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WO2013019427A1 - Procédé de génération d'un biocide - Google Patents

Procédé de génération d'un biocide Download PDF

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Publication number
WO2013019427A1
WO2013019427A1 PCT/US2012/047558 US2012047558W WO2013019427A1 WO 2013019427 A1 WO2013019427 A1 WO 2013019427A1 US 2012047558 W US2012047558 W US 2012047558W WO 2013019427 A1 WO2013019427 A1 WO 2013019427A1
Authority
WO
WIPO (PCT)
Prior art keywords
capacitive electrode
electrical current
aqueous solution
acts
capacitive
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/US2012/047558
Other languages
English (en)
Inventor
Zijun Xia
Rihua Xiong
Chihyu Sui
Hai Yang
Qunjian Huang
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
General Electric Co
Original Assignee
General Electric Co
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by General Electric Co filed Critical General Electric Co
Publication of WO2013019427A1 publication Critical patent/WO2013019427A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
    • C02F1/4672—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation
    • C02F1/4674—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation with halogen or compound of halogens, e.g. chlorine, bromine
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/469—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
    • C02F1/4691—Capacitive deionisation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/46104—Devices therefor; Their operating or servicing
    • C02F1/46109—Electrodes
    • C02F2001/46133—Electrodes characterised by the material
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2201/00—Apparatus for treatment of water, waste water or sewage
    • C02F2201/46—Apparatus for electrochemical processes
    • C02F2201/461—Electrolysis apparatus
    • C02F2201/46105—Details relating to the electrolytic devices
    • C02F2201/4612—Controlling or monitoring
    • C02F2201/46125—Electrical variables
    • C02F2201/4613—Inversing polarity

