Magnetite toner processes

• US 6,656,658 B2
• Filed: 03/25/2002
• Issued: 12/02/2003
• Est. Priority Date: 03/25/2002
• Status: Expired due to Fees

• Current Assignee: Xerox Corporation (Xerox Holdings Corp.)
• Original Assignee: Xerox Corporation (Xerox Holdings Corp.)
• Inventors: Zwartz, Edward G., Bartel, Joseph, Patel, Raj D., Hopper, Michael A.
• Primary Examiner(s): Goodrow, John
• Application Number:
  US10/106,512
• Publication Number:
  US 20030180649A1
• Time in Patent Office: 617 Days
• Field of Search: 430/137.14, 430/106.2, 523/335
• US Class Current: 430/137.14
• CPC Class Codes: C08J 3/2053 the additives only being premixed with a liquid phase
• CPC Class Codes: G03G 9/0804 whereby the components are brought together in a liquid dispersing medium
• CPC Class Codes: G03G 9/0821 characterised by physical parameters magnetic parameters G03G9/083
• CPC Class Codes: G03G 9/0833 Oxides
• CPC Class Codes: G03G 9/08782 Waxes
• CPC Class Codes: G03G 9/0904 Carbon black

Abstract

A toner process comprising heating an acidified dispersion of an acicular magnetite, a carbon black colorant dispersion, an optional wax dispersion, and an acicular latex.

Claims

1. A toner process comprising heating a mixture of an acidified dispersion of an acicular magnetite with a colorant dispersion of carbon black, a wax dispersion, and an acidic latex emulsion, and wherein said heating comprises a first heating and a second heating, and wherein the second heating is at a higher temperature than the first temperature;

and wherein said second heating is equal to about or above about the glass transition temperature of a polymer contained in said acidic latex.

2. A process in accordance with claim 1 wherein said acidified dispersion of said acicular magnetite particles contains water, and an anionic surfactant wherein said acidified dispersion is at a pH of about 1.8 to about 2.2, and which pH is achieved by the addition of an acid, resulting in inducing a positive charge on the surface of the magnetite particles and subsequently adding said dispersion of carbon black containing water, carbon black and an anionic surfactant, and thereafter adding said wax dispersion comprised of submicron wax particles of from about 0.1 to about 0.5 micron in diameter by volume, and which wax is dispersed in an anionic surfactant;

(ii) mixing said magnetite, carbon black, and wax dispersions with said latex emulsion comprised of an anionic surfactant, water and resin, and which emulsion is at a pH of about 1.5 to about 2.3;

(iii) wherein the resulting blend possesses a pH of about 2 to about 2.2 thereby retaining sufficient positive charge on the magnetite particles to initiate flocculation or aggregation of said magnetite, carbon black, wax and resin latex;

(iv) heating the resulting mixture below about the glass transition temperature (Tg) of the latex resin to form toner sized aggregates;

(v) optionally adding to the formed toner aggregates a second latex comprised of resin suspended in an aqueous phase containing an anionic surfactant and water, which second latex possesses a pH of about 1.5 to about 2.2 and stirring to enable the incorporation of the second latex on the aggregate surface thereby providing a shell;

(vi) adding to the resulting mixture a base to thereby change the pH which is initially from about 1.8 to about 2.2 to a pH of from about 6.9 to about 7.3 for the resulting toner aggregate mixture;

(vii) heating the resulting aggregate suspension of (vi) above about the Tg of the latex resin of (i), while maintaining the pH at a value of about 6.9 to about 7.3;

(viii) optionally retaining the mixture temperature at from about 85°

C. to about 95°

C., followed by a pH reduction with an acid to arrive at a pH of about 5.3 to about 5.8;

(ix) optionally retaining the mixture temperature at from about 85°

C. to about 95°

C. to obtain smooth toner particles; and

(x) isolating the toner.

