Styrene → Isobutylene styrene

HRID 1774243Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1774243
[CH3:1][CH:2]1[CH2:7]CCC[CH2:3]1.[C:8](Cl)([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)(C)[CH3:9].N1C=CC=CC=1C.CC(=C)C.C=CC1C=CC=CC=1>[Ti](Cl)(Cl)(Cl)Cl.CO.C(Cl)CCC>[CH2:9]=[CH:8][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.[CH3:3][C:2](=[CH2:1])[CH3:7]

Komponenten

9

Edukt 5

HCID 7501StyreneHCID 7962MethylcyclohexaneHCID 79752-MethylpyridineHCID 8255IsobutyleneHCID 70281(1-Chloro-1-methylethyl)benzene

Produkt 1

HCID 44154101Isobutylene styrene

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 24193Titanium TetrachlorideKatalysatorHCID 887MethanolLösungsmittelHCID 8005Butyl ChlorideLösungsmittel

Reaktionsbedingungen

Temperatur
-70 °C

Versuchsvorschrift

Methylcyclohexane (dried with molecular sieves) of 589 mL, n-butyl chloride (dried with molecular sieves) of 613 mL, and cumyl chloride of 0.550 g were added to a 2 L reaction container having an agitator. After cooling the reaction container to −70° C., α-picoline (2-methylpyridine) of 0.35 mL and isobutylene of 179 mL were added. Titanium tetrachloride of 9.4 mL was further added, and the polymerization was stared. The solution was agitated at −70° C. and allowed to react for 2.0 hours. Next, styrene of 59 mL was added to the reaction container, and the reaction was continued for 60 minutes. After that, a large amount of methanol was added to stop the reaction. After a solvent and the like were removed from the reaction solution, the polymer was dissolved in toluene and washed twice. The toluene solution was added to a methanol mixture to deposit the polymer, and the obtained polymer was dried at 60° C. for 24 hours to obtain a styrene-isobutylene diblock copolymer.

Aufarbeitung

  1. customto react for 2.0 hours
  2. customthe reaction
  3. customAfter a solvent and the like were removed from the reaction solution
  4. dissolutionthe polymer was dissolved in toluene
  5. washwashed twice
  6. additionThe toluene solution was added to a methanol mixture
  7. customthe obtained polymer was dried at 60° C. for 24 hours

Quellen und Nachweise

ORD-Eintrag
ord-87527eaccbca4443b490e5c7bedd1d20
Quelldatensatz
uspto-grants-2016_02
Patentnummer
US09259969B2

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