US3839307A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Process of producing polyvinyl alcohol microgels
Assignee: EIDP Inc
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Filing: 1972-06-05
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Granted: 1974-10-01
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Expires: 1992-06-05
Abstract
Abstract Polyvinyl alcohol microgels which comprise stable fluids comprising water and about 0.05 to 10 percent by weight of polyvinyl alcohol partially crosslinked with tetravalent titanium ions, said microgels being derived from polyvinyl alcohol which has a Hoeppler viscosity of about 4 to 150 centipoises and in which at least about 50 mole percent of the monomeric units are vinyl alcohol units, said partially crosslinked polyvinyl alcohol and water having a Brookfield viscosity of about 1.15 to 2000 centipoises, said viscosity being at least about 15 percent greater than the viscosity of the aqueous polyvinyl alcohol solution from which the microgel is derived, are useful as sizes for paper and paperboard, in paper and paperboard coatings, as warp sizes for textile fibers, as adhesives, and as soil and dust stabilizers.
Inventors
- 👤 J Schmifg
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-25 22:50
CPC Classifications
B; B01; B01J; B01J13/00; B01J13/0052; B01J13/0065; D; D21; D21H; D21H17/00; D21H17/71; D21H19/00; D21H19/10; D21H19/14; D21H19/20; D21H17/03; D21H17/05; D21H17/06; D21H17/07; D21H17/20; D21H17/33; D21H17/34; D21H17/36; D21H17/63; D21H17/66; D21H17/67; D21H21/00; D21H21/14; D21H21/16
Claims Analysis
Total Claims: 10
Claim 1
Independent Claim
188 words
A PROCESS FOR PREPARING A STABLE, FLUID POLYVINYL ALCOHOL MICROGEL CONTAINING WATER AND 0.05 TO 10 PERCENT BY WEIGHT OF POLYVINYL ALCOHOL PARTIALLY CROSSLINKED WITH TETRAVALWNT TITANIUM IONS WHICH COMPRISES MIXING (A) WATER, (B) 0.05 TO 10 PERCENT BY WEIGHT, BASED ON THE TOTAL WATER AND POLYVINYL ALCOHOL COMPONENTS, OF POLYVINYL ALCOHOL WHICH HAS HOEPPLER VISCOSITY OF 4 TO 150 CENTIPOISES MASURED AS A 4 PERCENT AQUEOUS SOLUTION AT 20*C. BY FALLING BALL METHOD, AND IN WHICH AT LEAST 50 MOL PERCENT OF THE MONOMERIC UNITS ARE VINYL ALCOHOL UNITS, AND (C) A TITANIUM SALT OF A CHELATING ORGANIC ACID OR TWO TO 10 CARBON ATOMS WHICH IS PRESENT IN AN AMOUNT SUFFICIENT TO PROVIDE 0.05 TO 10 PARTS BY WEIGHT OF TETRAVALENT TITANIUM ION PER 100 PARTS BY WEIGHT OF POLYVINYL ALCOHOL AND CONVERTING SAID TITANIIUM COMPLEX TO TETRAVALENT TITANIUM ION BY ADJUSTING THE PH TO 6 TO 10 THEREBY FORMING A POLYVINYL ALCOHOL MICROGEL HAVING A BROOKFIELD VISCOSITY OF 1.15 TO 2000 CENTIPOISES, SAID VISCOSITY BEING AT LEAST 15 PERCENT GREATER THAN THE VISCOSITY OF THE AQUEOUS POLYVINYL ALCOHOL SOLUTION FROM WHICH THE MICROGEL IS DERIVED.
