- Document Number:
20060049064
- Appl. No:
10/533098
- Application Filed:
September 19, 2003
- نبذة مختصرة :
The present invention concerns a process for oxidizing an aqueous phase comprising ferrocyanide (V) which is recovered from an oxidative phenolic coupling reaction, to an aqueous phase comprising ferricyanide (IV), in a divided electrochemical cell, comprising preparing an anolyte comprising pretreating the aqueous phase comprising ferrocyanide (V) which is recovered from an oxidative phenolic coupling reaction by decantation or extraction or filtration; placing the anolyte in contact with an anodic electrode of the divided electrochemical cell; placing a catholyte in contact with a cathodic electrode of the divided electrochemical cell; and applying electrical power to the divided electrochemical cell, wherein the electrical power has an amperage or voltage and wherein the applying is for a time period sufficient to oxidize the ferrocyanide (V) to ferricyanide (IV).
- Inventors:
Horvath, Andras (Turnhout, BE); Verbraeken, Jurgen Alois (Vosselaar, BE); Novak, Mihaly (Szeged, HU); De Knaep, Alfons Gaston Maria (Turnhout, BE)
- Claim:
1. A process for oxidizing an aqueous phase comprising ferrocyanide (V) which is recovered from an oxidative phenolic coupling reaction, to an aqueous phase comprising ferricyanide (IV), in a divided electrochemical cell, comprising preparing an anolyte comprising pretreating the aqueous phase comprising ferrocyanide (V) which is recovered from an oxidative phenolic coupling reaction by decantation or extraction or filtration; placing the anolyte in contact with an anodic electrode of the divided electrochemical cell; placing a catholyte in contact with a cathodic electrode of the divided electrochemical cell; and applying electrical power to the divided electrochemical cell, wherein the electrical power has an amperage or voltage and wherein the applying is for a time period sufficient to oxidize the ferrocyanide (V) to ferricyanide (IV).
- Claim:
2. The process of claim 1 wherein the divided electrochemical cell is divided by a cation selective membrane.
- Claim:
3. The process of claim 2 wherein the cation selective membrane is a Nafion® perfluorinated polyethylene sulfonic acid membrane.
- Claim:
4. The process of claim 1 wherein the pre-treatment of the aqueous phase comprising ferrocyanide (V) which is recovered from an oxidative phenolic coupling reaction comprises storing said aqueous phase at 60° C. or more during a period of time sufficient to let precipitate suspended particles and decanting the supernatant aqueous phase so as to separate it from the precipitated particles.
- Claim:
5. The process of claim 1 wherein the pre-treatment of the aqueous phase comprising ferrocyanide (V) which is recovered from an oxidative phenolic coupling reaction comprises extracting the aqueous phase with an organic solvent.
- Claim:
6. The process of claim 1 wherein the pre-treatment of the aqueous phase comprising ferrocyanide (V) which is recovered from an oxidative phenolic coupling reaction comprises filtering the aqueous phase.
- Claim:
7. The process of claim 1 wherein the catholyte comprises an alkali metal hydroxy or an alkali metal salt (e.g. KOH, K2CO3, KHCO3, KCl, KCN) solution having a concentration in the range of from 0.0001 to 1 M.
- Claim:
8. The process of claim 1 wherein the anodic electrode is graphite; and the cathodic electrode is selected from the group of copper, nickel, stainless steel and graphite.
- Claim:
9. The process of claim 1 wherein the electrical power applied to the divided electrochemical cell has a voltage between 2 V and 2.6 V.
- Claim:
10. The process of claim 9 wherein the voltage is 2.6 V±0.1 V.
- Claim:
11. The process of claim 1 wherein the anolyte and catholyte are kept at a temperature of 50° C. or more.
- Claim:
12. The process of claim 1 further comprising one or all of the monitoring steps selected from the group of recording of the current passing through the divided electrochemical cell; recording of the ferrocyanide (V) concentration decay; recording of the ferricyanide (IV) concentration accumulation; recording of the apparition of free cyanide (CN—); and recording of the conductivity of the catholyte.
- Claim:
13. An aqueous phase comprising ferricyanide (IV) obtainable by a process as described in claim 1.
- Claim:
14. Use of an aqueous phase comprising ferricyanide (IV) as described in claim 13 for effecting an oxidative phenolic coupling reaction on substrates susceptible to such reaction.
- Claim:
15. The use of claim 14 wherein the oxidative phenolic coupling reaction is conducted on the substrate of formula (II) [chemical expression included] yielding a compound of formula (III) [chemical expression included]
- Current U.S. Class:
205687/000
- Current International Class:
02; 25
- الرقم المعرف:
edspap.20060049064
Processing Request
No Comments.