Methacrylic Acid → Propylene glycol methyl ether acetate

Temperature

80 °C

A monomer solution was prepared by placing 7000 g of MEK in a tank kept at a nitrogen atmosphere and dissolving 2220 g of (B) 5-methacryloyloxy-2,6-norbornanecarbolactone (hereinafter inscribed as “NLM”), 2480 g of EAM and 90 g of methacrylic acid. Also, a polymerization initiator was prepared by placing and dissolving 700 g of MEK and 80 g of AIBN in another container kept at the nitrogen atmosphere. Into a polymerization tank kept at the nitrogen atmosphere, 3300 g of MEK was put and the temperature was raised to 80° C. with stirring. Subsequently, the monomer solution and the polymerization initiator solution kept at the temperature of 25 to 30° C. were fed into the polymerization tank kept at 8.0° C. over 4 hours, respectively. After the completion of feed, the polymerized solution was matured for 2 hours with keeping the polymerization temperature at 80° C., then cooled to room temperature and taken out. Polymer was precipitated from the resulting polymerized solution by dropping in 80 kg of aqueous methanol and filtrated. The resultant wet cake was washed with 80 kg of methanol, filtrated subsequently dissolved in MEK again, and passed through a filter 40QSH supplied from Cuno Incorporated to remove a trace amount of metals. Then, the solvent was replaced by PGMEA with removing MEK by heating under reduced pressure to prepare PGMEA solution containing 15% polymer. The features of the resultant polymer, the content of high polymer and the evaluation results of storage stability of PGMEA solution are shown in Table 1.

1. customA monomer solution was prepared
2. customAlso, a polymerization initiator was prepared
3. customkept at the temperature of 25 to 30° C.
4. waitAfter the completion of feed, the polymerized solution was matured for 2 hours
5. customat 80° C.
6. temperaturecooled to room temperature
7. customPolymer was precipitated from the resulting
8. custompolymerized solution
9. filtrationfiltrated
10. washThe resultant wet cake was washed with 80 kg of methanol
11. filtrationfiltrated subsequently
12. dissolutiondissolved in MEK again
13. filtrationa filter
14. customto remove a trace amount of metals
15. temperatureby heating under reduced pressure
16. customto prepare PGMEA solution

ORD record

ord-9dce0c5232394236b39a4e596685ffa5

Source dataset

uspto-grants-2012_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08163852B2