Toner aggregation processes

• US 5,501,935 A
• Filed: 01/17/1995
• Issued: 03/26/1996
• Est. Priority Date: 01/17/1995
• Status: Expired due to Term

• Current Assignee: Xerox Corporation (Xerox Holdings Corp.)
• Original Assignee: Xerox Corporation (Xerox Holdings Corp.)
• Inventors: Gerroir, Paul J., Patel, Raj D., Kmiecik-Lawrynowicz, Grazyna E., Hopper, Michael A.
• Primary Examiner(s): MARTIN, ROLAND E
• Application Number:
  US08/373,806
• Time in Patent Office: 434 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
• CPC Class Codes: G03G 9/0819 characterised by the dimensions of the particles
• CPC Class Codes: G03G 9/08706 Polymers of alkenyl-aromatic compounds
• CPC Class Codes: G03G 9/08708 Copolymers of styrene
• CPC Class Codes: G03G 9/08711 with esters of acrylic or methacrylic acid
• CPC Class Codes: G03G 9/08728 Polymers of esters
• CPC Class Codes: G03G 9/09733 Organic compounds G03G9/08782 takes precedence
• CPC Class Codes: G03G 9/0975 anionic

Abstract

A process for the preparation of toner compositions consisting essentially of

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

(ii) shearing said pigment dispersion with a latex or emulsion blend comprised of resin, a counterionic surfactant with a charge polarity of opposite sign to that of said ionic surfactant, and a nonionic surfactant;

(iii) heating the above sheared blend below about the glass transition temperature (Tg) of the resin to form electrostatically bound toner size aggregates with a narrow particle size distribution;

(iv) subsequently adding further anionic or nonionic surfactant solution to minimize further growth in the coalescence (v); and

(v) heating said bound aggregates above about the Tg of the resin and wherein said heating is from a temperature of about 103° to about 120° C., and wherein said toner compositions are spherical in shape.

Claims

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

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

(ii) shearing said pigment dispersion with a latex or emulsion blend comprised of resin, a counterionic surfactant with a charge polarity of opposite sign to that of said ionic surfactant, and a nonionic surfactant;

(iii) heating the above sheared blend below about the glass transition temperature (Tg) of the resin to form electrostatically bound toner size aggregates with a narrow particle size distribution;

(iv) subsequently adding further anionic or nonionic surfactant solution to minimize further growth in the coalescence (v); and

(v) heating said bound aggregates above about the Tg of the resin and wherein said heating is from a temperature of about 103°

to about 120°

C., and wherein said toner compositions are spherical in shape.

2. A process in accordance with claim 1 wherein the temperature below the resin Tg of (iii) controls the size of the aggregated particles in the range of from about 2.5 to about 10 microns in average volume diameter.

3. A process in accordance with claim 1 wherein the size of said aggregates can be increased to from about 2.5 to about 10 microns by increasing the temperature of heating in (iii) to from about room temperature to about 50°

C.

4. A process in accordance with claim 1 wherein the particle size distribution of the aggregated particles is from about 1.16 to about 1.30.

5. A process in accordance with claim 1 wherein the toner average volume particle diameter is from about 3 to about 10 microns.

6. A process in accordance with claim 1 wherein temperature in (v) is in the range of 103°

to 119°

C. and heating is accomplished for a period of from about 15 minutes to about 45 minutes.

7. 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.

8. 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.

9. A process in accordance with claim 1 wherein said the heating temperature in (v) is in the range of 103°

to 119°

C.

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

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

13. A process in accordance with claim 1 wherein the shearing or homogenization (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.

14. 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 of from about 20°

C. to about 5°

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

15. 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-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(propyimethacrylate-isoprene), poly(butylmethacrylate-isoprene), poly(methylacrylate-isoprene), poly(ethylacrylate-isoprene), poly(propylacrylate-isoprene), and poly(butylacrylate-isoprene).

16. 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-butylmethacrylateacrylic acid), or poly(styrene-butylacrylate-acrylic acid), polyethyleneterephthalate, polypropylene-terephthalate, polybutylene-terephthalate, polypentylene-terephthalate, polyhexalene-terephthalate, polyheptadeneterephthalate, polystyrene-butadiene, and polyoctalene-terephthalate.

17. 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.

18. 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.

19. A process in accordance with claim 1 wherein the cationic surfactant is a quaternary ammonium salt.

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

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

and the pigment particles are from about 0.01 to about 3 microns in volume average diameter.

22. 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 from about 0.1 to about 5 weight percent of the toner components of resin, pigment and charge agent.

23. 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 of the obtained toner particles.

24. 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.

25. A process in accordance with claim 1 where subsequent to (iv) there is provided said a toner composition comprised of resin;

followed by optionally

(v) separating said toner particles from said water by filtration; and

(vi) drying said toner particles.

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

C. to about 25°

C. below the resin Tg.

27. A process in accordance with claim 1 wherein heating in (iii) is accomplished at a temperature of from about 29°

to about 59°

C.

28. A process in accordance with claim 1 wherein the resin Tg in (iii) is from about 50°

to about 80°

C.

29. A process in accordance with claim 1 wherein the resin Tg in (iii) is from about 52°

to about 65°

C.;

the resin Tg in (iv) is from about 52°

to about 650°

C.; and

the heating in (iii) is equal to or slightly above the resin Tg.

31. A process in accordance with claim 1 wherein the temperature (v) is 106°

C.

32. A process in accordance with claim 1 wherein the temperature (v) is 105°

C.

33. A process in accordance with claim 1 wherein the temperature (v) is 103°

C.

34. A process in accordance with claim 1 wherein the temperature (v) is 119°

C.

35. A process in accordance with claim 1 wherein the temperature (v) is 108°

C.

11. A process in accordance with claim I 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.

30. A process consisting essentially of

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

(ii) shearing said pigment dispersion with a latex or emulsion blend comprised of resin, a counterionic surfactant with a charge polarity of opposite sign to that of said ionic surfactant, and a nonionic surfactant;

(iii) heating the above-sheared blend below about the glass transition temperature (Tg) of the resin to form electrostatically bound toner size aggregates with a narrow particle size distribution;

(iv) subsequently adding further anionic or nonionic surfactant solution to minimize further growth of the electrostatically bound toner size aggregates in the coalescence (v); and

(v) heating said bound aggregates above about the Tg of the resin and wherein said heating is from a temperature of about 103°

to about 119°

C., and wherein subsequent to cooling there is provided a toner spherical in shape.