Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Isoprene | HCID 6557 | — |
| Reactant | Styrene | HCID 7501 | — |
| Reactant | N,N,N',N'-Tetramethylethylenediamine | HCID 8037 | — |
| Reactant | 2-Methylbuta-1,3-diene;styrene | HCID 159989 | — |
| Reactant | Butyllithium | HCID 178418339 | — |
| Solvent | Cyclohexane | HCID 8078 | — |
| Product | HCID 19842620 | HCID 19842620 | — |
Reaction Steps
In a pressure resistant reactor, 23.3 kg of cyclohexane, 2.57 millimoles of TMEDA, and 1.10 kg of styrene were added, and while the mixture was stirred at 40° C., 85.7 millimoles of n-butyllithium was added thereto. While the temperature was elevated to 50° C., polymerization was carried out for one hour. The polymerization conversion ratio for styrene was 100%. Subsequently, while the temperature was controlled to be maintained at 50° C. to 60° C., 7.00 kg of isoprene was continuously added to the reactor for one hour. After completion of the addition of isoprene, polymerization was carried out for another one hour. Subsequently, 60.0 millimoles of methanol was added to the reactor as a polymerization terminator, and a polymerization termination reaction was carried out for one hour. The active terminal of a portion of the styrene-isoprene block copolymer having an active terminal was deactivated, and thereby a styrene-isoprene diblock copolymer which would serve as the polymer C (block copolymer C1) was formed. Thereafter, while the temperature was controlled to be maintained at 50° C. to 60° C., 1.90 kg of styrene was continuously added to the reactor for one hour. After completion of the addition of styrene, polymerization was carried out for another one hour, and thus a styrene-isoprene-styrene block copolymer was formed. The polymerization conversion ratio for styrene was 100%. Subsequently, 171.4 millimoles of methanol was added to the system as a polymerization terminator, the resulting mixture was thoroughly mixed, and the reaction was terminated. A portion of the reaction liquid thus obtained was taken out and was subjected to the same analyses as in Reference Example 1. These values are presented in Table 2. The subsequent operation was carried out in the same manner as in Reference Example 1, and a composition of Reference Example 10 was collected.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08791196B2 |
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| Source dataset | uspto-grants-2014_07 |
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| ORD ID | ord-9072c5d4a5a64b1895087937c64ddf78 |
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| Source note | uspto-grants-2014_07 |
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