Toner aggregation processes

• US 5,366,841 A
• Filed: 09/30/1993
• Issued: 11/22/1994
• Est. Priority Date: 09/30/1993
• Status: Expired due to Term

• Current Assignee: Xerox Corporation (Xerox Holdings Corp.)
• Original Assignee: Xerox Corporation (Xerox Holdings Corp.)
• Inventors: Patel, Raj D., Kmiecik-Lawrynowicz, Grazyna E., Hopper, Michael A., Croucher, Melvin D.
• Primary Examiner(s): MARTIN, ROLAND E
• Application Number:
  US08/129,476
• Time in Patent Office: 418 Days
• Field of Search: 430/137, 523/322, 523/335, 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 9/0812 Pretreatment of components
• CPC Class Codes: G03G 9/0815 Post-treatment

Abstract

A process for the preparation of toner compositions comprising:

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

(ii) shearing the pigment dispersion with a latex blend comprised of resin particles, a counterionic surfactant with a charge polarity of opposite sign to that of said ionic surfactant and a nonionic surfactant thereby causing a flocculation or heterocoagulation of the formed particles of pigment, resin and charge control agent to form a uniform dispersion of solids in the water, and surfactant;

(iii) heating the above sheared blend at a critical temperature region about equal to or above the glass transition temperature (Tg) of the resin, while continuously stirring, to form electrostatically bounded toner size aggregates with a narrow particle size distribution and wherein said critical temperature is from about 0° C. to about 10° C. above the resin Tg, and wherein the resin Tg is from about 30° C. to about 65° C. and preferably in the range of from about 45° C. to about 65° C.;

(iv) heating the statically bound aggregated particles from about 10° C. to about 45° C. above the Tg of the resin particles to provide a toner composition comprised of polymeric resin, pigment and optionally a charge control agent; and

(v) optionally separating and drying said toner.

Claims

1. A process for the preparation of toner compositions comprising:

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

(ii) shearing the pigment dispersion with a latex blend comprised of resin particles, a counterionic surfactant with a charge polarity of opposite sign to that of said ionic surfactant and a nonionic surfactant thereby causing a flocculation or heterocoagulation of the formed particles of pigment, resin and optional charge control agent to form a uniform dispersion of solids in the water, and surfactant;

(iii) heating the uniform disperion of solids in water and surfactant of (ii) at a critical temperature region about equal to or above the glass transition temperature (Tg) of the resin, while continuously stirring, to form electrostatically bounded toner size aggregates with a narrow particle size distribution and wherein said critical temperature is from about 0°

C. to about 10°

C. above the resin Tg, and wherein the resin Tg is from about 30°

C. to about 65°

C. and preferably in the range of from about 45°

C. to about 65°

C.;

(iv) heating the electrostatically bounded toner size aggregates from about 10°

C. to about 45°

C. above the Tg of the resin particles to provide a toner composition comprised of polymeric resin, pigment and optionally a charge control agent; and

(v) optionally separating and drying said toner.

2. A process in accordance with claim 1 wherein the temperature of the stirring in the critical resin Tg temperature region (iii) controls the size of the aggregated particles in the range of from about 4 to about 15 microns in average volume diameter.

3. A process in accordance with claim 1 wherein aggregate particles with narrow size distribution are obtained by performing step (iii) for from about 1 to about 2 hours, and wherein the temperature above the resin Tg is about 10°

C.