Definitions

  • the present invention relates to methods for generating biocides, such as chlorine, hypochlorite, bromine, and hypobromide.
  • Bacteriostatic treatment/sterilization of water is usually done by introducing biocides, e.g., at least one of chlorine, hypochlorite, bromine, and hypobromide, to the water.
  • biocides e.g., at least one of chlorine, hypochlorite, bromine, and hypobromide
  • U.S. patent No. 6,045,704 discloses a raw water purification system for purifying raw water with a first d.c. voltage applied between a conductive adsorber portion and a primary electrode in the raw water and accelerating generation of chlorine from the raw water with a second d.c. voltage higher than the first d.c. voltage.
  • the first d.c. voltage is of a low level sufficient to capture the microorganisms and the bacteria and the second d.c. voltage is of a relatively high level capable of performing electrolysis of the raw water to generate chlorine.
  • this raw water purification system electrolysis of the raw water does not happen when the first d.c. voltage is applied and only happens when the second d.c. voltage is applied.
  • the concentration of chlorine generated in this raw water purification system is as low as, e.g., 1 ppm.
  • biocides at least one of chlorine, hypochlorite, bromine, and hypobromide.
  • the present invention relates to a method, comprising: positioning a first capacitive electrode and a first non-capacitive electrode in a first aqueous solution comprising at least one of sodium chloride, potassium chloride, sodium bromide and potassium bromide; applying a first electrical current on the first capacitive electrode and the first non-capacitive electrode to electrolyse the first aqueous solution to generate at least one of chlorine and bromine, while the first capacitive electrode acts as cathode and the first non-capacitive electrode acts as anode; applying a second electrical current on the first capacitive electrode and the first non-capacitive electrode to electrolyse the first aqueous solution to generate hydrogen, while the first capacitive electrode acts as anode and the first non- capacitive electrode acts as cathode; and switching polarities of the first capacitive electrode and the first non-capacitive electrode before the first capacitive electrode is fully occupied.
  • FIG. 1 is a schematic diagram of a cell used in one embodiment
  • FIG. 2 is a schematic diagram showing the cell of FIG. 1 connects to a power supplier
  • FIG. 3 is a schematic diagram showing a capacitive electrode of the cell of FIG. 2 is close to be fully occupied;
  • FIG. 4 is a schematic diagram showing the cell of FIG. 3 is switched in polarities thereof;
  • FIG. 5 is a schematic diagram of the cell of FIG. 4 after electrochemical reactions
  • FIG. 6 is a schematic diagram of the cell of FIG. 5 while the capacitive electrode is close to be fully occupied.
  • FIG. 7 is an image view under a scanning electron microscope of an activated carbon sheet used in the examples.
  • Approximating language may be applied to modify any quantitative representation that is not to be limited to the specific quantity specified and could permissibly vary without resulting in a change in the basic function to which it is related. Accordingly, a value modified by a term or terms, such as "about”, is not to be limited to the precise value specified. In some instances, the approximating language may correspond to the precision of an instrument for measuring the value. Moreover, the suffix "(s)" as used herein is usually intended to include both the singular and the plural of the term that it modifies, thereby including one or more of that term.
  • any numerical value ranges recited herein include all values from the lower value to the upper value in increments of one unit provided that there is a separation of at least 2 units between any lower value and corresponding higher value.
  • the amount of a component or a value of a process variable such as, for example, temperature, pressure, time and the like is, for example, from 1 to 90, from 20 to 80, or from 30 to 70, it is intended that values such as 15 to 85, 22 to 68, 43 to 51, 30 to 32 etc. are expressly enumerated in this specification.
  • one unit is considered to be 0.0001, 0.001, 0.01 or 0.1 as appropriate.
  • the method for generating biocides further comprises: positioning a second capacitive electrode and a second non-capacitive electrode in a second aqueous solution comprising at least one of sodium chloride, potassium chloride, sodium bromide and potassium bromide; applying a third electrical current on the second capacitive electrode and the second non-capacitive electrode to electrolyse the second aqueous solution to generate at least one of chlorine and bromine, while the second capacitive electrode acts as cathode and the second non-capacitive electrode acts as anode; applying a fourth electrical current on the second capacitive electrode and the second non-capacitive electrode to electrolyse the second aqueous solution to generate hydrogen, while the second capacitive electrode acts anode and the second non- capacitive electrode acts as cathode; and switching polarities of the second capacitive electrode and the second non-capacitive electrode before the second capacitive electrode is fully occupied.
  • the first aqueous solution and the second aqueous solution may be from a same source or different sources.
  • the first cell comprising the first non-capacitive electrode and the first capacitive electrode and the second cell comprising the second non-capacitive electrode and the second capacitive electrode may be the same or different from each other.
  • the first and the second cells may generate the at least one of chlorine and bromine at the same time or at different times.
  • the first electrical current and the third electrical current may be the same as or different from the second electrical current and the fourth electrical current, respectively. If the first electrical current is higher than the second electrical current, the time to apply the first electrical current before the first capacitive electrode is fully occupied may be shorter than the time to apply the second electrical current before the first capacitive electrode is fully occupied. If the third electrical current is higher than the fourth electrical current, the time to apply the third electrical current before the second capacitive electrode is fully occupied may be shorter than the time to apply the fourth electrical current before the second capacitive electrode is fully occupied. During the time period while the capacitive and the non-capacitive electrodes are in a certain polarity, the first, the second, the third and the fourth electrical currents may be increased or decreased, respectively.
  • the first electrical current is applied at the same time as the fourth electrical current is applied and the second electrical current is applied at the same time as the third electrical current is applied, and product streams from the two cells are mixed together.
  • the at least one of chlorine and bromine is generated at a place different from where hydrogen is generated and the at least one of chlorine, bromine, hypochlorite and hypobromide may be continually obtained from the combination of the two cells.
