Toner aggregation processes

• US 5,496,676 A
• Filed: 03/27/1995
• Issued: 03/05/1996
• Est. Priority Date: 03/27/1995
• 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., Grushkin, Bernard
• Primary Examiner(s): MARTIN, ROLAND E
• Application Number:
  US08/411,196
• Time in Patent Office: 344 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 9/0815 Post-treatment

Abstract

A process comprising:

(i) preparing a pigment dispersion comprised of pigment, ionic surfactant, and optional charge control agent;

(ii) mixing at least two resins in the form of latexes, each latex comprising a resin, ionic and nonionic surfactants and optionally a charge control agent, and wherein the ionic surfactant has a countercharge to the ionic surfactant of (i) to obtain a latex blend;

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

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

(v) subsequently adding further anionic surfactant solution to minimize further growth of the bound aggregates (vi);

(vi) heating said bound aggregates above about the glass transition temperature Tg of the resin to form stable toner particles; and optionally

(vii) separating and drying the toner.

Claims

1. A process comprising:

(i) preparing a pigment dispersion comprised of pigment, ionic surfactant, and optional charge control agent;

(ii) mixing at least two resins of different molecular composition, molecular weight or Tg in the form of latexes, each latex comprising a resin, ionic and nonionic surfactants and optionally a charge control agent, and wherein the ionic surfactant has a countercharge to the ionic surfactant of (i) to obtain a latex blend;

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

(iv) heating the above sheared blends of (iii) below about the glass transition temperature (Tg) of the resins, to form electrostatically bound toner size aggregates with a narrow particle size distribution; and

(v) subsequently adding further anionic surfactant solution to minimize further growth of the bound aggregates (vi);

(vi) heating said bound aggregates above about the glass transition temperature Tg of the resins to form stable toner particles; and

optionally

(vii) separating and drying the toner.

2. A process in accordance with claim 1 wherein one of said latexes employed in (ii) is comprised of styrene/butylacrylate/acrylic acid, styrene butadiene/acrylic acid, or styrene/isoprene/acrylic acid.

3. A process in accordance with claim 1 wherein a first and second latex are selected, and wherein the first latex is comprised of styrene/butylacrylate/acrylic acid, styrene/butadiene/acrylic acid, or styrene/isoprene/acrylic acid resin, which resin possesses a dissimilar molecular weight and/or a dissimilar glass transition temperature Tg than that of the second resin latex.

4. A process in accordance with claim 1 wherein the latexes selected are comprised of resins that are compatible evidencing substantially no phase separation, thus enabling a toner with high, of from about 40 to about 80 gloss, and excellent fixing characteristics.

5. A process in accordance with claim 1 wherein the latexes employed are comprised of resins that are incompatible resulting in a toner with low gloss, excellent fix, and wherein the toner formed enables images with a matte finish.

6. A process in accordance with claim 1 wherein one latex is comprised of styrene/butylacrylate acrylic acid, 82:

18;

2 parts per hundred, and a second latex is comprised of styrene/butylacrylate acrylic acid, 88;

12;

2 parts per hundred.

7. A process in accordance with claim 1 wherein one latex is present in an amount of from about 5 to about 95 weight percent and the second or latex is present in an amount of from about 95 to about 5 weight percent.

8. A process in accordance with claim 1 wherein one latex is present in an amount of from about 40 to about 60 weight percent and the second latex comprising the blend is present in an amount of from about 60 to about 40 weight percent.

9. A process in accordance with claim 1 wherein the toner that results has a narrow geometric size distribution of from about 1.18 to about 1.27, and the average volume particle diameter of the toner is from about 4 to about 7 microns.

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

11. A process in accordance with claim 1 wherein the ionic surfactant utilized in preparing the pigment dispersion is a cationic surfactant, and the counterionic surfactants present in the latex mixtures are comprised of anionic surfactants.

12. A process in accordance with claim 1 wherein the ionic surfactant utilized in preparing the pigment dispersion is an anionic surfactant, and the counterionic surfactants present in the latex mixture are comprised of cationic surfactants.

13. A process in accordance with claim 1 wherein there are selected at least two latexes that are compatible.

14. A process in accordance with claim 1 wherein there are selected from 2 to about 10 latexes.

15. A process in accordance with claim 1 wherein the shearing or homogenization in (iii) 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.

16. A process in accordance with claim 1 wherein the heating of the blends of 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.

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, 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.

18. A process in accordance with claim 1 wherein the resin for one of the latexes 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), poly(butylacrylate-isoprene), poly(styrene-butadiene-acrylic acid), poly(styrene-butadiene-methacrylic acid), poly(styrene-butylmethacrylate-acrylic acid), and poly(styrene-butylacrylate-acrylic acid).

19. A process in accordance with claim 1 wherein the resin selected for a second latex 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), poly(butylacrylate-isoprene), poly(styrene-butadiene-acrylic acid), poly(styrene-butadiene-methacrylic acid), poly(styrene-butylmethacrylate-acrylic acid), and poly(styrene-butylacrylate-acrylic acid).

20. 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 for both latexes.

21. 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.

