Process of producing a phthalocyanine pigment

• US 4,158,572 A
• Filed: 10/11/1977
• Issued: 06/19/1979
• Est. Priority Date: 10/15/1976
• Status: Expired due to Term

• Current Assignee: Ciba Specialty Chemicals Corp (BASF SE)
• Original Assignee: Ciba-Geigy Corporation (Novartis Ag)
• Inventors: Blackburn, John B., Irvine, Alexander M., McLaren, George, Sutcliffe, Michael
• Primary Examiner(s): Garvin, Patrick
• Assistant Examiner(s): Howard, J. V.
• Application Number:
  US05/840,886
• Time in Patent Office: 616 Days
• Field of Search: 106/288 Q, 106/309, 106/308 Q, 260/314.5
• US Class Current: 106/412
• CPC Class Codes: C09B 67/0016 of phthalocyanines

Abstract

A process of producing a phthalocyanine pigment comprising dry grinding a crude phthalocyanine, stirring the ground product with an aqueous medium containing a surfactant and isolating the pigmentary product which, when dispersed into surface coating media, provide colorations having high brillance and depth of shade.

Claims

1. A process of producing a β

-phthalocyanine pigment comprising

(a) dry grinding a crude phthalocyanine to obtain an α

-/β

-phthalocyanine,

(b) stirring the product of stage (a) with an aqueous medium, in the absence of an organic solvent, and wherein said aqueous medium contains a surfactant exhibiting a net non-ionic character or said surfactant complexed with an ionic surfactant, to convert said α

-/β

-phthalocyanine to the β

-phthalocyanine form and

(c) isolating the resulting β

-phthalocyanine pigmentary product.

2. A process as claimed in claim 1 wherein the starting material is β

-form copper phthalocyanine as obtained directly from its synthesis.

3. A process as claimed in claim 1 wherein the dry grinding in stage (a) is effected in a ball mill for a sufficient length of time to obtain a crude ground phthalocyanine having a mean primary particle size in the range of from 0.01 to 1 micron.

4. A process as claimed in claim 1 wherein the surfactant in step (b) is a non-ionic surfactant.

5. A process as claimed in claim 4 wherein the non-ionic surfactant is a homo- or copolymer of alkoxylated-acids, -alcohols, -phenols or -amines.

6. A process as claimed in claim 5 wherein the surfactant is a

poly(ethoxylated) C1-C12 alkyl phenol, a

poly(ethoxylated) C10-C18 alcohol, a

poly(ethoxylated) C12-C18 alkyl amine, a

poly(ethoxylated) C10-C18 aliphatic acid or a

poly(ethoxylated) C10-C18 aliphatic acid amine.

7. A process as claimed in claim 1 wherein the amount of surfactant used is from 1 to 30% by weight, based on the weight of the phthalocyanine starting material.

8. A process as claimed in claim 1 wherein the process of step (b) is effected at a temperature within the range of from 25°

C. to the boil.

9. A process as claimed in claim 1 wherein the non-ionic surfactant which is used to convert α

/β

copper phthalocyanine to β

copper phthalocyanine pigment is complexed with an ionic surfactant.

10. A process as claimed in claim 9 wherein the ionic surfactant is a polymeric carboxylic acid.

11. A process as claimed in claim 9 wherein the complex formation is effected by adding a solution of the ionic surfactant to the slurry formed by mixing the pigment and the non-ionic surfactant solution and reducing the pH value of the mixture by the addition of acid, until the slurry is flocculated to an extent sufficient to allow isolation of the pigment by filtration.

12. A process as claimed in claim 11 wherein the pH value to which the slurry is reduced is within the range of 1.0 to 2.5.

13. A process as claimed in claim 1 wherein there is added during step (b) one or more agents known to improve the applicational properties of a pigment.

14. A process as claimed in claim 1 wherein the stage (c) is effected by acidifying the mixture, filtering off the solid pigmentary material and washing it free from water-soluble materials prior to drying it.