Patent Application
20080058457
A 250 ml flask outfitted with a magnetic stirrer, a reflux condenser, a thermocouple, and a N2-inlet was charged with 130 g EtOH, 0.7 g AIBN, 0.8 g AESH.HCl, and 79.38 g NIPAM. The flask was purged with N2, then heated to 80° C., at which point the heating mantel was removed and air cooling was used to offset the exotherm and return the flask to 78° C. The temperature was held at 78° C. for 4 hrs, then cooled to room temperature. 1.13 g of ICEMA was added to the flask. After standing overnight, the solids were determined to be 37.0%. The copolymerized macromer was determined to have a cloud point of 28° C.
A 500 ml flask outfitted with a magnetic stirrer, a reflux condenser, a thermocouple, and a N2-inlet was charged with 220 g EtOH, 1.6 g AIBN. For a Theoretical Molecular Weight of 5000 g/mol, 1.72 g of AESH.HCL was added to the flask; for a Theoretical Molecular Weight of 10000 g/mol, 0.86 g of AESH.HCL was added to the flask; and for a Theoretical Molecular Weight of 20000 g/mol, 0.43 g of AESH.HCL was added to the flask. For each copolymerized macromer composition, the mass of each monomer was added as indicated in TABLE 1. The flask was purged with N2, then heated to 78° C., at which point the heating mantel was removed and air cooling was used to offset the exotherm and return the flask to 78° C. The temperature was held at 78° C. for 4 hrs, then cooled to room temperature. For a Theoretical Molecular Weight of 5000 g/mol, 3.2 g of ICEMA was added to the flask; for a Theoretical Molecular Weight of 10000 g/mol, 1.6 g of ICEMA was added to the flask; and for a Theoretical Molecular Weight of 20000 g/mol, 0.8 g of ICEMA was added to the flask. After standing overnight, the solids were determined to be 37.0%.
A 250 ml flask outfitted with a magnetic stirrer, a reflux condenser, a thermocouple, and a N2-inlet was charged with 220 g EtOH, 1.6 g AIBN, 0.94 g APhSH, 0.45 g of acid acetic and 75 g NIPAM. The flask was purged with N2, then heated to 78° C., at which point the heating mantel was removed and air cooling was used to offset the exotherm and return the flask to 78° C. The temperature was held at 78° C. for 4 hrs, then cooled to room temperature. 3.6 g of ICEMA was added to the flask. After standing overnight, the solids were determined to be 37.0%. The copolymerized macromer was determined to have a cloud point of 28° C.
A 250 ml flask outfitted with a magnetic stirrer, a reflux condenser, a thermocouple, and a N2-inlet was charged with 50 g Dioxane, 0.28 g of VAZO 52, 17.5 g HEMA and 5 g MAM and 7 g CoBF solution. The CoBF solution was made my mixing 0.005 of CoBF with 50 g of Dioxane. The flask was purged with N2, then heated to 75° C., at which point the heating mantel was removed and air cooling was used to offset the exotherm and return the flask to 75° C. The temperature was held at 75° C. for 3 hrs, then cooled to room temperature. The copolymerized macromer was determined to have a cloud point of 28° C.
A 250 ml flask was charged with 10.71 g of Example 1M and air was blown through the flask while stirring to remove the ethanol. 69.8 g water and 0.38 g Disponil FES-32 was added to the flask and stirring continued to dissolve the pNIPAM macromer. A monomer emulsion was made by combining 22.21 g water, 2.01 g Disponil FES-32, 37.1 g BA, and 34.2 g MMA. 6.13 g of the monomer emulsion was added to flask at room temperature, then the flask was purged with N2 and heated to 85° C. 0.31 g APS in 2.5 g water was added to flask, and the flask was held at 85° C. for 10 min, then the rest of the monomer emulsion was fed in over 1 hr. The flask was held at 85° C. for 20 min after the feed was completed, then the reaction was chased with one addition of 0.41 g FeSO4 (1%) and two additions of 0.06 g tBHP/0.83 g water+0.025 g IAA/0.83 g water, with 15 min between chases. After cooling to room temperature, the particle size was measured as 310 nm.
A 500 ml flask was charged with 120 g of water, 0.6 g of sodium carbonate and 0.76 g Disponil FES-32. A monomer emulsion was made by combining 33 g of water, 4.02 g Disponil FES-32, 74.2 g BA, 68.4 g MMA and 1.43 g of MAA. 12.26 g of the monomer emulsion was added to flask at room temperature, and then the flask was purged with N2 and heated to 85° C. 0.62 g APS in 5 g water was added to flask and the flask was held at 85° C. for 10 min, and then 90% of the monomer emulsion was fed in over 1 hr. The flask was held at 85° C. for 20 min, then cooled to RT. 8 g of 2M macromer dissolved in 55 g of water added to the flask, then flask heated up to 85° C. The feed of the rest of monomer emulsion was terminated, the flask was held at 85° C. for 20 min after the feed was completed, then the reaction was chased with one addition of 0.82 g FeSO4 (1%) and two additions of 0.12 g tBHP/1.7 g water+0.05 g IAA/1.7 g water, with 15 min between chases. After cooling to room temperature, the particle size was measured as 180 nm, and solid content was 38.2%.
| Number | Date | Country | Kind |
|---|---|---|---|
| 06291398.3 | Aug 2006 | EP | regional |
| 06291398.3 | Aug 2006 | FR | national |
