Indene → Isopropenyltoluene indene

Isopropenyltoluene, indene, dehydrated and purified toluene, and a boron trifluoride phenolate complex (1.6-times equivalent of phenol) diluted to 10-times volume with dehydrated and purified toluene were continuously supplied to an autoclave having a net capacity of 1270 ml equipped with a stirring blade, so that the ratio by mol of isopropenyltoluene to indene was 50/50 and the total supplied amount of isopropenyltoluene and indene was 1.0 l/h. The mixture was polymerized at a reaction temperature of 5° C. Subsequently, the reaction mixture was transferred to a second-stage autoclave and the polymerization reaction was continued at 5° C. Then, when the total retention time in the first- and second-stage autoclaves reached 1.5 hours, the reaction mixture was discharged continuously. After a period of time three times of the retention time had elapsed, the polymerization reaction was completed. After completion of the polymerization, an aqueous 1N NaOH solution was added to the reaction mixture to terminate the polymerization reaction. The resulting reaction mixture was washed with large amounts of water five times; then, the solvent and unreacted monomers were distilled off under reduced pressure by an evaporator to obtain an isopropenyltoluene/indene copolymer (4). This copolymer had a softening point Tm of 95° C., a number average molecular weight Mn of 770, and a weight average molecular weight Mw of 960.

1. custompurified toluene
2. additiona boron trifluoride phenolate complex (1.6-times equivalent of phenol) diluted to 10-times volume with dehydrated and
3. custompurified toluene
4. customequipped with a stirring blade, so that the ratio by mol of isopropenyltoluene to indene
5. customThe mixture was polymerized at a reaction temperature of 5° C
6. customthe polymerization reaction
7. customwas continued at 5° C
8. waitAfter a period of time three times of the retention time had elapsed
9. customthe polymerization reaction
10. customAfter completion of the polymerization
11. customto terminate
12. customthe polymerization reaction
13. customThe resulting reaction mixture
14. washwas washed with large amounts of water five times
15. distillationthen, the solvent and unreacted monomers were distilled off under reduced pressure by an evaporator

ORD 기록

ord-c926e99b0a054b38bd450bcab5a72f2e

출처 데이터셋

uspto-grants-1999_10

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US05972547