US5370964A
Expired / Lapsed
US
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Toner aggregation process
Assignee: Xerox Corp
•
Filing: 1993-11-29
•
Granted: 1994-12-06
•
Expires: 2013-11-29
Abstract
Abstract A process for the preparation of toner comprising: (i) preparing a pigment dispersion in water, which dispersion is comprised of pigment, an ionic surfactant, and an optional charge control agent; (ii) shearing the pigment dispersion with a polymeric latex comprised of resin, a counterionic surfactant with a charge polarity of opposite sign to that of said ionic surfactant, and which latex contains a nonionic surfactant thereby forming a homogeneous or a uniform blend; (iii) heating the above sheared homogeneous blend below about the glass transition temperature (Tg) of the resin to form electrostatically bound toner size aggregates; (iv) reshearing the above electrostatically bound toner aggregates (iii) to fragment or break down said toner aggregates of (iii) into smaller average diameter particle size; (v) heating the resulting formed sheared homogeneous blend (iv) comprised of resin, pigment particles, and the ionic, counterionic and nonionic surfactants in water below about the glass transition temperature (Tg) of the resin while continuously stirring at about 450 to about 800 revolutions per minute to form electrostatically bound toner size aggregates with a narrow particle size distribution; (vi) adding further ionic or nonionic surfactant in an amount of from about 0.1 to about 10 percent by weight of water to minimize further growth or enlargement of the particles in the coalescence step (vii); and (vii) heating the formed statically bound aggregated particles of (vi) about above the Tg of the resin to provide coalesced particles of toner (viii) separating said toner; and (ix) drying said toner.
Inventors
- 👤 Raj D. Patel
- 👤 Grazyna E. Kmiecik-Lawrynowicz
- 👤 Michael A. Hopper
- 👤 Melvin D. Croucher
- 👤 T. Hwee Ng
- 👤 William J. Dale
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-25 13:41
CPC Classifications
G; G03; G03G; G03G9/00; G03G9/08; G03G9/0802; G03G9/0815; G03G9/0804
Claims Analysis
Total Claims: 45
Claim 1
Independent Claim
334 words
A process for the preparation of toner comprising: (i) preparing a pigment dispersion in water, which dispersion is comprised of pigment, an ionic surfactant, and an optional charge control agent; (ii) shearing the pigment dispersion with a polymeric latex comprised of resin, a counterionic surfactant with a charge polarity of opposite sign to that of said ionic surfactant, and which latex contains a nonionic surfactant thereby forming a homogeneous or a uniform blend dispersion of flocs comprised of resin, pigment, and optional charge additive; (iii) heating the above sheared homogeneous blend below about the glass transition temperature (Tg) of the resin to form electrostatically bound toner size aggregates with an average volume diameter of from about 3 to about 10 microns and a particle size distribution (GSD) of between about 1.10 and about 1.30; (iv) reshearing the above electrostatically bound toner aggregates (iii) to fragment or break down said toner aggregates of (iii) into smaller average diameter particle size in the range of from about 0.5 to about 2 microns to allow reaggregation (step v) of said fragment particles; (v) heating the resulting formed sheared homogeneous blend (iv) comprised of resin, pigment particles, and the ionic, counterionic and nonionic surfactants in water below about the glass transition temperature (Tg) of the resin while continuously stirring at about 450 to about 800 revolutions per minute corresponding to an agitator tip speed of between 240 and 440 centimeters per second to form electrostatically bound toner size aggregates with a narrow particle size distribution; (vi) adding further ionic or nonionic surfactant in an amount of from about 0.1 to about 10 percent by weight of water to control, prevent, or minimize further growth or enlargement of the particles in the coalescence step (vii); and (vii) heating the formed statically bound aggregated particles of (vi) about above the Tg of the resin to provide coalesced particles of toner comprised of resin, pigment and optional charge control agent; and optionally (viii) separating said toner; and (ix) drying said toner.
