Low shear toner aggregation processes

• US 5,650,255 A
• Filed: 09/03/1996
• Issued: 07/22/1997
• Est. Priority Date: 09/03/1996
• Status: Expired due to Term

• Current Assignee: Xerox Corporation (Xerox Holdings Corp.)
• Original Assignee: Xerox Corporation (Xerox Holdings Corp.)
• Inventors: Torres, Francisco E., Sanders, David J., Patel, Raj D., Kurceba, David, Kmiecik-Lawrynowicz, Grazyna E., Ng, T. Hwee, Helbrecht, Arthur
• Primary Examiner(s): MARTIN, ROLAND E
• Application Number:
  US08/706,880
• Time in Patent Office: 322 Days
• Field of Search: 430/137, 523/334, 523/339
• 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 9/0819 characterised by the dimensions of the particles

Abstract

An in situ chemical process for the preparation of toner comprised of

(i) the provision of a latex, which latex is comprised of polymeric resin particles, an ionic surfactant and a nonionic surfactant;

(ii) providing a pigment dispersion, which dispersion is comprised of a pigment solution, a counterionic surfactant with a charge polarity of opposite sign to that of said ionic surfactant, and optionally a charge control agent;

(iii) mixing said pigment dispersion with said latex with a stirrer equipped with an impeller, stirring at speeds of from about 100 to about 900 rpm for a period of from about 10 minutes to about 150 minutes;

(iv) heating the above resulting blend of latex and pigment mixture to a temperature below about the glass transition temperature (Tg) of the resin to form electrostatically bound toner size aggregates;

(v) adding further aqueous ionic surfactant or stabilizer in the range amount of from about 0.1 percent to 5 percent by weight of reactants to stabilize the above electrostatically bound toner size aggregates;

(vi) heating said electrostatically bound toner sized aggregates above about the Tg of the resin to form toner size particles containing pigment, resin and optionally a charge control agent;

(vii) optionally isolating said toner, optionally washing with water; and optionally

(viii) drying said toner.

Claims

1. An in situ chemical process for the preparation of toner comprised of

(i) the provision of a latex, which latex is comprised of polymeric resin particles, an ionic surfactant and a nonionic surfactant;

(ii) providing a pigment dispersion, which dispersion is comprised of a pigment, a dispersing liquid, a counterionic surfactant with a charge polarity of opposite sign to that of said ionic surfactant, and optionally a charge control agent;

(iii) mixing said pigment dispersion with said latex with a stirrer equipped with an impeller, stirring at speeds of from about 100 to about 900 rpm for a period of from about 10 minutes to about 150 minutes;

(iv) heating the above resulting blend of latex and pigment dispersion to a temperature below about the glass transition temperature (Tg) of the resin to form electrostatically bound toner size aggregates;

(v) adding further aqueous ionic surfactant or stabilizer in the range amount of from about 0.1 percent to 5 percent by weight of reactants to stabilize the above electrostatically bound toner size aggregates;

(vi) heating said electrostatically bound toner sized aggregates above about the Tg of the resin to form toner size particles containing pigment, resin and optionally a charge control agent;

(vii) optionally isolating said toner, optionally washing with water; and

optionally

(viii) drying said toner.

2. A process in accordance with claim 1 (iii) wherein the mixing is from about 150 to about 600 rpm for a duration of from about 30 minutes to about 90 minutes.

3. A process in accordance with claim 1 (ii) wherein the counterionic surfactant for the pigment dispersion is a cationic surfactant, and the ionic surfactant present in the latex mixture is an anionic surfactant.

4. A process in accordance with claim 1 (iii) wherein the mixing is accomplished with impellers operating at speeds of from about 150 to about 600 rpm.

5. A process in accordance with claim 1 wherein the dispersion of (ii) is prepared with stirring at speeds of from about 100 revolutions per minute to about 900 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 60 minutes.

6. A process in accordance with claim 1 wherein the charge control agent is dispersed in the stabilizer in (v).

7. A process in accordance with claim 1 wherein the heating of the blend comprising latex, pigment, surfactants and optional charge control agent in (iv) is accomplished at temperatures of from about 20°

C. to about 5°

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

8. A process in accordance with claim 1 (vi) wherein the heating of the statically bound toner 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 10°

C. above the Tg of the resin to about 95°

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

9. A process in accordance with claim 1 (i) wherein the resin is selected from the group consisting of poly(styrene-butadiene), poly(para-methyl styrene-butadiene), poly(meta-methylstyrene-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(meta-methylstyrene-isoprene), poly(alpha-methylstyrene-isoprene), poly(methylmethacrylate-isoprene), poly(ethylmethacrylate-isoprene), poly(propylmethacrylate-isoprene), poly(butyl methacrylate-isoprene), poly(methylacrylate-isoprene), poly(ethylacrylate-isoprene), poly(propylacrylate-isoprene), and poly(butylacrylate-isoprene), and wherein each of said resins contain acrylic acid.

