Toner processes

• US 5,346,797 A
• Filed: 02/25/1993
• Issued: 09/13/1994
• Est. Priority Date: 02/25/1993
• Status: Expired due to Term

• Current Assignee: Xerox Corporation (Xerox Holdings Corp.)
• Original Assignee: Xerox Corporation (Xerox Holdings Corp.)
• Inventors: Sacripante, Guerino G., Patel, Raj D., Kmiecik-Lawrynowicz, Grazyna E.
• Primary Examiner(s): GOODROW, JOHN L
• Application Number:
  US08/022,575
• Time in Patent Office: 565 Days
• Field of Search: 430/106, 430/108, 430/110, 430/137
• 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 9/0812 Pretreatment of components

Abstract

A process for the preparation of toner compositions comprising

(i) preparing a pigment dispersion in a solvent, which dispersion is comprised of a pigment, an ionic surfactant and optionally a charge control agent;

(ii) shearing the pigment dispersion with a latex mixture comprised of a counterionic surfactant with a charge polarity of opposite sign to that of said ionic surfactant, a nonionic surfactant and resin particles, thereby causing a flocculation or heterocoagulation of the formed particles of pigment, resin and charge control agent to form electrostatically bound toner size aggregates; and

(iii) heating the statically bound aggregated particles to form said toner composition comprised of polymeric resin, pigment and optionally a charge control agent.

Claims

1. A process for the preparation of toner compositions consisting essentially of

(i) preparing a pigment dispersion in a solvent, which dispersion is comprised of a pigment, an ionic surfactant and optionally a charge control agent;

(ii) shearing the pigment dispersion with a latex mixture comprised of a counterionic surfactant with a charge polarity of opposite sign to that of said ionic surfactant, a nonionic surfactant and resin particles, thereby causing a flocculation or heterocoagulation of the formed particles of pigment, resin and charge control agent to form electrostatically bound toner size aggregates; and

(iii) heating the statically bound aggregated particles to form said toner composition comprised of polymeric resin, pigment and optionally a charge control agent.

2. A process in accordance with claim 1 wherein the surfactant utilized in preparing the pigment dispersion is a cationic surfactant, and the counterionic surfactant present in the latex mixture is an anionic surfactant.

3. A process in accordance with claim 1 wherein the surfactant utilized in preparing the pigment dispersion is an anionic surfactant, and the counterionic surfactant present in the latex mixture is a cationic surfactant.

4. A process in accordance with claim 1 wherein the dispersion of step (i) is accomplished by homogenizing at from about 1,000 revolutions per minute to about 10,000 revolutions per minute at a temperature of from about 25°

C. to about 35°

C. and for a duration of from about 1 minute to about 120 minutes.

5. A process in accordance with claim 1 wherein the dispersion of step (i) is accomplished by an ultrasonic probe at from about 300 watts to about 900 watts of energy, at from about 5 to about 50 megahertz of amplitude, at a temperature of from about 25°

C. to about 55°

C., and for a duration of from about 1 minute to about 120 minutes.

6. A process in accordance with claim 1 wherein the dispersion of step (i) is accomplished by microfluidization in a microfluidizer or in nanojet for a duration of from about 1 minute to about 120 minutes.

7. A process in accordance with claim 1 wherein the homogenization of step (ii) is accomplished by homogenizing at from about 1,000 revolutions per minute to about 10,000 revolutions per minute, and for a duration of from about 1 minute to about 120 minutes.

8. A process in accordance with claim 1 wherein the heating of the statically bound aggregate particles to form toner size composite particles comprised of pigment, resin and optional charge control agent is accomplished at a temperature of from about 60°

C. to about 95°

C., and for a duration of from about 1 hour to about 8 hours.

9. A process in accordance with claim 1 wherein the resin particles are selected from the group consisting of poly(styrene-butadiene), poly(para-methyl styrene-butadiene), poly(meta-methyl styrene-butadiene), poly(alpha-methylstyrene-butadiene), poly(methylmethacrylate-butadiene), poly(ethylmethacrylate-butadiene), poly(propylmethacrylate-butadiene), poly(butylmethacrylate-butadiene), poly(methylacrylate-butadiene), poly(ethylacrylate-butadiene), poly(propylacrylate-butadiene), poly(butylacrylate-butadiene), poly(styrene-isoprene), poly(para-methyl styrene-isoprene), poly(metamethyl styrene-isoprene), poly(alpha-methylstyrene-isoprene), poly(methylmethacrylate-isoprene), poly(ethylmethacrylate-isoprene), poly(propylmethacrylate-isoprene), poly(butylmethacrylate-isoprene), poly(methylacrylate-isoprene), poly(ethylacrylate-isoprene), poly(propylacrylate-isoprene), and poly(butylacrylate-isoprene) terpolymers.

