Toner aggregation processes

• US 5,405,728 A
• Filed: 06/25/1993
• Issued: 04/11/1995
• Est. Priority Date: 06/25/1993
• 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.
• Primary Examiner(s): GOODROW, JOHN L
• Application Number:
  US08/083,116
• Time in Patent Office: 655 Days
• Field of Search: 430/137, 430/109
• 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 containing a controlled solid contents of from about 50 weight percent to about 20 percent of polymer or resin, counterionic surfactant and nonionic surfactant in water, counterionic surfactant with a charge polarity of opposite sign to that of said ionic surfactant thereby causing a flocculation or heterocoagulation of the formed particles of pigment, resin and charge control agent to form a dispersion of solids of from about 30 weight percent to 2 percent comprised of resin, pigment and optionally charge control agent in the mixture of nonionic, anionic and cationic surfactants;

(iii) heating the above sheared blend at a temperature of from about 5° to about 25° C. about below the glass transition temperature (Tg) of the resin while continuously stirring to form toner sized aggregates with a narrow size dispersity; and

(iv) heating the electrostatically bound aggregated particles at a temperature of from about 5° to about 50° C. about above the (Tg) of the resin to provide a toner composition comprised of resin, pigment and optionally a charge control agent.

Claims

1. A process for the preparation of toner compositions comprising

(i) preparing a pigment dispersion in water, which dispersion is comprised of pigment, a counterionic surfactant with a charge polarity of opposite sign to the anionic surfactant of (ii) and optionally a charge control agent;

(ii) shearing the pigment dispersion with a latex comprised of resin, anionic surfactant, nonionic surfactant, and water; and

wherein the latex solids content, which solids are comprised of resin, is from about 50 weight percent to about 20 weight percent thereby causing a flocculation or heterocoagulation of the formed particles of pigment, resin and optional charge control agent;

diluting with water to form a dispersion of total solids of from about 30 weight percent to 1 weight percent, which total solids are comprised of resin, pigment and optional charge control agent contained in a mixture of said nonionic, anionic and cationic surfactants;

(iii) heating the above sheared blend at a temperature of from about 5°

to about 25°

C. below about the glass transition temperature (Tg) of the resin while continuously stirring to form toner sized electrostatically bound aggregates with a narrow size dispersity; and

(iv) heating the electrostatically bound aggregates at a temperature of from about 5°

to about 50°

C. above about the Tg of the resin to provide a toner composition comprised of 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 Tg in (iii) and (iv) from about 45°

to about 90°

C.

3. A process in accordance with claim 1 wherein the total solids content is from about 2 to about 10 weight percent.

4. A process in accordance with claim 1 wherein the concentration of resin in the latex is from about 60 percent to about 20 percent.

5. A process in accordance with claim 1 (ii) wherein the content of the resin solids after flocculation is controlled to from about 20 percent to about 5 percent by weight, and the particle size of the aggregate in (iii) is from about 1 micron to about 15 microns in average volume diameter.

6. A process in accordance with claim 1 wherein larger aggregated particles of from about 8 microns to about 20 microns are formed at lower total solids content of about 6 percent to about 20 percent in polymeric latex particles, pigment particles, and wherein smaller aggregated particles of from about 7 microns to about 2 microns are formed at a higher total solids content of about 7 percent to about 25 percent.

7. A process in accordance with claim 1 wherein the dispersion of (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. for a duration of from about 1 minute to about 120 minutes.

8. A process in accordance with claim 1 wherein the dispersion of (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.

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

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

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

C. to about 20°

C. below the Tg of the resin, which Tg is in the range of from about 48°

C. to about 72°

C., and which heating is accomplished for a duration of from about 0.5 hour to about 6 hours.

12. A process in accordance with claim 1 wherein the heating of the electrostatically 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 10°

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

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

13. 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(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-methyl 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).