22. A process in accordance with claim 2 wherein the ionic surfactant is a cationic surfactant of a quaternary ammonium salt.

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

24. A process in accordance with claim 1 wherein the resin utilized in a first latex and a second latex (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.

25. A process in accordance with claim 1 wherein the toner particles isolated are from about 2 to about 15 microns in average volume diameter, and the geometric size distribution thereof is from about 1.10 to about 1.30.

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

27. A process in accordance with claim 1 wherein the nonionic surfactant concentration selected is an amount of 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.

28. A process in accordance with claim 1 wherein there is added to the surface of the toner obtained 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.

29. 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.

30. A process in accordance with claim 1 wherein the toner particles isolated are from about 3 to about 15 microns in average volume diameter, and the geometric size distribution thereof is from about 1.15 to about 1.27.

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

32. A process in accordance with claim 2 wherein the nonionic surfactant concentration is about 0.1 to about 5 weight percent of the toner components;

and wherein the anionic surfactant concentration is about 0.1 to about 5 weight percent of the toner components.

33. A process in accordance with claim 2 wherein the toner is washed with warm water, and the surfactants are removed from the toner surface, followed by drying.

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

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

C. to about 25°

C. below the Tg.

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

to about 59°

C.

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

to about 80°

C.

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

to about 50°

C. above the Tg.

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

to about 80°

C.

41. A process in accordance with claim 1 wherein the resin Tg is 54°

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

to about 104°

C.

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

to about 65°

C.; and

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

to about 65°

C.

45. A process in accordance with claim 1 wherein the toner resulting has a gloss of from about 40 to about 80 gloss units at temperatures below the minimum fixing temperature of the toner, and fixing characteristics in the range of from about 1.6 to about 2.0 units.

46. A process in accordance with claim 1 wherein the toner resulting has excellent fixing characteristics in the range of 1.6 to 2.0 units.

35. A process for the preparation of toner particles with a particle size of from about 1 to about 25 microns in average volume diameter comprising:

(i) preparing a pigment dispersion in water, which dispersion is comprised of a pigment with a diameter of from about 0.01 to about 1 micron, and an ionic surfactant;

(ii) mixing at least two latexes comprised of resins of different molecular composition, molecular weight or Tg, ionic and nonionic surfactants and optionally a charge control agent, and wherein the ionic surfactant employed has countercharging characteristics with reference to the ionic surfactant of (i);

(iii) shearing the pigment dispersion with a mixture of the latex blend (ii) comprised of resins, a counterionic surfactant with a charge polarity of opposite sign to that of said ionic surfactant and a nonionic surfactant, and wherein said blend is submicron in size of from about 0.01 to about 1 micron, thereby which shearing enables a flocculation or heterocoagulation of the formed particles of pigment, and resin to form a uniform dispersion of solids in the water and surfactant;

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

to about 20°

C. below the Tg of the resins to form electrostatically bound toner size aggregates with a narrow particle size distribution;

followed by the addition of further anionic surfactant;

(v) heating the electrostatically bound toner size aggregate particles at a temperature of from about 5°

to about 50°

C. above the Tg of the resins to provide a mechanically stable toner composition comprised of polymeric resin and pigment; and

optionally

(vi) separating said toner particles; and

(vii) drying said toner particles.

43. A process in accordance with claim 35 wherein the heating in (v) is equal to or slightly below the resin Tg.

44. A process in accordance with claim 35 wherein the heating in (iv) is equal to or slightly above the resin Tg.

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

(i) preparing a pigment dispersion comprised of pigment, ionic surfactant, and optional charge control agent;

(ii) preparing a latex blend of two or more latexes containing resins of different molecular composition, molecular weight or Tg with a polytron or a mixer operating for a period of from about 0.5 to 2 minutes to obtain a latex blend;

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

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

(v) subsequently adding further anionic surfactant solution to minimize further growth of the aggregates in the coalescence step (vi); and

(vi) heating said bound aggregates above about the Tg of the resins.

48. A process for the preparation of toner comprising:

(i) preparing a pigment dispersion comprised of pigment, ionic surfactant, and optional charge control agent;

(ii) mixing a first and a second latex, each latex comprising a resin of different molecular composition, molecular weight or Tg from the resin of the other latex, ionic and nonionic surfactants and optionally a charge control agent, and wherein the ionic surfactant possesses a countercharge opposite to that of said ionic surfactant used in (i) and wherein a latex blend results;

(iii) shearing said pigment dispersion with the latex blend of (ii) comprised of resins, a counterionic surfactants with a charge polarity of opposite sign to that of said ionic surfactant and a nonionic surfactant;

(iv) heating the above sheared blends below about the glass transition temperature (Tg) of the latex resins to form electrostatically bound toner size aggregates with a narrow particle size distribution;

(v) subsequently adding further an ionic surfactant solution to minimize further growth of the aggregates in the coalescence step (vi);

(vi) heating said bound aggregates above about the Tg of the latex resins to form stable toner particles; and

optionally

(vii) separating the toner particles from the aqueous medium by filtration, washing the toner to remove traces of surfactant, and drying to produce an electrophotographic toner.