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Isoprene → 2-Methylbuta-1,3-diene;styrene

HRID 718481
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HRID 718481 반응식
CN(CCN(C)C)C.[CH2:9]=[CH:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.C([Li])CCC.C=CC(=C)C>C1CCCCC1>[CH2:9]=[CH:10][C:11](=[CH2:12])[CH3:16].[CH2:9]=[CH:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1
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참가 물질

6

반응물 4

HCID 6557Isoprene2회HCID 7501Styrene2회HCID 8037N,N,N',N'-TetramethylethylenediamineHCID 178418339Butyllithium

생성물 1

HCID 1599892-Methylbuta-1,3-diene;styrene

시약·촉매·용매 1

HCID 8078Cyclohexane용매

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온도
40 °C

실험 절차

In a pressure-resistant reactor, 23.3 kg of cyclohexane, 2.6 millimoles of TMEDA, and 1.35 kg of styrene were introduced, and while the content was stirred at 40° C., 86 millimoles of n-butyllithium was added thereto. Polymerization was carried out for one hour while the temperature was increased to 50° C. The polymerization conversion ratio of styrene was 100%. Subsequently, 7.1 kg of isoprene was continuously added to the reactor over one hour while the temperature was controlled to be maintained at 50° C. to 60° C. After the addition of isoprene was completed, polymerization was carried out for another one hour, and thus a styrene-isoprene block copolymer was formed. The polymerization conversion ratio of isoprene was 100%. Thereafter, 172 millimoles of methanol as a polymerization terminator was added thereto and mixed thoroughly therein, and thus the reaction was terminated. Incidentally, the amounts of the various reagents used in the reaction are summarized in Table 1. The reaction liquid obtained as described above was treated in the same manner as in Production Example 1, and thus a composition of Production Example 6 (block copolymer) was collected. Furthermore, a portion of the reaction liquid thus obtained was taken, and the same measurements as in Production Example 1 were carried out. These measurement values are presented in Table 2.

후처리

  1. customPolymerization
  2. temperaturewas increased to 50° C
  3. temperatureto be maintained at 50° C. to 60° C
  4. custompolymerization
  5. waitwas carried out for another one hour

출처 및 근거

ORD 기록
ord-53ad9b1b51f0478a8bcee6985599dfc7
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09193893B2

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