4. A process in accordance with claim 1 wherein toner with a particle size of about 4 to about 15 microns in average volume diameter can be obtained by performing step (iii) within from about 5°

C. to about 10°

C. of the resin Tg.

5. A process in accordance with claim 1 wherein the aggregation in (iii) is kinetically controlled.

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

7. A process in accordance with claim 1 wherein the dispersion of step (i) is accomplished by homogenizing at from about 1,000 revolution per minute to about 10,000 revolutions per minute, or by microfluidization in a microfluidizer or in nanojet, or by an ultrasonic probe at from about 300 watts to about 900 watts of energy at a temperature of from about 25°

C. to about 35°

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

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

9. A process in accordance with claim 1 wherein the heating of the blend of latex, pigment, surfactants and optional charge control agent in step (iii) is accomplished at temperatures of from about 5°

C. to about 8°

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

10. 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 15°

C. to about 95°

C. above the Tg of the resin for a duration of from about 1 to about 8 hours.

11. A process in accordance with claim 1 wherein the resin is selected from the group consisting of poly(styrene-butadiene), poly(paramethyl styrene-butadiene), poly(meta-methyl styrene-butadiene), poly(alpha-methylstyrene-butadiene), poly(methylmethacrylatebutadiene), poly(ethylmethacrylate-butadiene), poly(propylmethacrylatebutadiene), poly(butylmethacrylate-butadiene), poly(methylacrylatebutadiene), poly(ethylacrylate-butadiene), poly(propylacrylate-butadiene), poly(butylacrylate-butadiene), poly(styrene-isoprene), poly(paramethylstyrene-isoprene), poly(meta-methylstyrene-isoprene), poly(alphamethylstyrene-isoprene), poly(methylmethacrylate-isoprene), poly(ethylmethacrylate-isoprene), poly(propylmethacrylate-isoprene), poly(butylmethacrylate-isoprene), poly(methylacrylate-isoprene), poly(ethylacrylate-isoprene), poly(propylacrylate-isoprene), and poly(butylacrytate-isoprene).

12. 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 methacrylateacrylic acid), poly(styrene-butyl acrylate-acrylic acid), polyethyleneterephthalate, polypropylene-terephthalate, polybutylene-terephthalate, polypentylene-terephthalate, polyhexalene-terephthalate, polyheptadeneterephthalate, and polyoctalene-terephthalate.

13. 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 methyl cellulose, polyoxyethylene cetyl ether, polyoxyethylene lauryl ether, polyoxyethylene octyl ether, polyoxyethylene octyphenyl ether, polyoxyethylene oleyl ether, polyoxyethylene sorbitan monolaurate, polyoxyethylene stearyl ether, polyoxyethylene nonylphenyl ether, and dialkylphenoxy poly(ethyleneoxy)ethanol.

14. A process in accordance with claim 1 wherein the anionic surfactant is selected from the group consisting of sodium dodecyl sulfate, sodium dodecylbenzene sulfate, and sodium dodecylnaphthalene sulfate.

15. A process in accordance with claim 6 wherein the cationic surfactant is a quaternary ammonium salt.

16. A process in accordance with claim 1 wherein the pigment is carbon black, cyan, yellow, magenta, red, blue, green, brown, or mixtures thereof.

17. A process in accordance with claim 1 wherein the resin utilized in (ii) is from about 0.01 to 3 microns in volume average diameter, and the pigment particles are from about 0.01 to about 1 micron in average volume diameter.

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

20. A process in accordance with claim 1 wherein in (ii) the solids concentration is about 12 percent.

21. A process in accordance with claim 1 wherein the heating in (iii) is accomplished at a temperature of from about 53°

C. to about 64°

C.

19. A process for the preparation of toner compositions with controlled particle size comprising:

(i) preparing a pigment dispersion in water, which dispersion is comprised of a pigment and an ionic surfactant;

(ii) shearing the pigment dispersion with a latex blend comprised of resin particles of submicron size, a counterionic surfactant with a charge polarity of opposite sign to that of said ionic surfactant, and which blend contains a nonionic surfactant thereby causing a flocculation or heterocoagulation of the formed particles of pigment;

(iii) heating the formed particles of pigment of (ii) in a critical temperature region or above the glass transition temperature (Tg) of the resin particles thereby forming aggregated particles of resin and pigment;

(iv) heating the formed aggregated particles of (iii) about above the resin glass transition temperature (Tg) to provide a toner composition comprised of polymeric resin, and pigment; and

(v) optionally separating and drying the toner product.