10. A process in accordance with claim 1 wherein the resin particles are selected from the group consisting of poly(styrene-butadieneacrylic acid), poly(styrene-butadiene-methacrylic acid), poly(styrene-butyl methacrylate-acrylic acid), or poly(styrene-butyl acrylate-acrylic acid);

PLIOTONE™

, polyethylene-terephthalate, polypropylene-terephthalate, polybutylene-terephthalate, polypentylene-terephthalate, polyhexaleneterephthalate, polyheptadene-terephthalate, and polyoctalene-terephthalate.

11. A process in accordance with claim 1 wherein the resin is comprised of poly(styrene-butadiene).

12. A process in accordance with claim 1 wherein the nonionic surfactant is selected from the group consisting of polyvinyl alcohol, methalose, methyl cellulose, ethyl cellulose, propyl cellulose, hydroxy ethyl cellulose, carboxy methylcellulose, polyoxyethylene cetyl ether, polyoxyethylene lauryl ether, polyoxyethylene octyl ether, polyoxyethylene octylphenyl ether, polyoxyethylene oleyl ether, polyoxyethylene sorbitan monolaurate, polyoxyethylene stearyl ether, polyoxyethylene nonylphenyl ether, and dialkylphenoxy poly(ethyleneoxy)ethanol.

13. A process in accordance with claim 1 wherein the anionic surfactant is selected from the group consisting of sodium dodecylsulfate, sodium dodecylbenzenesulfate and sodium dodecylnaphthalenesulfate.

14. A process in accordance with claim 2 wherein the cationic surfactant is a quaternary ammonium salt.

15. A process in accordance with claim 1 wherein the pigment is carbon black, magnetite, or mixtures thereof;

cyan, yellow, magenta, or mixtures thereof;

or red, green, blue, brown, or mixtures thereof.

16. A process in accordance with claim 1 wherein the resin particles formed in step (ii) are from about 0.01 to 3 microns in average volume diameter.

17. A process in accordance with claim 1 wherein the pigment particles are from about 0.01 to about 3 microns in volume average diameter.

18. A process in accordance with claim 1 wherein the toner particles isolated are from about 3 to 15 microns in average volume diameter, and the geometric size distribution is from about 1.15 to about 1.35.

19. A process in accordance with claim 1 wherein the statically bound aggregate particles formed in step (iii) are from about 1 to about 10 microns in average volume diameter.

20. A process in accordance with claim 1 wherein the nonionic surfactant concentration is about 0.1 to about 5 weight percent of the toner components.

21. A process in accordance with claim 2 wherein the anionic surfactant concentration is about 0.1 to about 5 weight percent of the toner components.

22. A process in accordance with claim 2 wherein the cationic surfactant concentration is about 0.1 to about 5 weight percent of the toner.

23. A process in accordance with claim 1 wherein there is added to the surface of the isolated toner particles surface additives of metal salts, metal salts of fatty acids, silicas, metal oxides, or mixtures thereof, in an amount of from about 0.1 to about 10 weight percent of the obtained toner particles.

24. A process in accordance with claim 1 wherein diluting the flocculated mixture of step (iii) is accomplished with water of from about 50 percent solids to about 15 percent solids.

25. A process in accordance with claim 1 wherein the toner is washed with warm water and the surfactants are removed from the toner surface, followed by drying.

26. A process in accordance with claim 1 wherein the solvent is water.

27. An in situ process for the preparation of toner particles which comprises mixing a dispersion of pigment, ionic surfactant, and optional additives with a latex mixture comprised of a counterionic surfactant with a charge of opposite polarity of said ionic surfactant, resin, and nonionic surfactant, which mixing results in flocculation of pigment, resin, and optional additives;

and heating.

28. An in situ process for the preparation of toner particles comprising

(i) preparing a pigment dispersion in a solvent, which dispersion is comprised of a pigment, an ionic surfactant and optionally a charge control agent;

(ii) shearing the pigment dispersion with a latex mixture comprised of a counterionic surfactant with a charge polarity of opposite sign to that of said ionic surfactant, a nonionic surfactant and resin particles, thereby causing a flocculation or heterocoagulation of the formed particles of pigment, resin and charge control agent to form electrostatically bound toner size aggregates; and

(iii) heating the statically bound aggregated particles to form said toner composition comprised of polymeric resin particles and pigment.