Styrene → Isobutylene styrene

HRID 2408162ノート

反応式

HRID 2408162 の反応式
[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].CC(=C)C.C=CC1C=CC=CC=1>[Ti](Cl)(Cl)(Cl)Cl.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]

参加物

7

反応条件

温度
-70 °C

実験手順

In a 2 L reaction vessel equipped with a stirrer, 589 mL of methylcyclohexane (dried over molecular sieves), 613 mL of n-butyl chloride (dried over molecular sieves) and 0.550 g of cumyl chloride were charged. After cooling the reaction vessel to −70° C., 0.35 mL of α-picoline(2-methylpyridine) and 179 mL of isobutylene were added. Further, 9.4 mL of titanium tetrachloride was added to start polymerization, and then the solution was reacted for 2.0 hours while being stirred at −70° C. Next, 59 mL of styrene was added into the reaction vessel and the reaction was continued for 60 minutes, and then the reaction was terminated by adding a large amount of methanol. After removing the solvent and the like from the reaction solution, a polymer was dissolved in toluene and washed twice with water. This toluene solution was added to the methanol mixture, thereby precipitating a polymer, and the resultant polymer was dried at 60° C. for 24 hours to obtain a styrene-isobutylene diblock copolymer. The resultant styrene-isobutylene diblock copolymer has a weight-average molecular weight of 70,000 and a styrene unit content of 15% by mass.

後処理

  1. customIn a 2 L reaction vessel
  2. customequipped with a stirrer
  3. custompolymerization
  4. customthe solution was reacted for 2.0 hours
  5. customthe reaction was terminated
  6. additionby adding a large amount of methanol
  7. customAfter removing the solvent
  8. dissolutionthe like from the reaction solution, a polymer was dissolved in toluene
  9. washwashed twice with water
  10. additionThis toluene solution was added to the methanol mixture
  11. customprecipitating a polymer
  12. dry with materialthe resultant polymer was dried at 60° C. for 24 hours

出典と根拠

ORDレコード
ord-e6a1c91ed9a94ae08fd5035513497206
出典データセット
uspto-grants-2014_08
特許番号
US08815033B2

反応ノート

読み込み中…