Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Isoprene | HCID 6557 | — |
| Reactant | Styrene | HCID 7501 | — |
| Reactant | N,N,N',N'-Tetramethylethylenediamine | HCID 8037 | — |
| Reactant | Tetramethoxysilane | HCID 12682 | — |
| 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, 3.26 millimoles of TMEDA, and 3.70 kg of styrene were added, and while the mixture was stirred at 40° C., 217.4 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., 6.3 C kg of isoprene was continuously added to the reactor over one hour. After completion of the addition of isoprene, polymerization was carried out for another one hour. The polymerization conversion ratio for isoprene was 100%. Subsequently, 18.5 millimoles of tetramethoxysilane was added to the reactor as a coupling agent, and a coupling reaction was carried out for 2 hours. Thus, a branched styrene-isoprene-styrene block copolymer was formed. Thereafter, 434.8 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 the same analyses as in Production Example 6 were carried out. These values are presented in Table 5. The subsequent operation was carried out in the same manner as in Production Example 6, and a block copolymer composition of Comparative Production Example 8 was collected.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08501869B2 |
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| Source dataset | uspto-grants-2013_08 |
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| ORD ID | ord-a8c1d8ad5ba340f59a9bc0139b9aba87 |
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| Source note | uspto-grants-2013_08 |
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