関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Acrylic Acid | HCID 6581 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Sodium Persulfate | HCID 62655 | — |
| 反応物 | gamma-Methyl-alpha-methylene-gamma-butyrolactone | HCID 99939 | — |
| 反応物 | Sodium Lauryl Sulfate | HCID 3423265 | — |
| 生成物 | alpha-Methylene-gamma-Valerolactone Acrylic Acid | HCID 86664974 | — |
反応手順
To a 50 mL round bottom flask equipped with a magnetic stir bar was added 7.3769 g (0.343 mol) water and 0.084 g (2.70×10−4 mol) sodium dodecyl sulfate. (20% aqueous solution). The mixture was heated under flowing nitrogen to 73° C., at which point a monomer mixture consisting of 3.4691 g (2.58×10−2 mol) α-methylene-γ-valerolactone and 0.184 g (2.56×10−3 mol) acrylic acid was added via syringe pump over 115 minutes. After 10 minutes of monomer mixture addition, an aqueous mixture consisting of 13.9194 g (0.649 mol) water, 0.2360 g (6.87×10−4 mol) sodium dodecyl sulfate (20% aqueous solution), 0.0201 g (1.68×10−5 mol) sodium persulfate, and 0.0376 g of a 20% aqueous sodium hydroxide solution was also added via syringe pump over 120 minutes. After both the monomer and aqueous mixtures were added completely, the emulsion was allowed to stir for an additional 60 minutes, after which the reaction was cooled to room temperature and dried under vacuum at 100° C. Analysis of the polymer by DSC showed a single Tg at 210° C. Size exclusion chromatography yielded a molecular weight of 931 kDa and a PDI of 2.00.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08846817B2 |
|---|
| 出典データセット | uspto-grants-2014_09 |
|---|
| ORD ID | ord-814aae88dde047788853e27ef440edc9 |
|---|
| 出典メモ | uspto-grants-2014_09 |
|---|