-PbO that thickness is the 0.013-0.15 millimeter
1Layer.
2, the preparation method of the described active lead dioxide electrode of a kind of claim 1, it is characterized in that the titanium plate behind acid etching, mixture masking liquid with 20% alkoxyl tin butanols liquid and 20% trichloride antimony butanols liquid applies 1-3 time again, behind hot blast drying, 450 ℃ of following thermal oxidations 1 hour, form the active tin-antimony oxide layer of a thin layer, the water flush away is floating thing, airing, again 450 ℃ of following thermal oxidation half an hour; Then with it as anode, in plumbi nitras, nitric acid, sodium fluoride electroplate liquid system, electro-deposition skim β-PbO
8, promptly made active ti-supported lead dioxide electric pole.
3, the preparation method of active lead dioxide electrode as claimed in claim 2 is characterized in that the volume ratio of described masking liquid alkoxyl tin butanols liquid and trichloride antimony butanols liquid is (2.5~3.5): 1.
4, the preparation method of active lead dioxide electrode as claimed in claim 2, it is characterized in that preparing that plumbi nitras is that 160~200g/l, nitric acid are that 5-15ml/l, sodium fluoride are 0.5-2g/l in the electroplate liquid of lead dioxide electrode, the anodic current density of electro-deposition is 1-12A/dm
2, electroplating temperature is that 80-90 ℃, electroplating time are that 1-15 minute, cathode material are stainless steel.
5, the purposes of the described active lead dioxide electrode of a kind of claim 1 is characterized in that and this electrode can be made anode, is used for diaphragm process and produces boric acid technology; During electrolysis, anodic current density is 250A/m
2-800A/m
8, electrolysis run channel voltage is 3.0-5.5V.
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CN93116984A CN1073747C (en) | 1993-09-04 | 1993-09-04 | Active lead dioxide electrode and preparation method and application thereof |
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CN93116984A CN1073747C (en) | 1993-09-04 | 1993-09-04 | Active lead dioxide electrode and preparation method and application thereof |
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CN1073747C CN1073747C (en) | 2001-10-24 |
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Cited By (11)
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CN101798690A (en) * | 2010-03-12 | 2010-08-11 | 浙江工业大学 | Electroplating liquid for preparing lead dioxide electrodes and application thereof |
CN102534654A (en) * | 2010-12-17 | 2012-07-04 | 北京有色金属研究总院 | Method for manufacturing lead dioxide electrode plate on metal substrate |
CN102642895A (en) * | 2012-04-26 | 2012-08-22 | 南京大学 | Lead dioxide electrode, preparation method of lead dioxide electrode and application of lead dioxide electrode in treatment of reactive dyes |
CN103700813A (en) * | 2013-11-07 | 2014-04-02 | 西安建筑科技大学 | New method for preparing Ti base PbO2 dimensionally-stable anode |
CN104047020A (en) * | 2014-07-03 | 2014-09-17 | 环境保护部华南环境科学研究所 | Titanium-based doped polyvinylidene fluoride lead dioxide anode plate as well as preparation method and application thereof |
CN105401191A (en) * | 2015-11-05 | 2016-03-16 | 昆明理工大学 | Method for electrochemically synthesizing alpha-PbO2 on rotating disk electrode |
CN105668718A (en) * | 2016-04-12 | 2016-06-15 | 上海应用技术学院 | Preparation method of boron carbide/graphite co-doped lead dioxide plastic piece electrode |
CN108130582A (en) * | 2017-12-20 | 2018-06-08 | 陕西科技大学 | A kind of preparation method of 2.5 dimension anodes of high catalytic activity carried magnetic particle |
CN108217852A (en) * | 2018-01-11 | 2018-06-29 | 重庆大学 | High life, high catalytic activity lead dioxide electrode |
CN109023420A (en) * | 2018-07-18 | 2018-12-18 | 昆明理工大学 | A kind of nickel electrodeposition aluminum-base composite anode and preparation method thereof |
CN111675289A (en) * | 2020-06-28 | 2020-09-18 | 盐城工学院 | Preparation method of porous titanium-based lead dioxide electrode |
Families Citing this family (1)
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CN102074702B (en) * | 2010-12-28 | 2012-11-07 | 株洲冶炼集团股份有限公司 | Preparation method of lead-carbon composite material |
Family Cites Families (3)
Publication number | Priority date | Publication date | Assignee | Title |
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JPS62274087A (en) * | 1986-05-22 | 1987-11-28 | Permelec Electrode Ltd | Durable electrode for electrolysis and its production |
JPS62284095A (en) * | 1986-06-02 | 1987-12-09 | Permelec Electrode Ltd | Durable electrolytic electrode and its production |
CN1033657A (en) * | 1987-10-27 | 1989-07-05 | 福州大学化学工程系 | The modified anode of lead dioxide that electrolytic industry is used |
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1993
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CN101798690A (en) * | 2010-03-12 | 2010-08-11 | 浙江工业大学 | Electroplating liquid for preparing lead dioxide electrodes and application thereof |
CN102534654A (en) * | 2010-12-17 | 2012-07-04 | 北京有色金属研究总院 | Method for manufacturing lead dioxide electrode plate on metal substrate |
CN102642895A (en) * | 2012-04-26 | 2012-08-22 | 南京大学 | Lead dioxide electrode, preparation method of lead dioxide electrode and application of lead dioxide electrode in treatment of reactive dyes |
CN102642895B (en) * | 2012-04-26 | 2013-05-22 | 南京大学 | Lead dioxide electrode, preparation method of lead dioxide electrode and application of lead dioxide electrode in treatment of reactive dyes |
CN103700813B (en) * | 2013-11-07 | 2016-01-20 | 西安建筑科技大学 | A kind of Ti base β-PbO 2the preparation method of dimensional stable anode |
CN103700813A (en) * | 2013-11-07 | 2014-04-02 | 西安建筑科技大学 | New method for preparing Ti base PbO2 dimensionally-stable anode |
CN104047020A (en) * | 2014-07-03 | 2014-09-17 | 环境保护部华南环境科学研究所 | Titanium-based doped polyvinylidene fluoride lead dioxide anode plate as well as preparation method and application thereof |
CN105401191A (en) * | 2015-11-05 | 2016-03-16 | 昆明理工大学 | Method for electrochemically synthesizing alpha-PbO2 on rotating disk electrode |
CN105401191B (en) * | 2015-11-05 | 2017-09-22 | 昆明理工大学 | Electrochemistry formated α PbO in a kind of rotating disk electrode (r.d.e)2Method |
CN105668718A (en) * | 2016-04-12 | 2016-06-15 | 上海应用技术学院 | Preparation method of boron carbide/graphite co-doped lead dioxide plastic piece electrode |
CN108130582A (en) * | 2017-12-20 | 2018-06-08 | 陕西科技大学 | A kind of preparation method of 2.5 dimension anodes of high catalytic activity carried magnetic particle |
CN108217852A (en) * | 2018-01-11 | 2018-06-29 | 重庆大学 | High life, high catalytic activity lead dioxide electrode |
CN108217852B (en) * | 2018-01-11 | 2020-09-25 | 重庆大学 | Lead dioxide electrode used as anode in electrocatalytic sewage treatment and preparation method thereof |
CN109023420A (en) * | 2018-07-18 | 2018-12-18 | 昆明理工大学 | A kind of nickel electrodeposition aluminum-base composite anode and preparation method thereof |
CN111675289A (en) * | 2020-06-28 | 2020-09-18 | 盐城工学院 | Preparation method of porous titanium-based lead dioxide electrode |
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