Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Isoprene | HCID 6557 | — |
| Reactant | Styrene | HCID 7501 | — |
| Reactant | N,N,N',N'-Tetramethylethylenediamine | HCID 8037 | — |
| Reactant | Butyllithium | HCID 178418339 | — |
| Solvent | Cyclohexane | HCID 8078 | — |
| Product | HCID 19842620 | HCID 19842620 | — |
Reaction Steps
To a pressure-resistant reactor, 23.3 kg of cyclohexane, 0.8 millimoles of TMEDA and 1.24 kg of styrene were added and stirred at 40° C. Added thereto was 14.1 millimoles of n-butyl lithium, and while the temperature was increased to 50° C., the mixture was polymerized for 1 hour. Next, 43.2 millimoles of n-butyl lithium was further added thereto, and 0.85 kg of isoprene was added thereto continuously over 30 minutes and the polymerization was performed for 1 hour. The degree of polymerization conversion of styrene was 100%. Subsequently, 7.05 kg of isoprene was added to the reactor continuously over 1 hour while the temperature was controlled to maintain 50 to 60° C. After the addition of isoprene was completed, the polymerization was performed for additional 1 hour. The degree of polymerization conversion of isoprene was 100%. Subsequently, 0.85 kg of styrene was added thereto continuously over 30 minutes. After the addition of styrene was completed, the polymerization was performed for additional 1 hour to produce two kinds of styrene-isoprene-styrene block copolymers, which are the block copolymer A and the block copolymer B. The degree of polymerization conversion of styrene was 100%. After that, 114.6 millimoles of methanol was added as a polymerization terminator and mixed well to terminate the reaction. Part of the reaction solution obtained was extracted and subjected to the same measurements as Preparation example 1. The values thereof are shown in Table 2. Subsequent treatments that were the same as those of Preparation example 1 were carried out to recover the block copolymer composition of Preparation example 4.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08578852B2 |
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| Source dataset | uspto-grants-2013_11 |
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| ORD ID | ord-5ff6a3b6fe934152be18b2586b03e574 |
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| Source note | uspto-grants-2013_11 |
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