US3914196A
Expired / Lapsed
US
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Polymeric pigments and method for preparation thereof
Assignee: Dow Chemical Co
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Filing: 1973-12-10
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Granted: 1975-10-21
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Expires: 1993-12-10
Abstract
Abstract Improved polymeric pigments for use in paper coatings are provided by a soap-free, emulsion polymerization process comprising the steps of (1) emulsion polymerizing at least 20 weight percent of total emulsion polymerizable monomer, (2) adding fluid base and (3) continuing emulsion polymerization of the remaining monomer charge.
Inventors
- 👤 Norman Raymond Loeffler
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-31 17:35
CPC Classifications
D; D21; D21H; D21H19/00; D21H19/36; D21H19/38; D21H19/42; C; C08; C08F; C08F2/00; C08F2/12; C08F2/16; C08F2/22; Y; Y10; Y10T; Y10T428/00; Y10T428/25; Y10T428/254
Claims Analysis
Total Claims: 16
Claim 1
Independent Claim
193 words
A METHOD FOR PREPARING AN AQUEOUS DISPERSION OF POLYMERIC PARTICLES WHICH ARE NON-FILM FORMING AT AMBIENT TEMPERATURE AND ARE USEFUL AS PIGMENT IN PAPER COATINGS, SAID PARTICLES HAVING ROUGH SURFACES AND AN AVERAGE PARTICLE DIAMETER IN THE RANGE FROM ABOUT 0.3 TO ABOUT 1.0 MICROMETER WITH NO MORE THAN ABOUT 5 WEIGHT PERCENT OF SAID OF PARTICLES BASED ON TOTAL WEIGHT OF PARTICLES HAVING DIAMETERS OUTSIDE SAID RANGE, WHICH METHOD COMPRISES THE STEPS OF (1) SUBJECTING TO EMULSION POLYMERIZATION A POLYMERIZATION REACTION MIXTURE COMPRISING AN AQUEOUS MEDIUM, A CATALYST AND AN INCREMENTALLYADDED INITIAL PORTION OF EMULSION POLYMERIZABLE MONOMER, ESSENTIALLY IN THE ABSENCE OF EXTERNAL EMULSIFIERS WHICH ARE CONVENTIONALLY EMPLOYED IN EMULSION POLYMERIZATION WHEREIN THE TERM EXTERNAL EMULSIFIERS EXCLUDES POLYMERIZATION CATALYSTS AND MONOMERIC MATERIALS, SAID INITIAL PORTION CONSTITUTING AT LEAST ABOUT 35 WEIGHT PERCENT UP TO AND INCLUDING 99.9 WEIGT PERCENT OF TOTAL MONOMER, (2) SUBSEQUENTLY ADDING FROM ABOUT 0.05 TO ABOUT 10 WEIGHT PERCENT BASED ON TOTAL MONOMER OF A FLUID BASE TO THE RECIPE: AND (3) CONTINUING ADDITION AND EMULSION POLYMERIZATION OF THE REMAINING PORTION OF THE TOTAL MONOMER, SAID TOTAL MONOMER BEING CAPABLE OF POLYMERIZING TO FORM A NON-FILM FORMING POLYMER.
Claim 2
Independent Claim
193 words
A METHOD FOR PREPARING AN AQUEOUS DISPERSION OF POLYMERIC PARTICLES WHICH ARE NON-FILM FORMING AT AMBIENT TEMPERATURE AND ARE USEFUL AS PIGMENT IN PAPER COATINGS, SAID PARTICLES HAVING ROUGH SURFACES AND AN AVERAGE PARTICLE DIAMETER IN THE RANGE FROM ABOUT 0.3 TO ABOUT 1.0 MICROMETER WITH NO MORE THAN ABOUT 5 WEIGHT PERCENT OF SAID OF PARTICLES BASED ON TOTAL WEIGHT OF PARTICLES HAVING DIAMETERS OUTSIDE SAID RANGE, WHICH METHOD COMPRISES THE STEPS OF (1) SUBJECTING TO EMULSION POLYMERIZATION A POLYMERIZATION REACTION MIXTURE COMPRISING AN AQUEOUS MEDIUM, A CATALYST AND AN INCREMENTALLYADDED INITIAL PORTION OF EMULSION POLYMERIZABLE MONOMER, ESSENTIALLY IN THE ABSENCE OF EXTERNAL EMULSIFIERS WHICH ARE CONVENTIONALLY EMPLOYED IN EMULSION POLYMERIZATION WHEREIN THE TERM EXTERNAL EMULSIFIERS EXCLUDES POLYMERIZATION CATALYSTS AND MONOMERIC MATERIALS, SAID INITIAL PORTION CONSTITUTING AT LEAST ABOUT 35 WEIGHT PERCENT UP TO AND INCLUDING 99.9 WEIGT PERCENT OF TOTAL MONOMER, (2) SUBSEQUENTLY ADDING FROM ABOUT 0.05 TO ABOUT 10 WEIGHT PERCENT BASED ON TOTAL MONOMER OF A FLUID BASE TO THE RECIPE: AND (3) CONTINUING ADDITION AND EMULSION POLYMERIZATION OF THE REMAINING PORTION OF THE TOTAL MONOMER, SAID TOTAL MONOMER BEING CAPABLE OF POLYMERIZING TO FORM A NON-FILM FORMING POLYMER.
