Electrodes for electrolytic removal of nitrates from water, methods of making same, and apparatus incorporating said electrodes

• US 5,935,392 A
• Filed: 11/27/1996
• Issued: 08/10/1999
• Est. Priority Date: 06/01/1995
• Status: Expired due to Fees

• Current Assignee: Upscale Water Technologies Incorporated
• Original Assignee: Upscale Water Technologies Incorporated
• Inventors: Otten, Sjef, Lubin, Mark
• Primary Examiner(s): Phasge, Arun S.
• Application Number:
  US08/758,584
• Time in Patent Office: 986 Days
• Field of Search: 204/290 R, 204/231, 204/294, 427/113, 427/372.2, 427/376.2
• US Class Current: 204/229.4
• CPC Class Codes: C02F 1/46109 Electrodes
• CPC Class Codes: C02F 1/4676 by electroreduction
• CPC Class Codes: C02F 1/58 by removing specified dissolved compounds using ion-exchange C02F1/42; softening water C02F5/00
• CPC Class Codes: C02F 2001/46138 Electrodes comprising a substrate and a coating
• CPC Class Codes: C02F 2001/46152 characterised by the shape or form electrodes in particulate form or with conductive or non-conductive particles between them C02F1/46114
• CPC Class Codes: C02F 2001/46157 Perforated or foraminous electrodes
• CPC Class Codes: C02F 2101/163 Nitrates
• CPC Class Codes: C02F 2201/4611 Fluid flow
• CPC Class Codes: C25B 11/03 perforated or foraminous

Abstract

A carbon fiber electrode is coated with a noble metal oxide to create a noble metal oxide electrode with a very large surface area. According to a presently preferred embodiment, the noble metal oxide is iridium oxide. A method of making the electrode includes preparing a solution of iridium chloride and isopropyl alcohol, dipping a carbon fiber electrode into the solution, drying the electrode in the presence of nitrogen and heat, and heat treating the electrode in the presence of oxygen. An apparatus for removing nitrates from water includes an electrochemical flow cell through which the aqueous solution containing nitrates flows or a holding tank cell into which the solution is introduced and then released after processing, and an electrode system including an anodic iridium oxide coated carbon fiber electrode as described above, a carbon fiber cathodic electrode and a reference electrode. All of the electrodes are immersed in the aqueous solution and coupled to an electronic control circuit which impresses a voltage across the electrodes such that the voltage causes electrochemical reduction/oxidation reactions on the surface of the cathodic electrode. The electrodes are at a potential wherein nitrates are reduced but hydrogen, oxygen, and chlorine are not produced. Electrodes having different geometries are also provided.

Claims

1. An electrode for use in an electrochemical reaction, said electrode comprising:

a polyacrylonitrile based carbon fiber substrate coated with a noble metal oxide, wherein said noble metal oxide is iridium oxide.

2. An electrode according to claim 1, wherein:

said carbon fiber substrate has approximately 12 k fibers per tow.

3. An electrode according to claim 1, wherein:

said carbon fiber substrate coated with a noble metal oxide is a carbon fiber substrate coated with a noble metal oxide which was dried in the presence of substantially pure nitrogen.

4. An electrode according to claim 1, wherein:

said substrate has the geometry of one of a pony tail, a fabric plate, and a fabric cylinder.

5. A method of making an electrode for use in an electrochemical reaction, comprising:

a) dissolving an iridium chloride compound in alcohol to form an iridium chloride solution;

b) dipping a polyacrylonitrile based carbon fiber electrode in the solution; and

c) heat treating the dipped electrode in at approximately 225-350°

C. for 1.5 to 1.75 hours.

6. A method according to claim 5, wherein:

prior to said dipping a carbon fiber electrode, the solution is warmed to approximately 35°

C.

7. A method according to claim 6, wherein:

prior to warming the solution, the solution is aged at room temperature for approximately 18 hours.

8. A method according to claim 5, wherein:

prior to said step of heat treating, the dipped electrode is dried in the presence substantially pure N₂ at approximately 105±

5°

C. for approximately 10-20 minutes.

9. A method according to claim 5, further comprising:

d) forming the carbon fiber electrode as a fabric sheet; and

e) attaching the fabric sheet to a frame.

10. An apparatus for reducing nitrates in an aqueous solution, comprising:

a) a cathodic electrode;

b) a reference electrode;

c) an iridium oxide coated carbon polyacrylonitrile based fiber anodic electrode; and

d) a control circuit which impresses a voltage across said electrodes.

11. An apparatus according to claim 10, wherein:

said cathodic electrode is a carbon fiber electrode.

12. An apparatus according to claim 10, further comprising:

e) an electrochemical cell in which the aqueous solution containing nitrates is treated.

13. An apparatus according to claim 10, wherein:

said cell is a flow cell through which the aqueous solution flows at a flow rate relative to said cathodic electrode in the range of 0.1 to 50 feet per minute.

14. An apparatus according to claim 10, wherein:

the anodic electrode to cathodic electrode surface area ratio is in the range of 5;

1 to 30;

1.

15. An apparatus according to claim 10, wherein:

said anodic electrode has the geometry of one of a pony tail, a fabric plate, and a fabric cylinder.

16. An apparatus according to claim 10, wherein:

said voltage across said cathodic electrode relative to said reference electrode is between approximately -1100 mV to approximately -1700 mV, and

said voltage across said anodic electrode relative to said reference electrode is below approximately +800 mV.

17. An apparatus for reducing nitrates in an aqueous solution, comprising:

a) a cathodic electrode;

b) a reference electrode;

c) a noble metal oxide coated carbon fiber anodic electrode, said noble metal oxide coated carbon fiber anodic electrode being coated with a single species noble metal oxide, said single species consisting of iridium oxide; and

d) a control circuit which impresses a voltage across said electrodes.

18. An electrode for use in an electrochemical reaction, said electrode comprising:

a carbon fiber substrate coated with a single species of noble metal oxide, said single species consisting of iridium oxide.