  • a cell 10 used in one embodiment has an entrance 20 for receiving a raw material stream 30 which is electrolysed to generate a product stream 40 flowing out from an export 50.
  • a non-capacitive electrode 1 and a capacitive electrode 2 of the cell 10 are positioned in an aqueous solution 3 from the raw material stream 30 in the cell 10.
  • the at least one of sodium chloride, potassium chloride, sodium bromide and potassium bromide in the aqueous solution 3 could be expressed as MX existing in the form of ion, in which X " is CI " or Br " and M + is Na + or K + .
  • FIG. 3 shows a status while the capacitive electrode 2 is close to fully occupied. If X2 generated on the anode is gaseous CI2, at least some of X2 leaves the solution, some flows out of the product stream 40 via the export 50, and some may be retained in the aqueous solution 3. If X2 is liquid Br 2 , at least some of X2 flows out of the product stream 40 via the export 50, and some may be retained in the aqueous solution 3.
  • the solution contains X 2 , at least some of the MOH generated reacts with the X 2 .
  • the overall reactions in the cell are: 2MX + 2H 2 0 ⁇ X 2 + 2MOH + H 2 and X 2 + 2MOH ⁇ MOX + MX + H 2 0. Therefore, X 2 (at least one of Cl 2 and Br 2 ) is generated in the cell, at least some of the X 2 (at least one of Cl 2 and Br 2 ) is further reacted into the MOX (at least one of hypochlorite and hypobromide), and the product stream from the cell comprises at least one of chlorine, bromine, hypochlorite and hypobromide.
  • FIG. 6 shows a status while the capacitive electrode 2 is close to be fully occupied. The processes described above can be conducted circularly.
  • H 2 and the X 2 (at least one of Cl 2 and Br 2 ) are generated at different times in a single cell.
  • H 2 can be discharged rapidly from the cell.
  • the possibility of mixing H 2 and X 2 (at least one of Cl 2 and Br 2 ) and the possibility of forming at least one of hydrogen chloride and hydrogen bromide, which is corrosive to the container during storage and/or transportation and is apt to explode at relatively high concentration, is eliminated/reduced.
  • the at least one of chlorine, bromine, hypochlorite and hypobromide generated is a biocide useful to remove microbes (microorganisms and bacteria etc.).
  • the product stream from the cell may flow into or be added into an aqueous stream comprising microbes to remove the microbes.
  • the cell may include other components besides the electrodes.
  • a spacer is positioned between the capacitive electrode and the non- capacitive electrode.
  • gasket, silicone rubber and enclosure plate may be used to package/support the electrodes.
  • the capacitive electrode may be made of any materials that are suitable for capacitive electrodes used in electrochemical super capacitors.
  • the capacitive electrode may be porous having relatively large surface area, e.g., 1000 m 2 /g, and capable of adsorption.
  • the capacitive electrode comprises carbon based materials, such as activated carbon.
  • the capacitive electrode comprises an activated carbon sheet and a current collector below the activated carbon sheet.
  • the current collector comprises at least one of titanium, platinum, gold and conducting polymer.
  • the current collector may be in the form of mesh. In some embodiments, there may be a cationic exchange coating on the activated carbon sheet.
  • the non-capacitive electrode may be made of any materials that are suitable for non-capacitive electrodes used in electrochemical cells.
  • the non-capacitive electrode comprises titanium.
  • the non- capacitive electrode comprises a coating of ruthenium oxide.
  • the electrolysis may be conducted at any suitable temperature and pressure such as room temperature and atmosphere pressure.
  • the pH of the product stream from the cells may change with the change of electro-chemical reaction in the cell, e.g., in some embodiments, when the first or the fourth electrical current is applied, the product stream may be acidic while when the second or the third electrical current is applied, the product stream may be alkaline.
  • “Fully occupied” referred to herein means the state of the capacitive electrode being fully occupied with adsorbed materials and the point when actions at the capacitive electrode change from adsorptions to electro-chemical reactions.
  • the capacitive electrode is fully occupied when hydrogen, bromine or chlorine generated begins to be detectable.
  • "before... fully occupied” means before the concentration of hydrogen, bromine, chlorine is as high as to cause explosion problems.
  • FIG. 7 is an image view under a scanning electron microscope of an activated carbon sheet used in the examples.
  • the surface area of activated carbon was about 1000 m 2 /g.
  • the carbon loading of the activated carbon sheet was about 0.42 g/cm 3 .
  • the projection area of the electrode was 512 cm 2 (16 cm x 32 cm).
  • Theoretically the activated carbon electrode area was about 53760 m 2 .
  • the electrode thickness was 0.25 cm.
  • the Ti mesh was used as the current collector in the activated carbon electrode.
  • Another sheet of Ti mesh (16 cm x 32 cm) was used as the non-capacitive electrode and was located opposite to the capacitive electrode.
  • An insulative spacer was positioned between the capacitive electrode and the non-capacitive electrode.
  • a gasket, a silicone rubber sheet and an enclosure sheet was located sequentially outside each of the non-capacitive and capacitive electrodes to package the electrodes therebetween.
  • a cationic exchange membrane was positioned between the capacitive and the non- capacitive electrodes of the cell used.
  • NaCl solution (52.8 g/1) was fed into the cell at a flow rate of 20 ml/min, 1.73 cm/s.
  • Electrical current of 500 mA was charged on the electrodes and increased with time to 1,500 mA and 3,000 mA, while titanium electrode served as anode and activated carbon electrode served as cathode.
  • samples were randomly taken from the product streams of the electrodes at three different times during each time period when certain electrical current is applied. Concentration of free chlorine and the pH of the samples were tested, respectively.
  • Free chlorine was detected in the sample from the Ti electrode, that is, the anode chamber and was not detectable in the sample from the cathode chamber, the activated carbon electrode side. Except the samples taken when the electrical current of 3,000 mA was applied, the pHs of the samples from both sides kept acidic, indicating that there was no 3 ⁇ 4 generated, since if 3 ⁇ 4 was generated, the product stream would turn into alkaline. There was no detectable 3 ⁇ 4 at both electrodes according to the ATi C16 3 ⁇ 4 detector too.
  • the current density was calculated with the following formula: current/effective area, in examples herein the effective area was 0.16 m x 0.32 m.
  • productivity is the average of the three samples.
  • Table 4 shows the pHs of samples from the cell generating 3 ⁇ 4 at different electrical currents and average voltages.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Molecular Biology (AREA)
  • Health & Medical Sciences (AREA)
  • Water Treatment By Electricity Or Magnetism (AREA)

