US4530956A
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Process for the preparation of aqueous dispersions of organic material and possible further conversion to a polymer dispersion when the organic material is a polymerizable monomer
Assignee: SINTEF AS
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Filing: 1982-10-19
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Granted: 1985-07-23
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Expires: 2002-10-19
Abstract
Abstract Process for preparing aqueous dispersions of a somewhat water-soluble low-molecular organic material, in which swellable particles prepared in a first step are swelled with the organic material in the second step. When the organic material is a polymerizable monomer the dispersion prepared is converted to a polymer dispersion. In the first step swellable oligomer or oligomer-polymer particles are prepared by (a) dispersing an aqueous mixture containing an oil-soluble initiator or a solution of an oil soluble initiator in an organic solvent, and then swelling the dispersed initiator-containing droplets with monomer and effecting polymerization, or (b) swelling polymer particles in aqueous dispersion with vinyl monomer and an oil-soluble initiator and effecting polymerization, the ratio between initiator and monomer used being so high that in the polymerization an oligomer having a degree of polymerization of 5-200 is formed. In the second step, optionally after dilution with water and addition of emulsifier, the organic material is added which has a solubility in water of >10, preferably >100 times higher than that of the oligomer and which diffuses through the aqueous phase and swells the oligomer or oligomer-polymer particles in a ratio by volume of >20:1. When the organic material is a polymerizable monomer, initiator is also added in the second step, and polymerization is effected.
Inventors
- 👤 John Ugelstad
- 👤 Arvid Berge
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-26 11:59
CPC Classifications
C; C08; C08F; C08F257/00; C08F257/02; C08F2/00; C08F2/12; C08F2/16; C08F2/22; C08F291/00
Claims Analysis
Total Claims: 11
Claim 1
Independent Claim
222 words
Process for the preparation of aqueous dispersions of somewhat water-soluble, low molecular weight organic material, in which swellable particles prepared in a first step are swelled with the organic material in a second step, and, if desired, the prepared dispersion is converted to a polymer dispersion when the organic material is a polymerizable monomer, and wherein in the first step, oligomer or oligomer-polymer particles are prepared by (a) dispersing an aqueous mixture which contains an oil-soluble initiator or a solution of an oil-soluble initiator in an organic solvent, and then swelling the dispersed initiator-containing drops with monomer and effecting polymerization, or (b) swelling polymer particles in an aqueous dispersion with vinyl monomer and an oil-soluble initiator and effecting polymerization, the ratio between initiator and monomer used being so high that in the polymerization an oligomer having a degree of polymerization of 5-200 is formed, and in the second step, if desired after dilution with water and addition of emulsifier, the organic material is added which has a solubility in water >10, preferably >100 times higher than that of the oligomer, and which diffuses through the aqueous phase and swells the oligomer or oligomer-polymer particles in a ratio by volume of >20:1, and when the organic material is a polymerizable monomer, initiator is also added in the second step, and polymerization is effected.
Claim 2
Dependent Claim
222 words
Process for the preparation of aqueous dispersions of somewhat water-soluble, low molecular weight organic material, in which swellable particles prepared in a first step are swelled with the organic material in a second step, and, if desired, the prepared dispersion is converted to a polymer dispersion when the organic material is a polymerizable monomer, and wherein in the first step, oligomer or oligomer-polymer particles are prepared by (a) dispersing an aqueous mixture which contains an oil-soluble initiator or a solution of an oil-soluble initiator in an organic solvent, and then swelling the dispersed initiator-containing drops with monomer and effecting polymerization, or (b) swelling polymer particles in an aqueous dispersion with vinyl monomer and an oil-soluble initiator and effecting polymerization, the ratio between initiator and monomer used being so high that in the polymerization an oligomer having a degree of polymerization of 5-200 is formed, and in the second step, if desired after dilution with water and addition of emulsifier, the organic material is added which has a solubility in water >10, preferably >100 times higher than that of the oligomer, and which diffuses through the aqueous phase and swells the oligomer or oligomer-polymer particles in a ratio by volume of >20:1, and when the organic material is a polymerizable monomer, initiator is also added in the second step, and polymerization is effected.
Claim 3
Dependent Claim
39 words
Process according to claim 1, wherein in the first step oligomer-polymer particles are prepared by swelling dispersed polymer particles with initiator and vinyl monomer, wherein the molar ratio between monomer and initiator is 0.25:1 to 50:1, and effecting polymerization.
Claim 4
Dependent Claim
68 words
Process according to claim 1, wherein in the first step oligomer-polymer-particles are prepared by first swelling the polymer particles in a dispersion with an initiator having a very low solubility in water in a ratio by volume between initiator and polymer particles of 0.25:1 to 20:1, and then swelling with monomer in a molar ratio of monomer to initiator of 0.25:1 to 50:1, and forming oligomer by polymerization.
Claim 5
Dependent Claim
31 words
Process according to claim 1, wherein as organic material in the second step there is added a vinyl monomer which after absorption in the particles is polymerized with an oil-soluble initiator.
Claim 6
Dependent Claim
102 words
Process according to claim 4, wherein in the second step the oligomer-polymer particles prepared in the first step are swelled with an oil-soluble initiator having a very low solubility in water in a ratio by volume of initiator:particles of 10:1 to 200:1, and then vinyl monomer is added in a proportion by volume relative to the initiator of 30:1 to 1000:1, under conditions in which the initiator added in the second step is not transported out of the particles prepared in the first step, while the vinyl monomer diffuses into said particles, whereby polymerization of the monomer takes place inside the particles.
Claim 7
Dependent Claim
53 words
Process according to claim 3, wherein to facilitate the incorporation of the initiator having a very low solubility in water in the polymer og oligomer-polymer particles respectively, a dispersion of the initiator or a solution of the initiator is prepared and is added to the dispersion of the polymer and oligomer-polymer particles respectively.
Claim 8
Dependent Claim
80 words
Process according to claim 3, wherein in order to increase the rate and the capacity of swelling with an initiator having a very low solubility in water into the polymer particles in the first step and/or the oligomer-polymer particles in the second step, there is used a solvent for the initiator which is miscible with water and which is used in an amount of 5 to 200% based on the water in the system, for the incorporation of the initiator.
Claim 9
Dependent Claim
27 words
Process according to claim 1 for the preparation of monodisperse polymer particles, wherein in the first step for the preparation of oligomer-polymer-particles, monodisperse polymer particles are used.
Claim 10
Dependent Claim
51 words
Process according to claim 1, wherein oligomer particles are prepared in the first step by (1) dispersing an oil-soluble initiator or a solution thereof in an organic solvent together with water and emulsifier, (2) adding monomer in a molar ratio to the initiator of 0.25:1 to 50:1 and (3) effecting polymerization.
Claim 11
Dependent Claim
86 words
Process according to claim 1, wherein to the oligomer particles prepared according to claim 9 there is added an initiator having a very low solubility in water of <10 -3 g/l H 2 O which is allowed to swell the oligomer particles and which is added in a ratio by volume to the oligomer particles of 10:1 to 200:1, whereafter vinyl monomer is added in a ratio by volume to the initiator of 30:1 to 1000:1, whereby polymerization of the monomer takes place inside the particles.
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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) | 1988-07-22 | 1989-01-21 | 1989-07-23 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1992-07-22 | 1993-01-21 | 1993-07-23 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1996-07-22 | 1997-01-21 | 1997-07-23 | $7700.00 | Window Closed / Lapsed |