Two-step milling process for preparing pigmentary copper phthalocyanine

• US 4,257,951 A
• Filed: 03/24/1980
• Issued: 03/24/1981
• Est. Priority Date: 07/31/1979
• Status: Expired due to Term

• Current Assignee: TOYO Ink Manufacturing Company Limited
• Original Assignee: E. I. du Pont de Nemours and Company (Corteva, Inc.)
• Inventors: Matrick, Howard
• Primary Examiner(s): Randolph, John D.
• Application Number:
  US06/128,458
• Time in Patent Office: 365 Days
• Field of Search: 260/314.5, 106/288 Q, 106/309
• US Class Current: 540/141
• CPC Class Codes: C09B 67/0016 of phthalocyanines
• CPC Class Codes: C09B 67/0023 of phthalocyanines

Abstract

Converting crude copper phthalocyanine (CPC) to pigmentary copper phthalocyanine (CPC) by two-stage milling with 5-400% by weight of alum and 0.6-3.7 cc of organic liquid per 100 grams of CPC in the first stage and 1.2-9.8 cc of organic liquid per 100 grams of CPC in the second stage with the total organic liquid being 4-13 cc per 100 grams CPC.

Claims

1. A two-stage milling process for preparing pigmentary copper phthalocyanine comprising milling crude copper phthalocyanine with a 5-400% by weight of Al₂ (SO₄)₃.15-18 H₂ O based on the crude and 0.6-3.7 cc per 100 grams of copper phthalocyanine of an organic liquid in the first stage, milling said crude further with an additional 1.2-9.8 cc per 100 grams of copper phthalocyanine of an organic liquid in a second stage, the total amount of organic liquid charged in both stages is in the range of 4-13 cc inclusive per 100 grams of copper phthalocyanine, treating the milled copper phthalocyanine with an emulsion of a water-insoluble organic liquid in water with or without a surface-active agent at a temperature of 24°

-97°

C. for 15 minutes to 10 hours, removing the organic liquid and recovering copper phthalocyanine in pigmentary form.

2. The process of claim 1 wherein the amount of organic liquid in the first milling stage is 1-3 cc and the amount in the second stage is 2-8 cc.

3. The process of claim 2 wherein the organic liquid in the milling stages is tetrachloroethylene.

4. The process of claim 1 wherein the amount of Al₂ (SO₄)₃.15-18 H₂ O is 25-200% by weight.

5. The process of claim 4 wherein the amount of organic liquid in the first milling stage is 1-3 cc and the amount in the second stage is 2-8 cc.

6. The process of claim 1 wherein the amount of Al₂ (SO₄)₃.15-18 H₂ O is 50-100% by weight.

7. The process of claim 6 wherein the amount of organic liquid in the first milling stage is 1-3 cc and the amount in the second stage is 2-8 cc.

8. The process of claim 1 wherein the organic liquid is tetrachloroethylene.

9. The process of claim 8 wherein the Al₂ (SO₄)₃.15-18 H₂ O is 25-200%.

10. The process of claim 8 wherein the Al₂ (SO₄)₃.15-18 H₂ O is 50-100% by weight.

11. The process of claim 1 wherein the milled copper phthalocyanine is treated in the emulsion formed without a surface-active agent.

12. The process of claim 11 wherein the amount of organic liquid in the first milling stage is 1-3 cc and the amount in the second stage is 2-8 cc.

13. The process of claim 11 wherein the amount of Al₂ (SO₄)₃.15-18 H₂ O is 25-200% by weight.

14. The process of claim 11 wherein the amount of Al₂ (SO₄)₃.15-18 H₂ O is 50-100% by weight.

15. The process of claim 11 wherein the organic liquid is tetrachloroethylene.