CN106917104A - A kind of method of use BDD electrodes electro synthesis persulfate - Google Patents

A kind of method of use BDD electrodes electro synthesis persulfate Download PDF

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Publication number
CN106917104A
CN106917104A CN201710176058.5A CN201710176058A CN106917104A CN 106917104 A CN106917104 A CN 106917104A CN 201710176058 A CN201710176058 A CN 201710176058A CN 106917104 A CN106917104 A CN 106917104A
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CN
China
Prior art keywords
persulfate
sulfuric acid
electrode
bdd electrodes
current density
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Pending
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CN201710176058.5A
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Chinese (zh)
Inventor
周明华
蔡静菊
卢晓晔
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Nankai University
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Nankai University
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Priority to CN201710176058.5A priority Critical patent/CN106917104A/en
Publication of CN106917104A publication Critical patent/CN106917104A/en
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25BELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00Electrolytic production of inorganic compounds or non-metals
    • C25B1/01Products
    • C25B1/28Per-compounds
    • C25B1/29Persulfates
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25BELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25BELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B9/00Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
    • C25B9/17Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof
    • C25B9/19Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof with diaphragms

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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)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)

Abstract

The present invention relates to a kind of method of utilization BDD electrodes electro synthesis persulfate.The method with BDD as electrode as anode, zirconium electrode as negative electrode and cation-exchange membrane composition electrolytic cell, separate anode chamber and cathode chamber forms recycle stream in the presence of pump, is electrolyte with 2 5M sulfuric acid, current density be 5 100mA/cm2, temperature is the system of structure under conditions of 9 20 DEG C.The method is higher compared to the persulfate concentration of other electro synthesis methods synthesis, and current efficiency is also higher, realizes product persulfate in situ.

Description

A kind of method of use BDD electrodes electro synthesis persulfate
Technical field
The invention belongs to field of environment engineering technology, it is related to a kind of method of use BDD electrodes electro synthesis persulfate.
Background technology
Persulfate S2O8 2-Due to having been obtained extensively in chemistry, weaving, electronics, oil and field of food containing active oxygen General application, is such as used as initiator, ripener and bleaching agent.The production common method of persulfate is electrolysis.It is generally sharp With platinum electrode or the Ti electrode of platinum plating higher than 500mA/cm2Current density under be electrolysed sulfate radical generation, but such method The side reaction for being often accompanied by water oxygen is produced and reduces current efficiency while the dissolution of platinum electrode can be caused to introduce secondary pollution.This The difficulty that the unstability of outer persulfate will also result in transport limits its application.Therefore a kind of more efficient electro synthesis are sought S2O8 2-Method has the very big market demand.
S2O8 2-Synthesis be anodic oxidation process, therefore the selection of anode material is most important.BDD electrodes Yin Qigao Oxygen evolution potential, the advantage of low background current and preferable chemical stability and low absorbability up to 3V and in Environmental electrochemistry field It is widely used, such as the negative electrode of heavy metal is reclaimed, biology sensor and electrochemical analysis measure etc., but mainly for the treatment of in waste water Organic pollution.Compared to metal electrode, BDD electrodes are more easy to realize under low current density due to the characteristic of oxygen evolution potential Electrosynthesis glyoxal S2O8 2-, therefore with good application prospect.Further, since anodic oxidation sulfuric acid generation persulfuric acid is heat release Process, this easily causes the S of thermally labile2O8 2-Decompose and reduce current efficiency, traditional monopole room reactor sulfate radical turns Change efficiency only less than 5%.
The content of the invention
Based on this, the purpose of the present invention is by the bar in separate anode chamber and the temperature of cathode chamber and control anode chamber Using BDD electrolysis sulfuric acid electro synthesis persulfates S under part2O8 2-, to realize the raising of current efficiency.
The present invention produces S2O8 2-Method it is as follows:With BDD electrodes as anode, zirconium electrode be negative electrode cation-exchange membrane The device for separating composition is electrolytic cell, and anode chamber and cathode chamber are the sulfuric acid of the 2-5M of same concentration, and rate of circulating flow is 120- 300L/h, control electric current density is 5-100mA/cm2, temperature is electrosynthesis glyoxal at 9-20 DEG C.
The present invention has following outstanding feature and beneficial effect:
(1) the method can prevent S under conditions of separate anode chamber and cathode chamber and temperature control2O8 2-Because of electrolysis heat release Decompose.
(2) the method can be electrolysed sulfuric acid under relatively low current density and produce S2O8 2-
(3) the method improves 2 times to the oxidation efficiency of sulfate radical compared with conventional method.
Brief description of the drawings
Fig. 1 is the S of generation under different current densities2O8 2-Amount.
Fig. 2 is the current efficiency under different current densities.
Specific embodiment
The present invention is described in further detail by following examples combination accompanying drawing.
(1) method of the present invention processing procedure
With BDD electrodes (a diameter of 10cm) as anode, zirconium electrode (a diameter of 10cm) is negative electrode, cation-exchange membrane composition The sulfuric acid concentration of electrolytic cell, anode chamber and cathode chamber is 2M, and rate of circulating flow is 200L/h, the temperature of control anode and cathode chamber It is 9 DEG C, is 5-100mA/cm in current density2, it is electrolysed 300min.
(2) embodiment obtains effect
It is electrolysed under the different current density conditions of the examples comparative and produces S2O8 2-Amount, as shown in figure 1, as electric current is close The increase of degree, S2O8 2-Content also increase.When current density is 5mA/cm2When, it is electrolysed 300min, the S of generation2O8 2-Amount It is 0.028M, and works as current density for 100mA/cm2When, it is electrolysed 300min, the S of generation2O8 2-Amount be 0.26M.This and industry Upper high current density (500mA/cm2) compare, greatly reduce industrial cost.
Fig. 2 compared for the current efficiency under different current density conditions.As the increase current efficiency of current density is presented Downward trend.When current density is 5mA/cm2When, current efficiency is up to 83%, and working as current density increases to 100mA/cm2 When, current efficiency is reduced to 35%.