Claim 2
Dependent Claim
188 words
A PROCESS FOR PREPARING A STABLE, FLUID POLYVINYL ALCOHOL MICROGEL CONTAINING WATER AND 0.05 TO 10 PERCENT BY WEIGHT OF POLYVINYL ALCOHOL PARTIALLY CROSSLINKED WITH TETRAVALWNT TITANIUM IONS WHICH COMPRISES MIXING (A) WATER, (B) 0.05 TO 10 PERCENT BY WEIGHT, BASED ON THE TOTAL WATER AND POLYVINYL ALCOHOL COMPONENTS, OF POLYVINYL ALCOHOL WHICH HAS HOEPPLER VISCOSITY OF 4 TO 150 CENTIPOISES MASURED AS A 4 PERCENT AQUEOUS SOLUTION AT 20*C. BY FALLING BALL METHOD, AND IN WHICH AT LEAST 50 MOL PERCENT OF THE MONOMERIC UNITS ARE VINYL ALCOHOL UNITS, AND (C) A TITANIUM SALT OF A CHELATING ORGANIC ACID OR TWO TO 10 CARBON ATOMS WHICH IS PRESENT IN AN AMOUNT SUFFICIENT TO PROVIDE 0.05 TO 10 PARTS BY WEIGHT OF TETRAVALENT TITANIUM ION PER 100 PARTS BY WEIGHT OF POLYVINYL ALCOHOL AND CONVERTING SAID TITANIIUM COMPLEX TO TETRAVALENT TITANIUM ION BY ADJUSTING THE PH TO 6 TO 10 THEREBY FORMING A POLYVINYL ALCOHOL MICROGEL HAVING A BROOKFIELD VISCOSITY OF 1.15 TO 2000 CENTIPOISES, SAID VISCOSITY BEING AT LEAST 15 PERCENT GREATER THAN THE VISCOSITY OF THE AQUEOUS POLYVINYL ALCOHOL SOLUTION FROM WHICH THE MICROGEL IS DERIVED.
Claim 3
Dependent Claim
57 words
The process of claim 1 in which the mixture contains 4 to 8 percent by weight of polyvinyl alcohol which has a Hoeppler viscosity of 10 to 70 centipoises and in which at least 85 mole percent of the monomeric units are vinyl alcohol units, and the microgel has a Brookfield viscosity of 25 to 1000 centipoises.
Claim 4
Dependent Claim
62 words
The process of claim 2 in which the mixture contains 2 to 6 percent by weight of polyvinyl alcohol which has a Hoeppler viscosity of 20 to 40 centipoises and in which at least 93 mole percent of the monomeric units in the polyvinyl alcohol are vinyl alcohol units, and the microgel has a a Brookfield viscosity of 30 to 500 centipoises.
Claim 5
Dependent Claim
21 words
The process of claim 1 in which the polyvinyl alcohol is a homopolymer which is at least 99 mole percent hydrolyzed.
Claim 6
Dependent Claim
13 words
The process of claim 4 in which the titanium complex is titanium citrate.
Claim 7
Dependent Claim
41 words
The process of claim 1 in which the polyvinyl alcohol is a copolymer derived 94 to 98 percent by weight from vinyl acetate and 2 to 6 percent by weight from methyl methacrylate and is at leasT 99 mole percent hydrolyzed.
Claim 8
Dependent Claim
13 words
The process of claim 6 in which the titanium complex is titanium citrate.
Claim 9
Dependent Claim
87 words
A dry polyvinyl alcohol microgel precursor mixture which comprises solid polyvinyl alcohol which has a Hoeppler viscosity of 4 to 150 centipoises measured as a 4 percent aqueous solution at 20*C. by the falling ball method and in which at least 50 mole percent of the monomeric units are vinyl alcohol units sprayed with a liquid mixture of lactic acid and tetraisopropyl titanate in an amount sufficient to provide 0.05 to 10 parts by weight of tetravalent titanium ion per 100 parts by weight of polyvinyl alcohol.
Claim 10
Dependent Claim
87 words
A dry polyvinyl alcohol microgel precursor mixture which comprises solid polyvinyl alcohol which has a Hoeppler viscosity of 4 to 150 centipoises measured as a 4 percent aqueous solution at 20*C. by the falling ball method and in which at least 50 mole percent of the monomeric units are vinyl alcohol units sprayed with a liquid mixture of lactic acid and tetraisopropyl titanate in an amount sufficient to provide 0.05 to 10 parts by weight of tetravalent titanium ion per 100 parts by weight of polyvinyl alcohol.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1977-09-30 | 1978-04-01 | 1978-10-01 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1981-09-30 | 1982-04-01 | 1982-10-01 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1985-09-30 | 1986-04-01 | 1986-10-01 | $7700.00 | Window Closed / Lapsed |