Toner processes

• US 5,827,633 A
• Filed: 07/31/1997
• Issued: 10/27/1998
• Est. Priority Date: 07/31/1997
• Status: Expired due to Term

• Current Assignee: Xerox Corporation (Xerox Holdings Corp.)
• Original Assignee: Xerox Corporation (Xerox Holdings Corp.)
• Inventors: Ong, Beng S., Patel, Raj D.
• Primary Examiner(s): MARTIN, ROLAND E
• Application Number:
  US08/903,694
• Time in Patent Office: 453 Days
• Field of Search: 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

Abstract

A process for the preparation of toner comprising

(i) preparing, or providing an aqueous colorant dispersion, which dispersion is comprised of a colorant and an ionic surfactant in water;

(ii) blending said colorant dispersion with a latex emulsion comprised of resin particles, a nonionic surfactant, and an ionic surfactant of opposite charge polarity to that of the ionic surfactant in said colorant dispersion;

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

(iv) heating the resulting aggregate suspension of (iii) above about the Tg of the latex resin; and

(v) retaining the temperature in the range of from about 30° C. to about 95° C., and subsequently, adding an aqueous solution of boric acid, or an aqueous solution of a metal salt; adjusting the pH of the resulting reaction mixture to from about 9 to about 12 by the addition of a base, followed by the addition of a salicylic acid or catechol; and optionally

(vi) isolating, washing and drying the toner obtained.

Claims

1. A process for the preparation of toner comprising

(i) preparing, or providing an aqueous colorant dispersion, which dispersion is comprised of a colorant and an ionic surfactant in water;

(ii) blending said colorant dispersion with a latex emulsion comprised of resin particles, a nonionic surfactant, and an ionic surfactant of opposite charge polarity to that of the ionic surfactant in said colorant dispersion;

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

(iv) heating the resulting aggregate suspension of (iii) above about the Tg of the latex resin; and

(v) retaining the temperature in the range of from about 30°

C. to about 95°

C., and subsequently, adding an aqueous solution of boric acid, or an aqueous solution of a metal salt;

adjusting the pH of the resulting reaction mixture to from about 9 to about 12 by the addition of a base, followed by the addition of a salicylic acid or catechol; and

optionally

(vi) isolating, washing and drying the toner obtained.

4. A process in accordance with claim 1 wherein the product toner size is from about 2 to about 15 microns in volume average diameter, and wherein the particle size distribution of the aggregates is from about 1.12 to about 1.35.

5. A process in accordance with claim 1 wherein the surfactant in the colorant dispersion is a cationic surfactant, and the ionic surfactant present in the latex emulsion is an anionic surfactant.

6. A process in accordance with claim 1 wherein the surfactant in the colorant dispersion is an anionic surfactant, and the ionic surfactant present in the latex emulsion is a cationic surfactant.

8. A process in accordance with claim 1 wherein the heating of the blend of latex, colorant, and surfactants in the aggregation (iii) is accomplished at a temperature of from about 15°

C. to about 1°

C. below the Tg of the latex resin for a duration of from about 0.5 hour to about 6 hours; and

wherein the heating of the aggregate suspension in the coalescence (iv) forms integral toner particles comprised of resin, colorant, and surfactants, and on the toner surface a charge control agent functionality derived from the reaction of said boric acid or a metal salt with said salicylic acid or said catechol.

9. A process in accordance with claim 1 wherein the latex emulsion is generated from the emulsion polymerization of vinyl monomers selected from the group consisting of styrene and substituted styrenes, 1,3-dienes, acrylates, methacrylates, acrylonitrile, acrylic acid, and methacrylic acid.

10. A process in accordance with claim 1 wherein the latex resin is 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), and 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-acrylonitrile), and poly(styrene-butyl acrylate-acrylonitrile-acrylic acid); and

wherein the resin is optionally present in an effective amount ranging from 80 percent by weight to about 98 percent by weight of toner.

11. A process in accordance with claim 1 wherein the resin is selected from the group consisting of poly(styrene-butadiene-acrylic acid) poly(styrene-butadiene-methacrylic acid), poly(styrene-butyl methacrylate-acrylic acid), poly(styrene-butyl acrylate-acrylic acid), poly(styrene-butyl acrylate-acrylonitrile), poly(styrene-butyl acrylate-acrylonitrile-acrylic acid), and poly(styrene-butadiene-acrylonitrile-acrylic acid).