3. A process in accordance with claim 1 wherein said magnetite dispersion comprises acicular magnetite particles dispersed in water, an anionic surfactant, and optionally a nonionic surfactant wherever said dispersion possesses an initial pH of from about 6.5 to about 6.8, which magnetite dispersion is then acidified to a pH of about 1.8 to about 2.2 resulting in an induction of a positive charge of about +35 to about +45 coulombs/cm² on the magnetite particles.

4. A process in accordance with claim 1 wherein said carbon black dispersion comprises carbon black particles dispersed in water and an anionic surfactant, and which dispersion possesses a pH of about 6.3 to about 6.8.

5. A process in accordance with claim 1 wherein said acidified dispersion contains acicular magnetite in an amount of from about 22 to about 35 percent by weight of toner, and wherein in the presence of an acidic anionic latex said magnetite is positively charged.

6. A process in accordance with claim 1 wherein said acicular magnetite is present in an amount of from about 23 to about 32 percent by weight of toner, and wherein in the presence of an acidic environment at a pH of about 1.8 to about 3.5, said magnetite possesses a positive charge, thereby also functioning as a coagulant.

7. A process in accordance with claim 1 wherein said acicular magnetite exhibits a coercivity of from about 250 to about 700 Oe.

8. A process in accordance with claim 1 wherein said acicular or needle shape magnetite particles has a particle size of about 0.6 micron in length by 0.1 micron in diameter.

9. A process in accordance with claim 1 wherein said toner exhibits a magnetic signal of from about 115 to about 150 percent of the nominal signal.

10. A process in accordance with claim 1 wherein the toner possesses a minimum fix temperature (MFT) of about 170°

C. to about 195°

C.

11. A process in accordance with claim 10 wherein the toner hot offset temperature (HOT) is about 210°

C. to about 250°

C.

12. A process in accordance with claim 1 wherein the magnetite dispersion is obtained by a ball milling, attrition, polytroning, homogenizing or media milling resulting in magnetite particles dispersed in water containing an anionic surfactant.

13. A process in accordance with claim 1 wherein the carbon black dispersion is present in an amount of about 4 to about 8 percent by weight of toner.

14. A process in accordance with claim 1 wherein the latex emulsion contains resin particles of from about 0.15 to about 0.3 micron in volume average diameter.

15. A process in accordance with claim 1 wherein said magnetite is of a size of about 0.6 micron to about 0.1 micron, and said carbon black is of a size of about 0.01 to about 0.2 micron each in average volume diameter.

16. A process in accordance with claim 2 wherein said acid is selected from the group consisting of nitric, sulfuric, hydrochloric, citric and acetic acid.

17. A process in accordance with claim 2 wherein said base is selected from the group consisting of sodium hydroxide, potassium hydroxide, and ammonium hydroxide.

18. A process in accordance with claim 2 wherein there is added to the formed toner aggregates a second latex comprised of submicron resin particles suspended in an aqueous phase containing an anionic surfactant, and wherein said second latex is selected in an amount of from about 10 to about 40 percent by weight of the initial latex to form a shell thereover on said formed aggregates, and which shell is of a thickness of about 0.2 to about 0.8 micron.

19. A process in accordance with claim 18 wherein the added latex contains the same resin as the initial latex of (i), or wherein said added latex contains a dissimilar resin than that of the initial latex.

20. A process in accordance with claim 2 (v) wherein the pH of the mixture resulting in (vi) is increased from about 2 to about 2.6 to about 6.5 to about 7.2, and wherein said base functions primarily as a stabilizer for the aggregates during coalescence, and no or minimal toner particle size increase results.

21. A process in accordance with claim 2 wherein the temperature at which toner sized aggregates are formed controls the size of the aggregates, and wherein the final toner size is from about 5 to about 12 microns in volume average diameter.

22. A process in accordance with claim 2 wherein the aggregation (iv) temperature is from about 45°

C. to about 60°

C., and wherein the coalescence temperature of (vii) is from about 85°

C. to about 95°

C.