Claims (3)

1. a kind of method of utilization BDD electrodes electro synthesis persulfate, the method is as follows:With BDD electrodes as anode, zirconium electrode be The sulfuric acid solution of same concentrations, is respectively placed in separate anode and cathode chamber by negative electrode and cation-exchange membrane composition electrolytic cell, Sulfuric acid rate of circulating flow is 120-300L/h, and under controlled temperature conditions, current density is 5-100mA/cm2Electrolysis.
2. method according to claim 1, it is characterised in that the sulfuric acid concentration is 2-5M.
3. method according to claim 1, it is characterised in that the temperature is 9-20 DEG C.
CN201710176058.5A 2017-03-17 2017-03-17 A kind of method of use BDD electrodes electro synthesis persulfate Pending CN106917104A (en)

Priority Applications (1)

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CN201710176058.5A CN106917104A (en) 2017-03-17 2017-03-17 A kind of method of use BDD electrodes electro synthesis persulfate

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Application Number Priority Date Filing Date Title
CN201710176058.5A CN106917104A (en) 2017-03-17 2017-03-17 A kind of method of use BDD electrodes electro synthesis persulfate

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110902776A (en) * 2019-11-23 2020-03-24 同济大学 Method for generating sulfate radical free radical oxidation pollutants through in-situ electrocatalysis

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001192874A (en) * 1999-12-28 2001-07-17 Permelec Electrode Ltd Method for preparing persulfuric acid-dissolving water
CN103380232A (en) * 2010-12-21 2013-10-30 氯工程公司 Electrically conductive diamond electrode, and sulfuric acid electrolysis method and sulfuric acid electrolysis apparatus each utilizing same
CN103384731A (en) * 2011-02-28 2013-11-06 栗田工业株式会社 Sulfuric acid electrolysis method and sulfuric acid electrolysis device
CN103518007A (en) * 2011-03-08 2014-01-15 氯工程公司 Apparatus for electrolyzing sulfuric acid and method for electrolyzing sulfuric acid

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001192874A (en) * 1999-12-28 2001-07-17 Permelec Electrode Ltd Method for preparing persulfuric acid-dissolving water
CN103380232A (en) * 2010-12-21 2013-10-30 氯工程公司 Electrically conductive diamond electrode, and sulfuric acid electrolysis method and sulfuric acid electrolysis apparatus each utilizing same
CN103384731A (en) * 2011-02-28 2013-11-06 栗田工业株式会社 Sulfuric acid electrolysis method and sulfuric acid electrolysis device
CN103518007A (en) * 2011-03-08 2014-01-15 氯工程公司 Apparatus for electrolyzing sulfuric acid and method for electrolyzing sulfuric acid

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
P-A. MICHAUD 等: "Electrochemical oxidation of water on synthetic boron-doped diamond thin film anodes", 《JOURNAL OF APPLIED ELECTROCHEMISTRY》 *
SUBRAMANIAN BALAJI 等: "Influence of cathode on the electro-generation of peroxydisulfuric acid oxidant and its application for effective removal of SO2 by room temperature electro-scrubbing process", 《JOURNAL OF HAZARDOUS MATERIALS》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110902776A (en) * 2019-11-23 2020-03-24 同济大学 Method for generating sulfate radical free radical oxidation pollutants through in-situ electrocatalysis

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