Toner processes

• US 5,650,256 A
• Filed: 10/02/1996
• Issued: 07/22/1997
• Est. Priority Date: 10/02/1996
• Status: Expired due to Term

• Current Assignee: Xerox Corporation (Xerox Holdings Corp.)
• Original Assignee: Xerox Corporation (Xerox Holdings Corp.)
• Inventors: Veregin, Richard P. N., Torres, Francisco E., Patel, Raj D., McDougall, Maria N. V., Kmiecik-Lawrynowicz, Grazyna E., Ng, T. Hwee, Helbrecht, Arthur
• Primary Examiner(s): GOODROW, JOHN L
• Application Number:
  US08/720,646
• Time in Patent Office: 293 Days
• Field of Search: 430/137, 430/106, 430/110, 430/111, 523/335
• 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 9/0815 Post-treatment

Abstract

A process for the preparation of toner comprising:

(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, and wherein said resin contains an acid functionality;

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

(iv) adding anionic surfactant to stabilize the aggregates obtained in (iii);

(v) coalescing said aggregates by heating said bound aggregates above about the Tg of the resin;

(vi) reacting said resin of (v) with acid functionality with a base to form an acrylic acid salt, and which salt is ion exchanged in water with a base or a salt, optionally in the presence of metal oxide particles, to control the toner triboelectrical charge, which toner is comprised of resin and pigment; and

(vii) optionally drying the toner obtained.

Claims

1. A process for the preparation of toner comprising:

(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, and wherein said resin contains an acid functionality;

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

(iv) adding anionic surfactant to stabilize the aggregates obtained in (iii);

(v) coalescing said aggregates by heating said bound aggregates above about the Tg of the resin;

(vi) reacting said resin of (v) with acid functionality with a base to form an acrylic acid salt, and which salt is ion exchanged in water with a base or a salt, optionally in the presence of metal oxide particles, to control the toner triboelectrical charge, which toner is comprised of resin and pigment; and

(vii) optionally drying the toner obtained.

2. A process in accordance with claim 1 wherein the acid functionality is acrylic acid.

3. A process in accordance with claim 1 wherein the resin is a styrene acrylate, and the base is an alkali metal hydroxide.

4. A process in accordance with claim 1 wherein a base of an alkali metal hydroxide is selected.

5. A process in accordance with claim 1 wherein the salt used in the ion exchange is a metal halide.

6. A process in accordance with claim 1 wherein the reaction between the toner resin of (vi) and the base is accomplished at a temperature of from about 0°

C. to about 5 to 10 degrees below the glass transition temperature of the resin, over a period of about 10 minutes to about 6 hours, and where the pH of the water is between about 7 and about 13.

7. A process in accordance with claim 1 wherein the base treated toner is ion exchanged in water, at a temperature of from about 0°

C. to about 5 to 10 degrees below the glass transition temperature of the resin, over a period of time of from about 15 minutes to about 6 hours.

8. A process in accordance with claim 1 wherein the base is sodium hydroxide, and the resin is a styrene acrylate acrylic acid.

9. A process in accordance with claim 1 wherein the base is potassium hydroxide, and the resin is a styrene acrylate acrylic acid.

10. A process in accordance with claim 1 wherein the ion exchange salt is a metal halide, and the resin is a styrene acrylate acrylic acid.

11. A process in accordance with claim 1 wherein the ion exchange salt is ZnCl₂ and the resin is a styrene acrylate acrylic acid, or wherein the ion exchange salt is CaCl₂, and the resin is a styrene acrylate acrylic acid.

12. A process in accordance with claim 1 wherein there are utilized metal oxide particles selected from a group consisting of silicon dioxide, titanium dioxide, tin oxide, aluminum oxide, and zirconium oxide, and the resin is a styrene acrylate acrylic acid.

13. A process in accordance with claim 1 wherein there are utilized metal oxide particles of hydrophobically modified silicon dioxide, and the resin is a styrene acrylate acrylic acid.

14. 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.

15. 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.

16. A process in accordance with claim 1 wherein said toner triboelectric charge is from about 5 to about 50 microcoulombs per gram.

17. 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, and reacted resin product 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.

18. A process in accordance with claim 1 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-methylstyrene-isoprene), poly(meta-methylstyrene-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), all containing optionally acrylic acid.

19. 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;

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.

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 volume average diameter, and the pigment is from about 0.01 to about 3 microns in volume average diameter.

22. A process in accordance with claim 1 wherein the toner isolated is from about 2 to about 15 microns in average volume diameter, and the geometric size distribution thereof is from about 1.15 to about 1.35.

23. A process in accordance with claim 1 wherein the aggregates formed in (v) are about 1 to about 10 microns in volume average diameter.

24. 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 agent.

25. A process in accordance with claim 1 wherein there is added to the surface of the formed dried toner 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 obtained toner of resin and pigment.

26. A process in accordance with claim 1 wherein said resin of (ii) is submicron in volume average diameter, the sheared blend of (iii) is continuously stirred, and subsequent to (v) said toner is separated by filtration and subjected to drying.

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

C. to about 25°

C. below the Tg, heating in (iii) is accomplished at a temperature of from about 29°

to about 59°

C., or the resin Tg in (iii) is from about 50°

to about 80°

C., heating in (iv) is from about 5°

to about 50°

C. above the Tg, or the resin Tg is 54°

C. and heating in (iv) is from about 59°

to about 104°

C.

28. A process in accordance with claim 27 wherein the heating in (iii) is equal to or slightly above the resin Tg.

29. A process for the preparation of toner comprising:

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

(ii) shearing said pigment dispersion with a latex blend comprised of resin, a counterionic surfactant with a charge polarity of opposite sign to that of said ionic surfactant and a nonionic surfactant, and wherein said resin contains an acid functionality;

(iii) heating the above sheared blend below about the glass transition temperature (Tg) of the resin to form aggregates;

(iv) adding anionic surfactant;

(v) heating said aggregates above about the Tg of the resin;

(vi) reacting in the presence of a metal oxide said resin with acid functionality with a base to form an acrylic acid salt; and

optionally

(vii) isolating and drying the toner.

30. A process in accordance with claim 29 wherein in (vi) said acrylic acid salt is ion exchanged in water with a base or a salt, in the presence of the metal oxide.

31. A process for the preparation of toner comprising shearing a pigment dispersion with a latex blend, and wherein the pigment dispersion is comprised of a pigment and an ionic surfactant, and wherein the latex blend is comprised of resin, a counterionic surfactant with a charge polarity of opposite sign to that of said ionic surfactant and a nonionic surfactant, and wherein said resin contains an acid functionality;

heating the above sheared blend below about the glass transition temperature (Tg) of the resin to form aggregates;

adding anionic surfactant to stabilize the formed aggregates;

heating said aggregates above about the Tg of the resin to effect coalescence thereof;

reacting said resin with acid functionality with a base to form an acrylic acid salt; and

optionally isolating and drying the toner.

32. A process in accordance with claim 31 wherein the toner is isolated and dried, and the salt ion exchange is accomplished in the presence of metal oxides, or a metal oxide.

33. The toner obtained by the process of claim 31.

34. A process in accordance with claim 31 wherein heating in (iii) and (v) is about at the resin Tg.