Styrene → Diisobutylene styrene

HRID 719621

反応式

HRID 719621 の反応式
[CH2:1]=[CH:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.C(OCCCO)(=O)C=C.C[C@@:19]12[CH:27]([C:28](C([O-])=O)=C)[CH2:26][C@H:22]([C:23]1([CH3:25])[CH3:24])CC2.C(OCCCC)(=O)C=C>>[CH3:28][C:27]([CH2:19][C:23]([CH3:25])([CH3:24])[CH3:22])=[CH2:26].[CH2:1]=[CH:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1

参加物

5

反応条件

温度
150 °C

実験手順

Charge 1 was added to a 4-liter stirred stainless steel pressure reactor. The reactor was pressurized with nitrogen providing a 5 psig pad on the reactor. The agitation on the reactor was set at 500 rpm and the reactor temperature was adjusted to 150° C. Charge 2 was added to the reactor at an addition rate of 36 grams/hour over a 2.5 hour period. After 15 minutes Charge 3 was added to reactor at an addition rate of 1000 grams/hour over a 2 hour period. During the monomer addition the temperature was maintained at 150° C. and 60 PSI. After Charges 2 and 3 were in the reactor, the reaction mixture was held for 2 hours. The reactor was than cooled to 25° C. GC analysis of the reaction mixture showed that all acrylates and styrene were reacted. The final solids of the resulting polymer was 83.12% determined at 110° C. for one hour. The copolymer had Mn=1400 and Mw/Mn=2.4. The 13C NMR spectrum was consistent with a molar copolymer composition of 22.1% diusobutylene, 35.0% hydroxypropyl acrylate, 15.6% isobornyl-acrylate, 7.8% styrene, and 19.5% butyl acrylate.

後処理

  1. additionCharge 1
  2. additionwas added to a 4-liter
  3. customwas adjusted to 150° C
  4. additionCharge 2
  5. additionwas added to the reactor at an addition rate of 36 grams/hour over a 2.5 hour period
  6. additionAfter 15 minutes Charge 3
  7. additionwas added to reactor at an addition rate of 1000 grams/hour over a 2 hour period
  8. additionDuring the monomer addition the temperature
  9. temperaturethan cooled to 25° C
  10. customwere reacted
  11. waitdetermined at 110° C. for one hour

出典と根拠

ORDレコード
ord-f79f904b4f1b486fa487f2652f896744
出典データセット
uspto-grants-2006_11
特許番号
US07132476B2

関連ノート

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