Claim 2
Dependent Claim
334 words
A process for the preparation of toner comprising: (i) preparing a pigment dispersion in water, which dispersion is comprised of pigment, an ionic surfactant, and an optional charge control agent; (ii) shearing the pigment dispersion with a polymeric latex comprised of resin, a counterionic surfactant with a charge polarity of opposite sign to that of said ionic surfactant, and which latex contains a nonionic surfactant thereby forming a homogeneous or a uniform blend dispersion of flocs comprised of resin, pigment, and optional charge additive; (iii) heating the above sheared homogeneous blend below about the glass transition temperature (Tg) of the resin to form electrostatically bound toner size aggregates with an average volume diameter of from about 3 to about 10 microns and a particle size distribution (GSD) of between about 1.10 and about 1.30; (iv) reshearing the above electrostatically bound toner aggregates (iii) to fragment or break down said toner aggregates of (iii) into smaller average diameter particle size in the range of from about 0.5 to about 2 microns to allow reaggregation (step v) of said fragment particles; (v) heating the resulting formed sheared homogeneous blend (iv) comprised of resin, pigment particles, and the ionic, counterionic and nonionic surfactants in water below about the glass transition temperature (Tg) of the resin while continuously stirring at about 450 to about 800 revolutions per minute corresponding to an agitator tip speed of between 240 and 440 centimeters per second to form electrostatically bound toner size aggregates with a narrow particle size distribution; (vi) adding further ionic or nonionic surfactant in an amount of from about 0.1 to about 10 percent by weight of water to control, prevent, or minimize further growth or enlargement of the particles in the coalescence step (vii); and (vii) heating the formed statically bound aggregated particles of (vi) about above the Tg of the resin to provide coalesced particles of toner comprised of resin, pigment and optional charge control agent; and optionally (viii) separating said toner; and (ix) drying said toner.
Claim 3
Dependent Claim
58 words
A process in accordance with claim 1 wherein said resin Tg of (iii) is in the range of from about 40° C. to about 85° C. and preferably in the range of from about 50° C. to about 75° C.; and said reshearing is accomplished at a speed of from about 3,000 to about 15,000 revolutions per minute.
Claim 4
Dependent Claim
47 words
A process in accordance with claim 2 wherein (iv) and (v) are repeated about five times, and until the aggregated particles have a particle size in the range of from about 3 to about 10 microns and a GSD of from between about 1.10 and about 1.27.
Claim 5
Dependent Claim
53 words
A process in accordance with claim 1 wherein in (iv) the resheated aggregates are stirred at speeds of from about 450 to about 800 revolutions per minute, or tip speeds of from about 240 to about 440 centimeters/second to enable a narrow toner particle size distribution of from about 1.18 to about 1.28.
Claim 6
Dependent Claim
37 words
A process in accordance with claim 1 wherein in (iv) the sheared aggregates are stirred at speeds of from about 450 to about 800 revolutions per minute, or tip speeds of about 240 to about 440 centimeters/second.
Claim 7
Dependent Claim
51 words
A process in accordance with claim 5 wherein the reshearing is accomplished at temperatures in the range of from about 10° C. to about 25° C. below the glass transition temperature (Tg) of the resin, which resin Tg is in the range of from about 40° C. to about 85° C.
Claim 8
Dependent Claim
52 words
A process in accordance with claim 2 wherein the reshearing of the electrostatically bound aggregates results in the generation of fine toner particles with an average volume diameter of from about 0.4 to about 1.5 microns as measured on the Coulter Counter and which particles are comprised of resin and pigment particles.
Claim 9
Dependent Claim
36 words
A process in accordance with claim 1 wherein a particle size distribution of from between about 1.31 and about 1,000 obtained in (iii) results from low stirring speeds of from about 150 to about 450 rpm.
Claim 10
Dependent Claim
43 words
A process in accordance with claim 1 wherein the homogeneous blend (ii) is achieved by shearing the dispersion of the latex, the pigment and oppositely charged surfactants in water at a high speed of from about 5,000 to about 15,000 revolutions per minute.
Claim 11
Dependent Claim
29 words
A process in accordance with claim 1 wherein the shearing (ii) of the latex particles, pigment particles and oppositely charged surfactants is achieved with a polytron or a homogenizer.
Claim 12
Dependent Claim
41 words
A process in accordance with claim 1 wherein the shearing (ii) of the latex particles, pigment and oppositely charged surfactants is achieved by a continuous shearing device comprising an indefinitely variable gap adjustment of from about 0.1 to about 3 millimeters.
Claim 13
Dependent Claim
35 words
A process in accordance with claim 1 wherein the shearing of the latex particles, pigment particles and oppositely charged surfactants of (ii) is achieved with a continuous online homogenizer comprising a 3 stage rotator stator.
Claim 14
Dependent Claim
42 words
A process in accordance with claim 1 wherein the shearing (ii) of the latex comprised of resin particles stabilized by ionic surfactant particles, pigment, and oppositely charged surfactants is achieved at a temperature of from about 0° C. to about 35° C.
Claim 15
Dependent Claim
43 words
A process in accordance with claim 1 wherein the homogeneous blend of the latex particles, pigment particles and oppositely charged surfactants to obtain narrow particle size distribution of aggregated particles is achieved by shearing at from about 2 minutes to about 120 minutes.
Claim 16
Dependent Claim
30 words
A process in accordance with claim 1 wherein the time of shearing (ii) controls the homogeneity of the blend of the latex particles, pigment and ionic, counterionic and nonionic surfactants.
Claim 17
Dependent Claim
33 words
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.
Claim 18
Dependent Claim
33 words
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.
