Toner processes

• US 6,627,373 B1
• Filed: 03/25/2002
• Issued: 09/30/2003
• 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: Patel, Raj D., Hopper, Michael A.
• Primary Examiner(s): Goodrow, John
• Application Number:
  US10/106,514
• Publication Number:
  US 20030180650A1
• Time in Patent Office: 554 Days
• Field of Search: 430/137.14, 430/106.2
• US Class Current: 430/137.14
• 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

An emulsion aggregation process for the preparation of a magnetite toner, and where the magnetite can function as a negatively charged coagulant to facilitate aggregation of a basic cationic latex, a cationic carbon black dispersion and a cationic wax dispersion.

Claims

1. A process for the preparation of a magnetic toner comprising the heating of a colorant dispersion comprised of a magnetite dispersion, and a carbon black dispersion, and thereafter mixing with a basic cationic latex emulsion and a wax dispersion, and wherein

(i) said magnetite in said dispersion is an acicular magnetite dispersed in water and a cationic surfactant, or a nonionic surfactant, and said dispersion of carbon black contains water and a cationic surfactant, or a nonionic surfactant, and wherein said dispersion of magnetite and carbon black possesses a pH of about 6.3 to about 6.8, and wherein said latex is an emulsion comprised of a cationic surfactant, water and resin, and which emulsion is at a pH of about 10 to about 11;

(ii) wherein said colorant dispersion is blended with said latex emulsion, and thereafter adding said wax dispersion, and which dispersion is 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 a cationic surfactant;

(iii) wherein the resulting blend possesses a pH of about 8.5 to about 9.5 thereby inducing a negative charge on the magnetite particles to thereby initiate flocculation or aggregation of said resin latex, said colorant, and said wax;

(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 a cationic surfactant and water, and optionally stirring for a period of time to permit stabilization of aggregate particle size;

(vi) adding to the resulting mixture an acid to thereby change the pH, which is initially from about 8.5 to about 9.5, to arrive at a pH of from about 6 to about 6.9 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 to about 6.8;

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

C. to about 95°

C. for an optional period of about 10 to about 60 minutes, followed by a pH increase with a base to arrive at a pH of about 7 to about 8;

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

C. to about 95°

C. for an optional period of about 7 to about 14 hours to assist in permitting the fusion or coalescence of the toner aggregates and to obtain smooth particles;

(x) washing the resulting toner slurry; and

(xi) isolating the toner.

2. A process in accordance with claim 1 wherein one of said colorant dispersions comprises acicular magnetite particles dispersed in water, a cationic surfactant and a nonionic surfactant, and wherein said dispersion possesses a pH of from about 6.5 to about 6.8.

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

4. A process in accordance with claim 1 wherein said magnetite in an acicular magnetite is present in an amount of from about 20 to about 35 percent by weight of toner, and wherein in the presence of a basic cationic latex, said magnetite is negatively charged thereby facilitating aggregation.

5. A process in accordance with claim 1 wherein said magnetite is an acicular magnetite present in an amount of from about 23 to about 32 percent by weight of toner.

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

7. A process in accordance with claim 1 wherein said acicular magnetite with a particle size of about 0.6 micron in length by 0.1 micron in diameter, and is comprised of about 21 percent FeO and about 79 percent Fe₂O₃.

8. 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.

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

C. to about 195°

C.

10. A process in accordance with claim 9 wherein the toner hot offset temperature (HOT) is from about 210°

C. to about 250°

C.

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

12. 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.

13. A process in accordance with claim 1 wherein the latex resin particles are from about 0.15 to about 0.3 micron in volume average diameter.

14. 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.

15. A process in accordance with claim 1 wherein the said acid is selected from the group consisting of nitric, sulfuric, hydrochloric, citric and acetic acid.

16. A process in accordance with claim 1 wherein said base is selected from the group consisting of sodium hydroxide, potassium hydroxide, and ammonium hydroxide.

17. A process in accordance with claim 1 wherein there is added to the formed toner aggregates a second latex comprised of submicron resin particles suspended in an aqueous phase containing a cationic 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.

18. A process in accordance with claim 17 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.

19. A process in accordance with claim 1 (v) wherein the pH of the mixture resulting in (vi) is decreased from about 8.5 to about 9.5 to about 6 to about 6.8 wherein said acid functions primarily as a of stabilizer for the aggregates during coalescence (vii), and no or minimal toner particle size increase results.

20. A process in accordance with claim 1 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 9 microns in volume average diameter.

21. A process in accordance with claim 1 wherein the aggregation (iv) temperature is from about 45°

C. to about 60°

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

C. to about 95°

C.

22. A process in accordance with claim 1 wherein the time of coalescence or fusion is from about 12 to about 20 hours, and wherein there are provided toner particles with a smooth morphology.

