関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Styrene | HCID 7501 | — |
| 反応物 | Methylcyclohexane | HCID 7962 | — |
| 反応物 | Isobutylene | HCID 8255 | — |
| 反応物 | (1-Chloro-1-methylethyl)benzene | HCID 70281 | — |
| 触媒 | Titanium Tetrachloride | HCID 24193 | — |
| 溶媒 | Butyl Chloride | HCID 8005 | — |
| 生成物 | Isobutylene styrene | HCID 44154101 | — |
反応手順
In a 2 L reaction vessel equipped with a stirrer, 589 mL of methylcyclohexane (dried over molecular sieves), 613 mL of n-butyl chloride (dried over molecular sieves) and 0.550 g of cumyl chloride were added. After cooling the reaction vessel to −70° C., 0.35 mL of α-picoline(2-methylpyridine) and 179 mL of isobutylene were added. Furthermore, 9.4 mL of titanium tetrachloride was added and the polymerization was initiated, and then the solution was reacted for 2.0 hours while stirring at −70° C. Next, 59 mL of styrene was added to the reaction vessel and the reaction was continued for 60 minutes, and then the reaction was terminated by adding a large amount of methanol. After removing the solvent from the reaction solution, a polymer was dissolved in toluene and washed twice with water. This toluene solution was added to the methanol mixture, thereby precipitating a polymer, and the resultant polymer was dried at 60° C. for 24 hours to obtain a styrene-isobutylene diblock copolymer.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08835557B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-8e81e160058e42609982d2effd7110fc |
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| 出典メモ | uspto-grants-2014_09 |
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