10. A process in accordance with claim 1 (i) wherein the nonionic surfactant 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, the anionic surfactant is selected from the group consisting of sodium dodecyl sulfate, sodium dodecylbenzene sulfate, and sodium dodecylnaphthalene sulfate, and the counterionic surfactant is a cationic surfactant of a quaternary ammonium salt.

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

12. A process in accordance with claim 1 wherein the toner isolated is from about 2 to about 15 microns in volume average diameter, the geometric size distribution (GSD) thereof is narrow and is from about 1.15 to about 1.20, and the aggregates formed in (iv) are from about 1 to about 10 microns in volume average diameter.

13. A process in accordance with claim 1 wherein the nonionic surfactant concentration is from about 0.1 to about 5 weight percent;

the anionic surfactant concentration is about 0.1 to about 5 weight percent; and

the cationic surfactant concentration is about 0.1 to about 5 weight percent of the toner components of resin, pigment and charge control agent.

14. A process in accordance with claim 1 wherein the toner is isolated and dried, and thereafter there is added to said toner surface metal salts, metal salts of fatty acids, silicas, metal oxides, or mixtures thereof, each in an amount of from about 0.1 to about 10 weight percent of the formed toner.

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

16. A process in accordance with claim 10 wherein the nonionic surfactant is linear or branched.

17. A process in accordance with claim 1 wherein heating in (iv) is from about 5°

C. to about 25°

C. below the resin Tg, or wherein said heating in (iv) is accomplished at a temperature of from about 29°

C. to about 59°

C., and wherein heating in (vi) is from about 5°

to about 50°

C. above the Tg, and wherein the resin Tg in (vi) is from about 50°

to about 80°

C.

22. A process in accordance with claim 1 wherein said resin is of submicron size of from about 0.001 to about 0.99 micron in volume average diameter.

18. A process for the preparation of pigmented toner size particles comprised of mixing a pigment dispersion with a latex, which mixing is accomplished with stirring at speeds of from about 100 to about 900 revolutions per minute and wherein the pigment dispersion is comprised of a pigment, a dispersing liquid containing a pigment dispersion component, a counterionic surfactant with a charge polarity of opposite sign to that of the ionic surfactant, and optionally a charge control agent;

and wherein the latex is comprised of submicron polymeric resin particles, an ionic surfactant and a nonionic surfactant;

heating the above formed blend of latex and pigment dispersion to a temperature below about the glass transition temperature (Tg) of the resin to form toner aggregates;

adding further ionic surfactant or stabilizer in the range amount of from about 0.1 percent to about 5 percent by weight of latex and resin components to stabilize said aggregates; and

thereafter, heating the toner aggregates above about the resin Tg.

19. A process in accordance with claim 18 wherein the stirrer is an impeller operating at speeds of from about 100 to about 900 rpm for a period of from 10 minutes to about 150 minutes.

20. A process in accordance with claim 18 wherein said submicron is less than about 1 micron.

21. A process in accordance with claim 18 wherein said submicron is from about 0.001 to about 0.99 micron in volume average diameter.

23. A process for the preparation of toner, which process comprises the mixing of a pigment dispersion with a latex and which mixing is accomplished at low stirring speeds of from about 100 to about 900 revolutions per minute, and wherein the pigment dispersion is comprised of a pigment, a dispersing liquid containing a pigment dispersion component, and a counterionic surfactant with a charge polarity of opposite sign to that of the ionic surfactant;

and wherein the latex is comprised of polymeric resin particles, an ionic surfactant, and a nonionic surfactant;

a first heating of the above formed blend of latex and pigment dispersion to a temperature below about, or at the glass transition temperature (Tg) of the resin, to form aggregates;

optionally adding further ionic surfactant or stabilizer;

thereafter a second heating of the toner aggregates above about, or at the resin Tg;

isolating and drying said toner.

24. A process in accordance with claim 23 wherein there is added further ionic surfactant or stabilizer in the amount of from about 0.1 percent to about 5 percent by weight of latex and resin components to stabilize said aggregates;

and wherein the first heating is below the resin Tg, and the second heating is above the resin Tg.

25. A process in accordance with claim 23 wherein said resin is submicron in size and said submicron is from about 0.001 to about 0.99 microns in volume average diameter.