Abstract

La présente invention concerne un procédé consistant à positionner une première électrode capacitive et une première électrode non-capacitive dans une première solution aqueuse contenant au moins soit du chlorure de sodium, soit du chlorure de potassium, soit du bromure de sodium, soit du bromure de potassium ; à appliquer un premier courant électrique sur la première électrode capacitive et sur la première électrode non-capacitive afin d'entraîner l'électrolyse de la première solution aqueuse et la génération d'au moins soit du chlore, soit du brome, la première électrode capacitive jouant le rôle de cathode et la première électrode non-capacitive d'anode ; à appliquer un second courant électrique sur la première électrode capacitive et sur la première électrode non-capacitive en vue d'entraîner l'électrolyse de la première solution aqueuse et la génération d'hydrogène, la première électrode capacitive jouant le rôle d'anode et la première électrode non-capacitive de cathode ; et à inverser les polarités de la première électrode capacitive et de la première électrode non-capacitive avant saturation complète de la première électrode capacitive.
PCT/US2012/047558 2011-07-29 2012-07-20 Procédé de génération d'un biocide Ceased WO2013019427A1 (fr)

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CN2011102169877A CN102897874A (zh) 2011-07-29 2011-07-29 制备杀菌剂的方法
CN201110216987.7 2011-08-01

