Indene → Isopropenyltoluene indene

HRID 1740697

반응식

HRID 1740697 반응식
[C:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[CH3:10])([CH3:3])=[CH2:2].[CH2:11]1[C:19]2[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=2)[CH:13]=[CH:12]1.[OH-].[Na+]>>[C:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[CH3:10])([CH3:3])=[CH2:2].[CH2:11]1[C:19]2[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=2)[CH:13]=[CH:12]1

참가 물질

4

실험 절차

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 40/60 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 2 hours, the reaction mixture was discharged continuously. After a period of time three times 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 (3). This copolymer had a softening point Tm of 170° C., a number average molecular weight Mn of 1500, and a weight average molecular weight Mw of 2700.

후처리

  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 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

출처 및 근거

ORD 기록
ord-582771cdf56949ff8e36596705921db6
출처 데이터셋
uspto-grants-1999_10
특허 번호
US05972547

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