Abstract
Oxidative polymerization of 2,6-dimethylphenol (2,6-DMP) is a convenient method to prepare poly (2,6-dimethyl-1,4-phenyleneoxide) (PPO), an important plastic in engineering. The polymerization of 2,6-DMP is carried out in organic solvents under oxygen; thus, a solvent-recovery system and an anti-explosive reactor are required for the industrial application. The use of scCO2 instead of organic solvents is expected to make the polymerization of 2,6-DMP safer and environmentally more benign. We have studied the oxidative polymerization of 2,6-DMP in scCO2. In this report, we have applied the 'double-step polymerization' method in scCO2 to synthesize PPO with better polymer properties, i.e., higher average molecular weight (Mw) and narrower molecular weight distribution (Mw/Mn). In the first step, a prepolymer with a narrow molecular weight distribution (Mw/Mn = 1.4) was synthesized under a homogeneous-phase condition. The prepolymer was purified and dried to remove water. In the second step, the prepolymer was further polymerized to increase the molecular weight. The second-step polymerization was performed at 40°C and 20 MPa. The Mw was increased from 4.9 × 103 to 9.0 × 103, keeping the narrow molecular weight distribution (Mw/Mn = 1.4). We further optimized the polymerization condition in the second step to obtain higher molecular weight. The Mw was increased to 3.4 × 104 (Mw/Mn = 2.3) at 80°C and 15 MPa in the presence of CuBr (0.0004 mol) and pyridine (0.019 mol).
| Original language | English |
|---|---|
| Pages (from-to) | 688-694 |
| Number of pages | 7 |
| Journal | Kobunshi Ronbunshu |
| Volume | 65 |
| Issue number | 11 |
| DOIs | |
| Publication status | Published - 2008 Nov |
| Externally published | Yes |
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Keywords
- Molecular weight distribution
- Oxidative polymerization
- Poly (phenylene oxide)
- Supercritical carbon dioxide
ASJC Scopus subject areas
- Polymers and Plastics
- Environmental Science(all)
- Materials Science (miscellaneous)
- Chemical Engineering (miscellaneous)
Cite this
Synthesis of poly (2,6-dimethyl-1,4-phenylene oxide) by double-step polymerization in supercritical carbon dioxide. / Murata, Hidenori; Sato, Takuro; Oyaizu, Kenichi; Furuya, Takeshi; Takebayashi, Yoshihiro; Yoda, Satoshi; Otake, Katsuto; Yuasa, Makoto.
In: Kobunshi Ronbunshu, Vol. 65, No. 11, 11.2008, p. 688-694.Research output: Contribution to journal › Article
}
TY - JOUR
T1 - Synthesis of poly (2,6-dimethyl-1,4-phenylene oxide) by double-step polymerization in supercritical carbon dioxide
AU - Murata, Hidenori
AU - Sato, Takuro
AU - Oyaizu, Kenichi
AU - Furuya, Takeshi
AU - Takebayashi, Yoshihiro
AU - Yoda, Satoshi
AU - Otake, Katsuto
AU - Yuasa, Makoto
PY - 2008/11
Y1 - 2008/11
N2 - Oxidative polymerization of 2,6-dimethylphenol (2,6-DMP) is a convenient method to prepare poly (2,6-dimethyl-1,4-phenyleneoxide) (PPO), an important plastic in engineering. The polymerization of 2,6-DMP is carried out in organic solvents under oxygen; thus, a solvent-recovery system and an anti-explosive reactor are required for the industrial application. The use of scCO2 instead of organic solvents is expected to make the polymerization of 2,6-DMP safer and environmentally more benign. We have studied the oxidative polymerization of 2,6-DMP in scCO2. In this report, we have applied the 'double-step polymerization' method in scCO2 to synthesize PPO with better polymer properties, i.e., higher average molecular weight (Mw) and narrower molecular weight distribution (Mw/Mn). In the first step, a prepolymer with a narrow molecular weight distribution (Mw/Mn = 1.4) was synthesized under a homogeneous-phase condition. The prepolymer was purified and dried to remove water. In the second step, the prepolymer was further polymerized to increase the molecular weight. The second-step polymerization was performed at 40°C and 20 MPa. The Mw was increased from 4.9 × 103 to 9.0 × 103, keeping the narrow molecular weight distribution (Mw/Mn = 1.4). We further optimized the polymerization condition in the second step to obtain higher molecular weight. The Mw was increased to 3.4 × 104 (Mw/Mn = 2.3) at 80°C and 15 MPa in the presence of CuBr (0.0004 mol) and pyridine (0.019 mol).
AB - Oxidative polymerization of 2,6-dimethylphenol (2,6-DMP) is a convenient method to prepare poly (2,6-dimethyl-1,4-phenyleneoxide) (PPO), an important plastic in engineering. The polymerization of 2,6-DMP is carried out in organic solvents under oxygen; thus, a solvent-recovery system and an anti-explosive reactor are required for the industrial application. The use of scCO2 instead of organic solvents is expected to make the polymerization of 2,6-DMP safer and environmentally more benign. We have studied the oxidative polymerization of 2,6-DMP in scCO2. In this report, we have applied the 'double-step polymerization' method in scCO2 to synthesize PPO with better polymer properties, i.e., higher average molecular weight (Mw) and narrower molecular weight distribution (Mw/Mn). In the first step, a prepolymer with a narrow molecular weight distribution (Mw/Mn = 1.4) was synthesized under a homogeneous-phase condition. The prepolymer was purified and dried to remove water. In the second step, the prepolymer was further polymerized to increase the molecular weight. The second-step polymerization was performed at 40°C and 20 MPa. The Mw was increased from 4.9 × 103 to 9.0 × 103, keeping the narrow molecular weight distribution (Mw/Mn = 1.4). We further optimized the polymerization condition in the second step to obtain higher molecular weight. The Mw was increased to 3.4 × 104 (Mw/Mn = 2.3) at 80°C and 15 MPa in the presence of CuBr (0.0004 mol) and pyridine (0.019 mol).
KW - Molecular weight distribution
KW - Oxidative polymerization
KW - Poly (phenylene oxide)
KW - Supercritical carbon dioxide
UR - http://www.scopus.com/inward/record.url?scp=57549106594&partnerID=8YFLogxK
UR - http://www.scopus.com/inward/citedby.url?scp=57549106594&partnerID=8YFLogxK
U2 - 10.1295/koron.65.688
DO - 10.1295/koron.65.688
M3 - Article
AN - SCOPUS:57549106594
VL - 65
SP - 688
EP - 694
JO - Kobunshi Ronbunshu
JF - Kobunshi Ronbunshu
SN - 0386-2186
IS - 11
ER -