Claim 19
Dependent Claim
63 words
A process in accordance with claim 1 wherein the pigment dispersion of step (i) is accomplished by homogenizing at from about 1,000 to about 10,000 revolutions per minute and preferably between about 2,000 to about 5,000 revolutions per minute at a temperature of from about 20° C. to about 35° C. for a duration of from about 1 minute to about 120 minutes.
Claim 20
Dependent Claim
65 words
A process in accordance with claim 1 wherein the pigment 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.
Claim 21
Dependent Claim
34 words
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.
Claim 22
Dependent Claim
40 words
A process in accordance with claim 1 wherein the 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.
Claim 23
Dependent Claim
55 words
A process in accordance with claim 1 wherein the heating of the blend of latex, pigment, surfactants and optional charge control agent in step (iii) 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 to about 6 hours.
Claim 24
Dependent Claim
69 words
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. above the Tg of the resin for a duration of from about 1 hour to about 8 hours.
Claim 25
Dependent Claim
46 words
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).
Claim 26
Dependent Claim
37 words
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-butyl methacrylate-acrylic acid), or poly(styrene-butyl acrylate-acrylic acid), polyethylene-terephthalate, polypropylene-terephthalate, polybutylene-terephthalate, polypentylene-terephthalate, polyhexalene-terephthalate, polyheptadene-terephthalate, poly(styrene-butadiene), and polyoctalene-terephthalate.
Claim 27
Dependent Claim
84 words
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; and which surfactant is selected in an effective amount of from about 0.1 to about 5 percent by weight of the aqueous mixture.
Claim 28
Dependent Claim
70 words
A process in accordance with claim 1 wherein the anionic surfactant is selected from the group consisting of sodium dodecyl sulfate, sodium dodecylbenzene sulfate, sodium dodecyl naphthalene sulfate, sodium lauryl sulfate, sodium alkyl naphthalene sulfonate, potassium alkyl sulfonate; and which surfactant is selected in an effective concentration of from about 0.01 to about 10 percent and preferably from about 0.02 to about 5 percent by total weight of aqueous mixture.
Claim 29
Dependent Claim
57 words
A process in accordance with claim 1 wherein the cationic surfactant is an alkylbenzalkonium chloride selected in an effective concentration of from about 0.01 to about 10 percent and preferably from about 0.02 to about 2 percent by total weight of the aqueous mixture comprised of resin particles, pigment particles, ionic, counterionic and nonionic surfactants and water.
Claim 30
Dependent Claim
47 words
A process in accordance with claim 1 wherein the pigment is carbon black, cyan, yellow, magenta present in the amount of from about 0.1 to about 10 percent by weight, and wherein said pigment optionally is from about 0.01 to about 1 micron in volume average diameter.
Claim 31
Dependent Claim
46 words
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 statically bound aggregate particles formed in (iii) are from about 1 to about 10 microns in average volume diameter.
Claim 32
Dependent Claim
27 words
A process in accordance with claim 1 wherein the coalesced toner particles formed in (iv) are from about 1 to about 20 microns in average volume diameter.
Claim 33
Dependent Claim
36 words
A process in accordance with claim 1 wherein the toner particles isolated are from about 1 to 20 microns in average volume diameter, and the geometric size distribution thereof is from about 1.15 to about 1.26.
Claim 34
Dependent Claim
28 words
A process in accordance with claim 1 wherein the resulting toner is washed with warm water and the surfactants are removed from the toner surface, followed by drying.
Claim 35
Dependent Claim
50 words
A process in accordance with claim 1 wherein there is added to the surface of the isolated toner 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 of the obtained toner particles.
Claim 36
Dependent Claim
58 words
A process in accordance with claim 1 wherein the speed of shearing (ii) is in the range of from about 4,000 to about 15,000 revolutions per minute and preferably in the range of from about 6,000 to about 12,000 rpm thereby controlling the homogeneity of the blend of the latex particles, pigment, and oppositely charged surfactants in water.
Claim 37
Dependent Claim
30 words
A process in accordance with claim 1 wherein stirring is accomplished continuously at from about 200 to about 1,000 and preferably between about 300 to about 700 revolutions per minute.
Claim 38
Dependent Claim
48 words
A process in accordance with claim 1 wherein the electrostatically bound aggregated particles are heated to a temperature of from about 5° C. to about 50° C. above the resin Tg (step vii), which resin Tg is in range of from about 40° C. to about 85° C.
Claim 39
Dependent Claim
17 words
A process in accordance with claim 9 wherein said speed is from about 6,000 to about 12,000.
Claim 40
Dependent Claim
28 words
A process in accordance with claim 1 wherein the particle size of the formed toner is from about 1 to about 25 microns in volume median diameter size.
Claim 41
Dependent Claim
27 words
A process in accordance with claim 1 wherein the particle size of the formed toner is from about 3 to about 7 microns in average volume diameter.