23. A process in accordance with claim 2 wherein the time of coalescence or fusion is from about 6 to about 15 hours, and wherein there are provided toner particles with a smooth morphology.

24. A process in accordance with claim 1 wherein the latex contains a resin or polymer selected from the group consisting of poly(styrene-alkyl acrylate), poly(styrene-1,3-diene), poly(styrene-alkyl methacrylate), poly(styrene-alkyl acrylate-acrylic acid), poly(styrene-1,3-diene-acrylic acid), poly(styrene-alkyl methacrylate-acrylic acid), poly(alkyl methacrylate-alkyl acrylate), poly(alkyl methacrylate-aryl acrylate), poly(aryl methacrylate-alkyl acrylate), poly(alkyl methacrylate-acrylic acid), poly(styrene-alkyl acrylate-acrylonitrile-acrylic acid), poly(styrene-1,3-diene-acrylonitrile-acrylic acid), and poly(alkyl acrylate-acrylonitrile-acrylic acid).

25. A process in accordance with claim 2 wherein the latex contains a resin selected from the group consisting of poly(styrene-butadiene), poly(methylstyrene-butadiene), poly(methyl methacrylate-butadiene), poly(ethyl methacrylate-butadiene), poly(propyl methacrylate-butadiene), poly(butyl methacrylate-butadiene), poly(methyl acrylate-butadiene), poly(ethyl acrylate-butadiene), poly(propyl acrylate-butadiene), poly(butyl acrylate-butadiene), poly(styrene-isoprene), poly(methylstyrene-isoprene), poly(methyl methacrylate-isoprene), poly(ethyl methacrylate-isoprene), poly(propyl methacrylate-isoprene), poly(butyl methacrylate-isoprene), poly(methyl acrylate-isoprene), poly(ethyl acrylate-isoprene), poly(propyl acrylate-isoprene), poly(butyl acrylate-isoprene);

poly(styrene-propyl acrylate), poly(styrene-butyl acrylate), poly(styrene-butadiene-acrylic acid), poly(styrene-butadiene-methacrylic acid), poly(styrene-butadiene-acrylonitrile-acrylic acid), poly(styrene-butyl acrylate-acrylic acid), poly(styrene-butyl acrylate-methacrylic acid), poly(styrene-butyl acrylate-acrylononitrile), and poly(styrene-butyl acrylate-acrylononitrile-acrylic acid).

26. A process in accordance with claim 1 wherein the acidification of the magnetite dispersion comprised of acicular magnetite particles, water, and an anionic surfactant possesses a positive charge and functions as a colorant and as a coagulant, and wherein said acidic pH is from about 1 to about 6.

27. A process in accordance with claim 1 wherein the latex comprises about 40 percent solids, about 1.3 percent anionic surfactant, and water;

the magnetite dispersion comprises about 30 percent magnetite, about 1.3 percent anionic surfactant, and water, and the wax is a polypropylene, a polyethylene, a carnuba wax, and mixtures thereof.

31. A process in accordance with claim 1 wherein there is further included in said mixture a coagulant.

28. A toner process comprising heating an acidified dispersion of an acicular magnetite, a carbon black colorant dispersion, an optional wax dispersion, and a latex, and which heating comprises a first heating and a second heating, and wherein the first heating is accomplished below the glass transition temperature (Tg) of a resin contained in said latex, and wherein the second heating is above the glass transition temperature of a resin contained in said latex.

29. A process in accordance with claim 28 wherein said acidified dispersion is at a pH of about 1 to about 5.

30. A process in accordance with claim 28 wherein acidified is at a pH of about 2 to about 4.

32. A toner process consisting essentially of heating a mixture of an acidified dispersion of an acicular magnetite with a colorant dispersion of carbon black, a wax dispersion, and an acidic latex emulsion, and wherein said heating comprises a first heating and a second heating, and wherein the second heating is at a higher temperature than the first heating;

and wherein said first heating is equal to about or above about the glass transition temperature of a polymer contained in said latex.