23. A process in accordance with claim 1 wherein the latex contains a resin or polymer selected from the group consisting of poly(styrene-propyl acrylate 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride), poly(styrene-butyl acrylate 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride), poly(styrene-alkyl acrylate 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride), poly(styrene-1,3-diene 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride), poly(styrene-alkyl methacrylate 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride), poly(styrene-alkyl acrylate-3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride, poly(styrene-1,3-diene-3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride, poly(styrene-alkyl methacrylate-3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride, poly(alkyl methacrylate-alkyl acrylate-3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride, poly(alkyl methacrylate-aryl acrylate-3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride, poly(aryl methacrylate-alkyl acrylate 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride, poly(alkyl methacrylate-acrylic acid 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride, poly(styrene-alkyl acrylate-acrylonitrile-3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride, poly(styrene-1,3-diene-acrylonitrile-3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride, and poly(alkyl acrylate-acrylonitrile-3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride.

24. A process in accordance with claim 1 wherein the latex contains a resin selected from the group consisting of poly(styrene-butadiene 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride), poly(methylstyrene-butadiene 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride), poly(methyl methacrylate-butadiene 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride), poly(ethyl methacrylate-butadiene 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride), poly(propyl methacrylate-butadiene 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride), poly(butyl methacrylate-butadiene 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride), poly(methyl acrylate-butadiene 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride), poly(ethyl acrylate-butadiene 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride), poly(propyl acrylate-butadiene 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride), poly(butyl acrylate-butadiene 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride), poly(styrene-isoprene 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride), poly(methylstyrene-isoprene 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride), poly(methyl methacrylate-isoprene 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride), poly(ethyl methacrylate-isoprene 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride), poly(propyl methacrylate-isoprene 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride), poly(butyl methacrylate-isoprene 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride), poly(methyl acrylate-isoprene 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride), poly(ethyl acrylate-isoprene 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride), poly(propyl acrylate-isoprene 3 metacryloxy-2-hydroxypropyltrimethyl ammonium chloride), poly(butyl acrylate-isoprene 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride);

poly(styrene-propyl acrylate 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride), poly(styrene-butyl acrylate 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride), poly(styrene-butadiene 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride), poly(styrene-butadiene 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride), poly(styrene-butadiene-acrylonitrile 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride), poly(styrene-butyl acrylate 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride), and poly(styrene-butyl acrylate-acrylononitrile 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride).

25. A process in accordance with claim 1 wherein said magnetite functions as a negatively charged coagulant and is present in an amount of about 22 to about 35 weight percent and is dispersed in a cationic surfactant in an amount of about 0.1 to about 5 weight percent;

said carbon black is present in an amount of about 3 to about 8 percent by weight dispersed in water containing a cationic surfactant in an amount of about 0.1 to about 5 weight percent;

said wax is present in the amount of about 4 to about 12 weight percent dispersed in water containing a cationic surfactant in the amount of about 0.1 to about 5 weight percent; and

the cationic latex is present in an amount of about 40 to about 65 percent by weight.

26. A process in accordance with claim 1 wherein heating is accomplished while mixing.

27. A process in accordance with claim 1 wherein said magnetite dispersion is comprised of about 25 to about 35 percent magnetite, about 65 to about 70 percent water, and about 0.5 to about 2 percent cationic surfactant;

carbon black dispersion comprised of said 4.5 percent carbon black, and about 2 percent cationic surfactant with the remainder being water, and wherein the latex emulsion comprises about 34 percent solids of styrene, 78.8 percent, butylacrylate, 17.3 percent, and 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride, 3.8 percent, and wherein said wax dispersion is comprised of about 30 percent wax, 2 percent cationic surfactant and the remaining percentage being water, wherein the latex contains a resin of poly(styrene-propyl acrylate 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride), poly(styrene-butyl acrylate 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride), poly(styrene-butadiene 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride), poly (styrene-butadiene 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride), poly(styrene-butadiene-acrylonitrile 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride), or poly(styrene-butyl acrylate-acrylononitrile 3-metacryloxy-2-hydroxypropyltrimethyl ammonium chloride) wherein the cationic surfactant is selected from the group consisting of a dialkyl benzenealkyl ammonium chloride, lauryl trimethyl ammonium chloride, alkyl benzyl methyl ammonium chloride, alkyl benzyl dimethyl ammonium bromide, benzalkonium chloride, cetyl pyridinium bromide, C₁₂, C₁₅, C₁₇ trimethyl ammonium bromides, halide salts of quaternized polyoxyethylalkylamines, dodecylbenzyl triethyl ammonium chloride, and wherein the wax selected is a polypropylene, a polyethylene or a carnuba wax.

28. A process in accordance with claim 1 wherein said heating is below about the latex resin glass transition temperature, followed by a heating above about the latex resin glass transition temperature.

29. An imaging method or printing process wherein the toner of claim 1 is selected.