Claim 42
Dependent Claim
33 words
A process in accordance with claim 1 wherein subsequent to (iv) the following steps are accomplished; (viii) separating said toner particles from water and surfactant by filtration; and (ix) drying said toner particles.
Claim 43
Dependent Claim
406 words
A process for the preparation of toner comprising: (i) preparing a pigment dispersion in water, which dispersion is comprised of a pigment of a diameter of from about 0.01 to about 1 micron, and an ionic surfactant; (ii) shearing the pigment dispersion with a latex blend comprised of resin of submicron size of from about 0.01 to about 1 micron, a counterionic surfactant with a charge polarity of opposite sign to that of said ionic surfactant and a nonionic surfactant thereby causing a flocculation or heterocoagulation of the formed particles of pigment, and resin to form a uniform viscous dispersion of solids comprised of resin and pigment particles in a combined content of from about 5 percent to about 25 percent in the water and anionic/nonionic/cationic surfactant system; (iii) heating the sheared blend of latex and pigment particles at a temperature of equal to or from about 25° C. to about 5° C. below the Tg of the resin, which resin Tg is in the range of about 40° C. to about 85° C. and preferably is in the range of from about 50° C. to about 75° C., while continuously stirring at about 150 to 450 revolutions per minute to form electrostatically bound toner size aggregates; (iv) reshearing the above electrostatically bound toner aggregates (iii) and which aggregates possess an undesirable, or out of specification broad particle size distribution of from about 1.30 to about 3.00; (v) heating the above sheared homogeneous blend equal to or below the glass transition temperature (Tg) of the resin particles while continuously stirring at about 450 to 800 rpm, or tip speeds of about 240 to about 440 centimeters/second to form electrostatically bound toner size aggregates with a narrow particle size distribution of from about 1.18 to about 1.28; (vi) adding further anionic or nonionic surfactant in the range of from about 0.1 to about 10 percent by weight of water to control, prevent, or minimize further growth or enlargement of the particles in the coalescence step (vii); (vii) heating the statically bound aggregated particles at a temperature of from about 5° to about 50° C. equal to or above the resin Tg, which Tg is in the range of from about 40° C. to about 80° C. to provide a mechanically stable toner composition comprised of polymeric resin, and pigment; and optionally (vii) separating said toner particles from the water by filtration, and (ix) drying said toner particles.
Claim 44
Dependent Claim
406 words
A process for the preparation of toner comprising: (i) preparing a pigment dispersion in water, which dispersion is comprised of a pigment of a diameter of from about 0.01 to about 1 micron, and an ionic surfactant; (ii) shearing the pigment dispersion with a latex blend comprised of resin of submicron size of from about 0.01 to about 1 micron, a counterionic surfactant with a charge polarity of opposite sign to that of said ionic surfactant and a nonionic surfactant thereby causing a flocculation or heterocoagulation of the formed particles of pigment, and resin to form a uniform viscous dispersion of solids comprised of resin and pigment particles in a combined content of from about 5 percent to about 25 percent in the water and anionic/nonionic/cationic surfactant system; (iii) heating the sheared blend of latex and pigment particles at a temperature of equal to or from about 25° C. to about 5° C. below the Tg of the resin, which resin Tg is in the range of about 40° C. to about 85° C. and preferably is in the range of from about 50° C. to about 75° C., while continuously stirring at about 150 to 450 revolutions per minute to form electrostatically bound toner size aggregates; (iv) reshearing the above electrostatically bound toner aggregates (iii) and which aggregates possess an undesirable, or out of specification broad particle size distribution of from about 1.30 to about 3.00; (v) heating the above sheared homogeneous blend equal to or below the glass transition temperature (Tg) of the resin particles while continuously stirring at about 450 to 800 rpm, or tip speeds of about 240 to about 440 centimeters/second to form electrostatically bound toner size aggregates with a narrow particle size distribution of from about 1.18 to about 1.28; (vi) adding further anionic or nonionic surfactant in the range of from about 0.1 to about 10 percent by weight of water to control, prevent, or minimize further growth or enlargement of the particles in the coalescence step (vii); (vii) heating the statically bound aggregated particles at a temperature of from about 5° to about 50° C. equal to or above the resin Tg, which Tg is in the range of from about 40° C. to about 80° C. to provide a mechanically stable toner composition comprised of polymeric resin, and pigment; and optionally (vii) separating said toner particles from the water by filtration, and (ix) drying said toner particles.
Claim 45
Dependent Claim
66 words
A process in accordance with claim 42 wherein said resin Tg of (iii) is in the range of from about 40° C. to about 85° C. and preferably in the range of from about 50° C. to about 75° C., said speed of reshearing is from about 3,000 to about 15,000 revolutions per minute accomplished for a period of from about 1 to about 60 minutes.
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