Claim 3
Dependent Claim
25 words
The method of claim 1 wherein the amount of base is in the range from about 0.05 to about 10 weight percent of total monomer.
Claim 4
Dependent Claim
23 words
The method of claim 1 wherein the initial portion of monomer constitutes from about 80 to about 95 weight percent of total monomer.
Claim 5
Dependent Claim
10 words
The method of claim 1 wherein the base is ammonia.
Claim 6
Dependent Claim
25 words
The method of claim 1 wherein the amount of base is in the range from about 0.2 to about 7 weight percent of total monomer.
Claim 7
Dependent Claim
20 words
The method of claim 1 wherein total monomer comprises at least 45 weight percent of a monovinylidene carbocyclic aromatic monomer.
Claim 8
Dependent Claim
13 words
The method of claim 6 wherein the monovinylidene carbocylic aromatic monomer is styrene.
Claim 9
Dependent Claim
204 words
The method of claim 1 wherein (1) total monomer polymerizes to form a copolymer which is non-film forming at ambient temperature comprising from about 45 to about 99.5 weight percent polymerizable hard monomer selected from the group consisting of monovinylidene carbocyclic aromatic monomer, esters of Alpha , Beta -ethylenically unsaturated carboxylic acids which polymerize to form non-film forming polymers, Alpha , Beta -ethylenically unsaturated esters of non-polymerizable carboxylic acids which polymerize to form non-film forming polymers, Alpha , Beta -ethylenically unsaturated nitriles, other vinyl monomers which polymerize to form non-film forming polymers and mixtures of said hard monomers; up to about 45 weight percent of an emulsion polymerizable soft monomer selected from the group consisting of conjugated aliphatic dienes, alkyl acrylates, unsaturated esters of saturated carboxylic acids, esters and half esters of Alpha , Beta ethylenically unsaturated polycarboxylic acids, other vinyl monomers which polymerize to form film forming polymers, and mixtures of said soft monomers; and from about 0.5 to about 10 weight percent of at least one Alpha , Beta -ethylenically unsaturated carboxylic acid, and (2) the base is selected from the group consisting of ammonia gas, aqueous solutions of ammonia, alkali metal hydroxides and alkaline earth metal hydroxides, alkyl and alkanol amines.
Claim 10
Dependent Claim
66 words
The method according to claim 1 wherein total monomer polymerizes to form a non-film forming copolymer comprising from about 50 to about 99 weight percent of monovinylidene carbocyclic aromatic monomer; from about 0 to about 49 weight percent of emulsion polymerizable, Alpha , Beta -ethylenically unsaturated nitrile and from about 1 to about 5 weight percent of emulsion polymerizable, Alpha , Beta -ethylenically unsaturated carboxylic acid.
Claim 11
Dependent Claim
49 words
An aqueous dispersion of non-film forming polymeric particles having an average diameter in the range from about 0.3 to about 1.0 micrometer with no more than about 5 weight percent of said particles having diameters outside of said range, said dispersion being prepared by the method of claim 1.
Claim 12
Dependent Claim
74 words
The aqueous dispersion according to claim 10 wherein the polymeric particles comprise a copolymer of from about 50 to about 99 weight percent of monovinylidene carbocyclic aromatic monomer; from about 0 to about 49 weight percent of emulsion polymerizable Alpha , Beta -ethylenically unsaturated nitrile and from about 1 to about 5 weight percent of emulsion polymerizable Alpha , Beta -ethylenically unsaturated carboxylic acid wherein the copolymer is non-film forming at 140*F or less.
Claim 13
Dependent Claim
126 words
An aqueous paper coating composition adapted to a paper coating process for printing comprising a binder and a pigment wherein at least a portion of the total pigment is in the form of discrete, non-film forming polymeric particles having an average diameter in the range of from about 0.3 to about 1.0 micrometer, with no more than 5 weight percent of said particles having diameters outside of said range, said particles being formed by the method of claim 1, said coating composition containing from about 1.3 to about 11.5 volume parts of binder per 38.8 volume parts of pigment, said portion of polymeric particles being sufficient in said coating composition to produce a coating having improved properties, said particles being insoluble in water and the binder.
Claim 14
Dependent Claim
120 words
A coated paper comprising a paper substrate having intimately adhered thereto an improved coating comprising a binder and a pigment, at least a portion of said total pigment being in the form of discrete, non-film forming polymeric particles having an average diameter in the range of from about 0.3 to about 1.0 micrometer, with no more than 5 weight percent of said particles having diameters outside of said range, said particles being formed by the method of claim 1, the volume ratio of binder to pigment being in the range from about 1.3 to about 11.5 volume parts of binder to 38.8 volume pArts of pigment, said portion of polymeric particles being sufficient in said coating to impart improved properties.
Claim 15
Dependent Claim
21 words
The method of claim 1 wherein the initial portion constitutes from about 35 to about 95 weight percent of total monomer.
Claim 16
Dependent Claim
21 words
The method of claim 1 wherein the initial portion constitutes from about 80 to about 95 weight percent of total monomer.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1978-10-20 | 1979-04-21 | 1979-10-21 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1982-10-20 | 1983-04-21 | 1983-10-21 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1986-10-20 | 1987-04-21 | 1987-10-21 | $7700.00 | Window Closed / Lapsed |