Ink toner particles with controlled surface morphology

• US 8,652,745 B2
• Filed: 07/20/2012
• Issued: 02/18/2014
• Est. Priority Date: 01/16/2008
• Status: Expired due to Fees

• Current Assignee: Penn Color, Inc.
• Original Assignee: Penn Color, Inc.
• Inventors: Schuck, Ronald W., Rybny, Charles B., Lai, Choung
• Primary Examiner(s): FRASER, STEWART A
• Application Number:
  US13/554,437
• Publication Number:
  US 20130045441A1
• Time in Patent Office: 578 Days
• Field of Search: 430/137.1, 430/137.14, 430/137.17
• US Class Current: 430/137.1
• 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 9/0821 characterised by physical parameters magnetic parameters G03G9/083
• CPC Class Codes: G03G 9/08711 with esters of acrylic or methacrylic acid
• CPC Class Codes: G03G 9/08753 Epoxyresins
• CPC Class Codes: G03G 9/08755 Polyesters
• CPC Class Codes: G03G 9/08764 Polyureas; Polyurethanes
• CPC Class Codes: G03G 9/08795 characterised by their chemical properties, e.g. acidity, molecular weight, sensitivity to reactants
• CPC Class Codes: G03G 9/08797 characterised by their physical properties, e.g. viscosity, solubility, melting temperature, softening temperature, glass transition temperature
• CPC Class Codes: G03G 9/09708 Inorganic compounds
• CPC Class Codes: G03G 9/09725 Silicon-oxides; Silicates

Abstract

The present invention provides a process for producing a colored toner having a textured surface, the process includes forming a polymer composition of at least one polymer and a colorant, where the at least one polymer has a softening temperature from about 60° C. to about 160° C.; forming an aqueous mineral suspension of at least one multivalent metal phosphate; forming a dispersion by combining the polymer composition and the aqueous mineral suspension under agitation to form a solid portion comprising dispersed particles of the polymer composition; heating the dispersion to a temperature above a glass transition temperature (Tg) of the polymer composition and increasing the pH to above 7.0; cooling the dispersion including the dispersed particles of the polymer composition to a temperature of from about 1° C. to about 89° C.; and recovering the particles.

Claims

1. A process for producing a colored toner comprising:

forming a polymer composition comprising at least one polymer and a colorant, wherein the at least one polymer has a softening temperature from about 60°

C. to about 160°

C.;

forming an aqueous mineral suspension of at least one multivalent metal phosphate;

forming a dispersion by combining the polymer composition and the aqueous mineral suspension under agitation to form a solid portion comprising dispersed particles of the polymer composition, wherein the temperature of the aqueous mineral suspension during the dispersion is at least about 70°

C.;

heating the dispersion to a temperature above a glass transition temperature (Tg) of the polymer composition and increasing the pH to above 7.0;

cooling the dispersion comprising the dispersed particles of the polymer composition; and

recovering the particles.

2. A process according to claim 1, wherein the pH is increased to 9.0 or above.

3. A process according to claim 1, wherein the particles comprise a textured surface.

4. A process according to claim 1, wherein the particles comprise an average surface roughness, Ra, of about 15 to about 55 nm.

5. A process according to claim 1, wherein the particles comprise a substantially spherical shape where a ratio of a shortest radius of the particles to a longest radius of the particles ranges from about 1:

1 to 1;

3.

6. A process according to claim 1, wherein the recovered particles are combined with a powder selected from the group consisting of colloidal silica, titanium oxide, calcium phosphate, barium carbonate, calcium carbonate, aluminum oxide, and mixtures thereof.

7. A process according to claim 6, wherein the recovered particles are combined with a surface active agent selected from the group consisting of polyvinyl pyrrolidone, polyvinyl alcohol, polyacrylic acid polymer, copolymers and combinations thereof.

8. The process of claim 1, wherein the volume average particle size of the recovered particles is less than 12 μ

m, and particle size distribution is less than 1.4.

9. The process of claim 1 wherein the volume average particle size is between about 4.0 μ

m and about 9.0 μ

m.

10. A process according to claim 1, wherein forming the aqueous mineral suspension of at least one multivalent metal phosphate occurs by contacting a water-soluble salt of the multivalent metal with an aqueous solution comprising:

a water-soluble phosphate salt; and

at least one crystal growth inhibitor selected from the group consisting of;

an organic polycarboxylic acid or a salt thereof, a pyrophosphate salt, phosphonic acid or a salt thereof, citric acid, L-Serine, 1,2-dihydroxy-1,2-bis(dihydroxyphosphonyl)ethane, and a Zn2+ salt, to precipitate the at least one multivalent metal phosphate, wherein the pH of the aqueous mineral suspension is from 5.5 to 14.

11. The process of claim 10, wherein the crystal growth inhibitor includes at least the organic polycarboxylic acid and the organic polycarboxylic acid is selected from the group consisting of:

phthalic acid, isophthalic acid, terephthalic acid, trimelitic acid, citric acid, anhydrides, polyacrylic acid and salts thereof.

12. The process of claim 10, wherein the aqueous solution during the step of forming an aqueous mineral suspension is at a temperature of from about 30°

C. to about 60°

C.

13. The process of claim 1, wherein the metal of the at least one multivalent metal phosphate is at least one of calcium and magnesium.

14. The process of claim 1, wherein the at least one polymer includes one or more polymers comprising polyesters, polyurethanes, styrene-acrylic copolymers, epoxy-containing polymers, polystyrene-acrylate polymers, and combinations thereof.

15. The process of claim 1, wherein the polymer composition further comprises at least one of a wax and a charge control agent.

16. The process of claim 1 further comprising a washing step prior to recovering the particles, the washing step comprising adding an acid to the aqueous mineral suspension comprising the dispersed particles to bring the pH of the aqueous mineral suspension to less than about 2.

17. A method of producing a colored toner with a given surface morphology comprising:

forming a polymer composition comprising at least one polymer and a colorant, wherein the at least one polymer has a softening temperature from about 60°

C. to about 160°

C.;

forming an aqueous mineral suspension of at least one multivalent metal phosphate;

forming a dispersion by combining the polymer composition and the aqueous mineral suspension under agitation to form a solid portion comprising dispersed particles of the polymer composition, wherein the temperature of the aqueous mineral suspension during the dispersion is at least about 70°

C.; and

either

(i) heating the dispersion to a temperature above a glass transition temperature (Tg) of the polymer composition and adjusting the pH of the dispersion to be basic;

cooling the dispersion comprising the dispersed particles of the polymer composition; and

recovering particles comprising a textured surface;

or

(ii) heating the dispersion to a temperature above a glass transition temperature (Tg) of the polymer composition and adjusting the pH of the dispersion to be acidic;

cooling the dispersion comprising the dispersed particles of the polymer composition; and

recovering particles comprising a smooth surface.

18. The process of claim 17, wherein particles comprising a smooth surface are formed by adjusting the pH using an acid selected from the group consisting of hydrochloric acid, nitric acid, phosphoric acid, acetic acid, propionic acid, butyric acid, phthalic acid, sulfuric acid, and mixtures thereof.

19. The process of claim 17, wherein particles comprising a textured surface are formed by adjusting the pH using a base selected from the group consisting of potassium hydroxide, ammonium hydroxide, ethyl amine, triethyl amine, sodium hydroxide, and mixtures thereof.