US5322912A — Polymerization processes and toner compositions t…

Claim 1

Independent Claim 79 words

A free radical polymerization process for the preparation of a thermoplastic resin or resins comprising: heating from about 100° to about 160° C. a mixture comprised of a free radical initiator, a stable free radical agent, and at least one polymerizable monomer compound to form said thermoplastic resin or resins with a polydispersity of about 1.0 to about 2.0; cooling said mixture; optionally isolating said thermoplastic resin or resins; and optionally washing and drying said thermoplastic resin or resins.

Claim 2

Dependent Claim 79 words

A free radical polymerization process for the preparation of a thermoplastic resin or resins comprising: heating from about 100° to about 160° C. a mixture comprised of a free radical initiator, a stable free radical agent, and at least one polymerizable monomer compound to form said thermoplastic resin or resins with a polydispersity of about 1.0 to about 2.0; cooling said mixture; optionally isolating said thermoplastic resin or resins; and optionally washing and drying said thermoplastic resin or resins.

Claim 3

Dependent Claim 17 words

A process in accordance with claim 1 wherein the heating is conducted in a solvent or diluent.

Claim 4

Dependent Claim 36 words

A process in accordance with claim 1 wherein the heating of said mixture is conducted with said mixture as a suspension in water or in a polar liquid which is not miscible with said monomer compound.

Claim 5

Dependent Claim 25 words

A process in accordance with claim 1 wherein the heating of said mixture is conducted with said mixture neat or in the absence of solvent.

Claim 6

Dependent Claim 33 words

A process in accordance with claim 1 wherein the thermoplastic resin product has a polydispersity of from about 1.1 to about 1.45 and a monomer to polymer conversion of greater than 50 percent.

Claim 7

Dependent Claim 17 words

A process in accordance with claim 1 wherein the heating is from about 1 to 60 hours.

Claim 8

Dependent Claim 21 words

A process in accordance with claim 1 wherein said polydispersity of said thermoplastic resin remains about constant throughout said polymerization process.

Claim 9

Dependent Claim 26 words

A process in accordance with claim 1 wherein said free radical initiator is selected from the group consisting of organic peroxides, azobisalkylnitriles, peroxycarbonates, and mixtures thereof.

Claim 10

Dependent Claim 21 words

A process in accordance with claim 1 wherein the stable free radical agent is comprised of a nitroxide stable free radical.

Claim 11

Dependent Claim 36 words

A process in accordance with claim 1 wherein the stable free radical agent is comprised of nitroxide stable free radicals selected from the group of consisting of 2,2,5,5-tetramethyl-1-pyrrolidinyloxy, derivatives thereof, 2,2,6,6-tetramethyl-1-piperidinyloxy, derivatives thereof, and mixtures thereof.

Claim 12

Dependent Claim 25 words

A process in accordance with claim 1 wherein the stable free radical agent to free radical initiator molar ratio is from about 0.4 to 2.5.

Claim 13

Dependent Claim 25 words

A process in accordance with claim 1 wherein the stable free radical agent to free radical initiator molar ratio is from about 0.9 to 1.8.

Claim 14

Dependent Claim 23 words

A process in accordance with claim 1 wherein the monomer to free radical initiator molar ratio is from about 100:1 to about 10,000:1.

Claim 15

Dependent Claim 20 words

A process in accordance with claim 1 wherein said monomer to polymer conversion is at least 90 percent by weight.

Claim 16

Dependent Claim 34 words

A process in accordance with claim 1 wherein the monomer compound is selected from the group consisting of styrene and derivatives thereof, conjugated dienes and derivatives thereof, acrylates and derivatives thereof, and mixtures thereof.

Claim 17

Dependent Claim 19 words

A process in accordance with claim 1 wherein said heating is from about 110° C. to about 160° C.

Claim 18

Dependent Claim 23 words

A process in accordance with claim 1 wherein said thermoplastic resin has a gel content of from 0.0 to about 0.5 weight percent.

Claim 19

Dependent Claim 26 words

A process in accordance with claim 1 wherein the weight average molecular weight (M w ) of the resin or resins are from 10,000 to 200,000.

Claim 20

Dependent Claim 32 words

A process in accordance with claim 1 wherein the polymeric chains of said resin are formed simultaneously at from about 0 to 10 minutes after said heating has attained about 100° C.

Claim 21

Dependent Claim 41 words

A process in accordance with claim 1 further comprising adding an organic sulfonic or organic carboxylic acid during heating of said mixture thereby increasing the rate of formation of said thermoplastic resin or resins from said polymerization of said monomer compound.

Claim 22

Dependent Claim 39 words

A process in accordance with claim 1 further comprising adding a tertiary amine promoter compound to said mixture thereby increasing the rate of dissociation of said free radical initiator and where said free radical initiator is an organic peroxide.

Claim 23

Dependent Claim 36 words

A process in accordance with claim 1 wherein said thermoplastic resin or resins has a polydispersity of from about 1.1 to about 2.0 and a monomer to polymer conversion of about 50 to about 90 percent.

Claim 24

Dependent Claim 29 words

A process in accordance with claim 1 wherein the molar ratio of monomer to stable free radical agent to free radical initiator is from about 100:0.2:1 to about 10,000:2.5:1.