12. A process in accordance with claim 1 wherein the nonionic surfactant present in the latex emulsion is selected from the group consisting of polyvinyl alcohol, methalose, methyl cellulose, ethyl cellulose, propyl cellulose, hydroxy ethyl cellulose, carboxy methyl cellulose, 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;

wherein the anionic surfactant is selected from the group consisting of sodium dodecyl sulfate, sodium dodecylbenzene sulfate and sodium dodecylnaphthalene sulfate, and wherein the ionic surfactant is a quaternary ammonium salt.

13. A process in accordance with claim 1 wherein the colorant is carbon black, magnetite, cyan, yellow, magenta, or mixtures thereof.

14. A process in accordance with claim 1 wherein the latex size is from about 0.05 to about 1 micron in average volume diameter;

and the colorant particle size is from about 0.01 to about 1 micron in volume average diameter.

15. A process in accordance with claim 1 wherein the nonionic, anionic and cationic surfactants are each present in an amount of from about 0.01 to about 5 weight percent of the total reaction mixture.

16. A process in accordance with claim 1 wherein for the toner surface modification (v) there is selected a salicylic acid in an amount of from about 0.05 to about 5 percent by weight of toner and a metal salt of zinc or chromium in an amount of from about 0.05 to about 5 percent by weight of toner.

17. A process in accordance with claim 1 wherein for the toner surface modification (v) there is selected a catechol in an amount of from about 0.05 to about 5 percent by weight of toner and a metal salt of zinc or chromium in an amount of about 0.05 to about 5 percent by weight of toner.

18. A process in accordance with claim 1 wherein there is added to the surface of the formed toner 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.

19. A process in accordance with claim 1 wherein the resin Tg is from about 45°

C. to about 65°

C.;

wherein the latex resin is derived from emulsion polymerization of styrene, butyl acrylate, and acrylic acid;

wherein the latex resin is derived from emulsion polymerization of styrene, butadiene, and acrylic acid;

wherein the latex resin is derived from emulsion polymerization of styrene, butyl acrylate, acrylonitrile, and acrylic acid;

or wherein the latex resin is derived from emulsion polymerization of styrene, butadiene, acrylonitrile, and acrylic acid.

2. A process for the preparation of toner comprising blending a colorant dispersion and a latex emulsion, and wherein the colorant dispersion contains an ionic surfactant, the latex contains a nonionic surfactant and an ionic surfactant of opposite charge polarity to that of ionic surfactant in the colorant dispersion;

heating the resulting mixture whereby aggregates form;

further heating said aggregate suspension;

followed by adjusting the pH of the reaction mixture to be from about 9 to about 12; and

then adding an aqueous solution of a metal salt, followed by the addition of a salicylic acid or a catechol; and

optionally isolating, washing and drying the toner.

3. A process in accordance with claim 2 wherein there is accomplished a heating of the resulting mixture at a temperature of from about 30°

C. to about 60°

C. to effect formation of aggregates of a particle size of from about 2 to about 10 microns in volume average diameter;

thereafter heating the formed aggregate suspension in the presence of a stabilizer agent to prevent, or minimize the aggregates from growing in size, which heating is at a temperature of from about 65°

C. to about 105°

C.;

subsequently maintaining the temperature at from about 30°

C. to about 90°

C.;

adding said base component to maintain the pH of the reaction mixture to be from about 9 to about 12; and

then adding a metal salt of aluminum, zinc, or chromium, followed by the addition of said salicylic acid or catechol; and

isolating the toner product.

7. A process in accordance with claim 2 wherein the ionic surfactant in the colorant dispersion is a cationic surfactant, and the ionic surfactant present in the latex emulsion is an anionic surfactant;

or wherein the surfactant in the colorant dispersion is an anionic surfactant, and the ionic surfactant present in the latex emulsion is a cationic surfactant.

20. A process comprising (i) mixing a colorant dispersion, which dispersion is comprised of a colorant and an ionic surfactant in water and a latex emulsion comprised of resin, a nonionic surfactant and an ionic surfactant of opposite charge polarity to that of the ionic surfactant in said colorant dispersion;

(ii) heating the resulting mixture below about the glass transition temperature (Tg) of the latex resin;

(iii) heating the resulting suspension of (ii) above about the Tg of the latex resin; and

(iv) subsequently adding an aqueous solution of boric acid or a metal salt;

adding a base, followed by the addition of a salicylic acid or catechol; and

optionally

(vi) isolating, washing and drying the toner obtained.

21. A process in accordance with claim 20 wherein a reaction is accomplished between the boric acid and carboxylic acid groups present on the toner surface, followed by the reaction of said boron ion with said added salicylic acid, or said catechol.

22. A process in accordance with claim 20 wherein a reaction is accomplished between the metal ion of said metal salt and carboxylic acid groups present on the toner surface, followed by the reaction of said metal ion with said added salicylic acid, or said catechol.