Process for the production of ferrocyanide blue

• US 4,046,861 A
• Filed: 10/07/1975
• Issued: 09/06/1977
• Est. Priority Date: 11/08/1974
• Status: Expired due to Term

• Current Assignee: Deutsche Gold- und Silber-Scheideanstalt vormals Roessler
• Original Assignee: Deutsche Gold- und Silber-Scheideanstalt vormals Roessler
• Inventors: Reinhardt, Helmut, Gratzfeld, Everhard, Clausen, Eva
• Primary Examiner(s): Thomas, Earl C.
• Application Number:
  US05/620,273
• Time in Patent Office: 700 Days
• Field of Search: 423/367, 106/304
• US Class Current: 423/367
• CPC Class Codes: C01P 2004/62 Submicrometer sized, i.e. from 0.1-1 micrometer
• CPC Class Codes: C01P 2006/80 Compositional purity
• CPC Class Codes: C09C 1/26 Iron blues

Abstract

Ferrocyanide blue is produced by reacting an aqueous ferrocyanide solution with an iron II salt and subsequently aging of the precipitate at elevated temperature and optionally at elevated pressure as well as oxidation in acid medium. The improvement comprises simultaneously leading the aqueous solution of ferrocyanide and the ferrous salt solution into a water receiver, whereby optimum mixing occurs during the precipitation and whereupon the precipitate formed, the so-called white stage is aged in known manner directly in the reaction medium in the presence of the salts formed in the reaction at elevated temperature and optionally under pressure and likewise in known manner is converted into Berlin blue by oxidation in acid medium.

Claims

1. In a process for the production of ferrocyanide blue by reaction of an aqueous ferrocyanide solution with an iron II salt and thereafter aging the precipitate at elevated temperature and oxidizing the aged precipitate to form ferrocyanide blue, the improvement comprising simultaneously introducing an aqueous solution of ferrocyanide consisting of a mixture of sodium and potassium ferrocyanides and an aqueous solution of the ferrous II salt into a water receiver containing water in an amount of 20 to 40 weight % based on the weight of the entire suspension formed to thereby provide optimum mixing and to form a suspension of the precipitate of ferrocyanide white in the resulting aqueous reaction medium, and aging the precipitate in the reaction medium in the presence of the salts formed in the reaction.

2. The process of claim 1 wherein the formation of the ferrocyanide white precipitate and the aging are carried out under superatmospheric pressure.

3. The process of claim 1 wherein the iron II salt is ferrous chloride or ferrous sulfate.

4. The process of claim 1 wherein the pH of the ferrocyanide solution 3.5 to 13 and the pH of the iron II salt solution is 0.8 to 6.

5. The process of claim 4 wherein the reaction is carried out in the presence of a greater than stoichiometric amount of iron salt to provide during and after the precipitation 0.3 to 3 grams of ferrous ion per liter of ferrocyanide white suspension.

6. The process of claim 5 wherein the amount of iron II salt is sufficient to provide 0.6 grams of ferrous ion.

7. The process of claim 4 wherein the reaction is carried out in the presence of a greater than stoichiometric amount of water soluble ferrocyanide to provide during and after the precipitation 0.25 to 20 grams of ferrocyanide ions per liter of ferrocyanide white suspension.

8. The process of claim 4 wherein the iron II salt solution is pickling solution.

9. The process of claim 4 wherein there is added 1/20 to 1/2 mole of ammonium ion per mole of ferrocyanide ion in the reaction mixture at a point between the precipitation of the ferrocyanide white and the beginning of the oxidation.

10. The process of claim 9 wherein the amount of ammonium ion is 1/6 to 1/3 mole per mole of ferrocyanide ion in the reaction mixture.

11. The process of claim 1 wherein the precipitation is carried out at 20°

-25°

C.

12. The process of claim 1 wherein the ferrocyanide employed is a mixture salt of equal molar amounts of sodium and potassium ferrocyanides.

13. The process of claim 12 wherein there is added 1/20 to 1/2 mole of ammonium ion per mole of ferrocyanide ion in the reaction mixture at a point between the precipitation of the ferrocyanide white and the beginning of the oxidation.

14. The process of claim 13 wherein the amount of ammonium ion is 1/6 to 1/3 mole per mole of ferrocyanide ion in the reaction mixture.