Claim 25

Dependent Claim 116 words

A free radical polymerization process for the preparation of a thermoplastic resin or resins comprising: heating from about 100° to about 160° C. for an effective time period a water suspension mixture comprised of a peroxide free radical initiator, a nitroxide stable free radical agent, and at least one polymerizable monomer compound to form said thermoplastic resin or resins; cooling said mixture; optionally isolating said thermoplastic resin or resins; and optionally washing and drying said thermoplastic resin or resins, wherein said thermoplastic resin possesses a narrow polydispersity of from about 1.1 to about 1.5, a modality of 1, and wherein the process affords a monomer to polymer conversion of from about 10 to about 100 percent.

Claim 26

Dependent Claim 116 words

A free radical polymerization process for the preparation of a thermoplastic resin or resins comprising: heating from about 100° to about 160° C. for an effective time period a water suspension mixture comprised of a peroxide free radical initiator, a nitroxide stable free radical agent, and at least one polymerizable monomer compound to form said thermoplastic resin or resins; cooling said mixture; optionally isolating said thermoplastic resin or resins; and optionally washing and drying said thermoplastic resin or resins, wherein said thermoplastic resin possesses a narrow polydispersity of from about 1.1 to about 1.5, a modality of 1, and wherein the process affords a monomer to polymer conversion of from about 10 to about 100 percent.

Claim 27

Dependent Claim 20 words

A process in accordance with claim 24 wherein said effective time period is from about 30 minutes to 10 hours.

Claim 28

Dependent Claim 22 words

A process in accordance with claim 1 wherein said heating is for a period of from about 30 minutes to 30 hours.

Claim 29

Dependent Claim 26 words

A process in accordance with claim 1 wherein the stable free radical agent to free radical initiator molar ratio SFR:INIT is from about 1.2 to 1.8.

Claim 30

Dependent Claim 40 words

A process in accordance with claim 1 wherein the process has a monomer to polymer conversion of from about 10 to about 100 percent and the resin or resins polydispersity is in the range of about 1.0 to about 2.0.

Claim 31

Dependent Claim 28 words

A process in accordance with claim 1 wherein said free radical initiator has a half life of less than or equal to 10 minutes at above 100° C.

Claim 32

Dependent Claim 28 words

A process in accordance with claim 1 wherein said free radical initiator has a half life of less than or equal to 1 minute at above 100° C.

Claim 33

Dependent Claim 29 words

A process in accordance with claim 1 wherein said free radical initiator has a half life of from about 5 seconds to about 10 minutes at above 100° C.

Claim 34

Dependent Claim 23 words

A process in accordance with claim 1 wherein the process has a monomer to polymer conversion of from about 50 to 100 percent.

Claim 35

Dependent Claim 26 words

A process in accordance with claim 1 wherein the thermoplastic resin or resins possess a polydispersity in the range of from about 1.1 to about 1.45.

Claim 36

Dependent Claim 43 words

A process in accordance with claim 1 wherein the thermoplastic resin or resins possesses a polydispersity in the range of from about 1.1 to about 1.45 and wherein the process has a monomer to polymer conversion of from about 10 to 100 percent.

Claim 37

Dependent Claim 60 words

A free radical polymerization process for the preparation of a thermoplastic resin or resins comprising heating from about 100° to about 160° C. a mixture comprised of a free radical initiator, a stable free radical agent, and at least one polymerizable monomer compound to form said thermoplastic resin or resins with a polydispersity of from about 1.1 to about 1.45.

Claim 38

Dependent Claim 60 words

A free radical polymerization process for the preparation of a thermoplastic resin or resins comprising heating from about 100° to about 160° C. a mixture comprised of a free radical initiator, a stable free radical agent, and at least one polymerizable monomer compound to form said thermoplastic resin or resins with a polydispersity of from about 1.1 to about 1.45.

Claim 39

Dependent Claim 72 words

A polymerization process for the preparation of a thermoplastic resin or resins comprising heating from about 100° to about 160° C. a mixture comprised of a free radical initiator, a stable free radical agent, and at least one polymerizable monomer compound to form said thermoplastic resin or resins with a monomer to polymer conversion of from about 10 to about 100 percent and a polydispersity of from about 1.1 to about 1.45.

Claim 40

Dependent Claim 72 words

A polymerization process for the preparation of a thermoplastic resin or resins comprising heating from about 100° to about 160° C. a mixture comprised of a free radical initiator, a stable free radical agent, and at least one polymerizable monomer compound to form said thermoplastic resin or resins with a monomer to polymer conversion of from about 10 to about 100 percent and a polydispersity of from about 1.1 to about 1.45.

Annuity Stage	Window Opens	Payment Deadline	Surcharge Period Until	Estimated Fee	Status
3.5 Years (Year 4)	1997-06-20	1997-12-20	1998-06-21	$2000.00	Window Closed / Lapsed
7.5 Years (Year 8)	2001-06-20	2001-12-20	2002-06-21	$3760.00	Window Closed / Lapsed
11.5 Years (Year 12)	2005-06-20	2005-12-20	2006-06-21	$7700.00	Window Closed / Lapsed

Polymerization processes and toner compositions therefrom

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