14. 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-butylmethacrylate-acrylic acid), poly(styrene-butylacrylate-acrylic acid), polyethylene-terephthalate, polypropylene-terephthalate, polybutylene-terephthalate, polypentylene-terephthalate, polyhexalene-terephthalate, polyheptadene-terephthalate, poly(styrene-butadiene), and polyoctalene-terephthalate.

15. 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 octylphenyl ether, polyoxyethylene oleyl ether, polyoxyethylene sorbitan monolaurate, polyoxyethylene stearyl ether, polyoxyethylene nonylphenyl ether, and dialkylphenoxy poly(ethyleneoxy)ethanol.

16. 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, and the cationic surfactant is a quaternary ammonium salt.

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

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

19. A process in accordance with claim 1 wherein the toner obtained is from about 2 to about 15 microns in average volume diameter, and the geometric size distribution is from about 1.15 to about 1.30.

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

21. 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 of resin and pigment;

the anionic surfactant concentration is about 0.1 to about 5 weight percent of the toner components of resin and pigment; and

the counterionic surfactant concentration is about 0.1 to about 5 weight percent of the toner of resin and pigment.

22. A process in accordance with claim 1 wherein there is added to the surface of the isolated toner particles 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.

23. 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.

24. A process in accordance with claim 1 wherein the toner particles isolated are from about 3 to about 15 microns in volume average diameter, and the geometric size distribution is from about 1.15 to about 1.25.

25. A process for the preparation of toner with controlled particle size comprising

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

(ii) shearing the pigment dispersion with a latex, which latex contains a resin content of from about 50 percent by weight to about 20 percent by weight, thereby causing a flocculation or heterocoagulation of the formed particles of pigment and resin;

diluting with water to form a uniform dispersion of total solids from about 30 percent by weight to about 2 percent by weight;

(iii) heating the above sheared blend at a temperature of from about 5°

C. to about 25°

C. about below the glass transition temperature (Tg) of the resin while continuously stirring to form toner sized electrostatically bound aggregates with a narrow size dispersity;

(iv) heating the electrostatically bound aggregates at a temperature of from about 5°

C. to about 50°

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

optionally

(v) separating said toner particles from the water; and

(vi) drying said toner particles;

wherein said latex comprises resin, anionic surfactant, nonionic surfactant and water, and said total solids components are comprised of resin and pigment.

26. A process in accordance with claim 25 wherein the (iii) and (iv) resin glass transition temperature (Tg) is from about 50°

C. to about 80°

C.

27. A process in accordance with claim 25 wherein the resin glass transition temperature (Tg) is from about 45°

C. to about 90°

C.

28. A process in accordance with claim 25 wherein the resin glass transition temperature (Tg) is from about 50°

C. to about 80°

C.

29. A process in accordance with claim 25 wherein heating in (iii) or (iv) is accomplished at the glass transition temperature.

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

(i) preparing a pigment dispersion in water, which dispersion is comprised of pigment, a counterionic surfactant with a charge polarity of opposite sign to the anionic surfactant of (ii) and optionally a charge control agent;

(ii) shearing the pigment dispersion with a latex comprised of resin, anionic surfactant, nonionic surfactant, and water; and

wherein the latex solids content, which solids are comprised of resin, is from about 50 weight percent to about 20 weight percent thereby causing a flocculation or heterocoagulation of the formed particles of pigment, resin and optional charge control agent;

diluting with water to form a dispersion of total solids of from about 30 weight percent to 1 weight percent, which total solids are comprised of resin, pigment and optional charge control agent contained in a mixture of said nonionic, anionic and cationic surfactants;

(iii) heating the above sheared blend at a temperature of from about 5°

to about 25°

C. below about the glass transition temperature (Tg) of the resin while continuously stirring to form toner sized electrostatically bound aggregates with a narrow size dispersity; and

(iv) heating the electrostatically bound aggregates at a temperature of from about 5°

to about 50°

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