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2016019055A1 (fr) * 2014-07-30 2016-02-04 Ecolab Usa Inc. Générateur de biocides mixtes
JP2018529511A (ja) * 2015-08-25 2018-10-11 バル−イラン ユニヴァーシティ 非対称電気化学電池装置およびその作動方法
KR20190124729A (ko) * 2017-03-06 2019-11-05 에보쿠아 워터 테크놀로지스 엘엘씨 개선된 전기화학 시스템 설계를 위한 피드백 제어의 실행
SE2151488A1 (en) * 2021-12-07 2023-06-08 Caplyzer Ab Unipolar half-cell and electrolysis system including the same

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EP1024116A2 (fr) * 1999-01-27 2000-08-02 Sanyo Electric Co., Ltd. Appareil pour purifier et distribuer de l eau et procédé de purification d eau contenant du chlore
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EP2070875A1 (fr) * 2007-12-14 2009-06-17 Unilever N.V. Électrode pour désionisation capacitive
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US6045704A (en) 1996-11-05 2000-04-04 Sanden Corporation Water purification system and method having a chlorine generating function in addition to a bacteriostatic function
EP1024116A2 (fr) * 1999-01-27 2000-08-02 Sanyo Electric Co., Ltd. Appareil pour purifier et distribuer de l eau et procédé de purification d eau contenant du chlore
WO2003055806A1 (fr) * 2002-01-04 2003-07-10 Johannes Petrus Paulus Tholen Dispositif electrolytique et procede de desinfection de l'eau dans un systeme d'approvisionnement en eau par la generation de chlore actif
EP2070875A1 (fr) * 2007-12-14 2009-06-17 Unilever N.V. Électrode pour désionisation capacitive
EP2298441A2 (fr) * 2009-08-21 2011-03-23 Samsung Electronics Co., Ltd. Système de filtre d'eau potable, son procédé de régénération et dispositif de purification de l'eau incluant le système de filtre d'eau potable

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2016019055A1 (fr) * 2014-07-30 2016-02-04 Ecolab Usa Inc. Générateur de biocides mixtes
US9695073B2 (en) 2014-07-30 2017-07-04 Ecolab Usa Inc. Dual biocide generator
JP2018529511A (ja) * 2015-08-25 2018-10-11 バル−イラン ユニヴァーシティ 非対称電気化学電池装置およびその作動方法
US11111160B2 (en) 2015-08-25 2021-09-07 Bar-Ilan University Asymmetric electrochemical cell apparatus, and operating methods thereof
KR20190124729A (ko) * 2017-03-06 2019-11-05 에보쿠아 워터 테크놀로지스 엘엘씨 개선된 전기화학 시스템 설계를 위한 피드백 제어의 실행
EP3593401A4 (fr) * 2017-03-06 2021-01-13 Evoqua Water Technologies LLC Mise en uvre d'une commande de rétroaction en vue d'une conception améliorée de système électrochimique
AU2018231091B2 (en) * 2017-03-06 2023-11-16 Evoqua Water Technologies Llc Implementation of feedback control for improved electrochemical system design
KR102645213B1 (ko) 2017-03-06 2024-03-07 에보쿠아 워터 테크놀로지스 엘엘씨 개선된 전기화학 시스템 설계를 위한 피드백 제어의 실행
SE2151488A1 (en) * 2021-12-07 2023-06-08 Caplyzer Ab Unipolar half-cell and electrolysis system including the same
WO2023104878A2 (fr) 2021-12-07 2023-06-15 Caplyzer Ab Système d'électrolyse comprenant au moins une demi-cellule capacitive
WO2023104878A3 (fr) * 2021-12-07 2023-07-20 Caplyzer Ab Système d'électrolyse comprenant au moins une demi-cellule capacitive
SE546000C2 (en) * 2021-12-07 2024-04-09 Caplyzer Ab Electrochemical system comprising two half-cells and method for electrochemical production of gas

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TW201321310A (zh) 2013-06-01

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