WANG Shuhui, YAN Hongxia, MA Xiaoyan, HUANG Yun, ZHANG Qilu. SYNTHESIS, STRUCTURE AND PROPERTIES OF COMB-LIKE COPOLYMER P(MMA-co-MAh)-g-PEGME. [J]. Acta Polymerica Sinica (9):880-886(2008)
DOI:
WANG Shuhui, YAN Hongxia, MA Xiaoyan, HUANG Yun, ZHANG Qilu. SYNTHESIS, STRUCTURE AND PROPERTIES OF COMB-LIKE COPOLYMER P(MMA-co-MAh)-g-PEGME. [J]. Acta Polymerica Sinica (9):880-886(2008) DOI: 10.3724/SP.J.1105.2008.00880.
SYNTHESIS, STRUCTURE AND PROPERTIES OF COMB-LIKE COPOLYMER P(MMA-co-MAh)-g-PEGME
In order to improve the ionic conductivity of the poly(methyl methacrylate-co-maleic anhydride)(P(MMA-co-MAh))-based gel polymer electrolytes
the poly(ethylene glycol)methyl ether chains were introduced in the side of P(MMA-co-MAh)binary copolymer to prepare comb-like poly(methyl methacrylate-co-maleic anhydride)-g-poly((ethylene glycol)methyl ether)(P(MMA-co-MAh)-g-PEGME)copolymer.The comb-like copolymer P(MMA-co-MAh)-g-PEGME was synthesized through two esterification reactions.The esterification of P(MMA-co-MAh)with PEGME at first in butanone
then injecting a definite volume of p-toluenesulfonic acid into the reaction mixture under a flow of nitrogen.The mixture was stirred continuously for 24 h at 80℃.After the reaction was complete
solvent in the mixture was then removed.An excess amount of methyl alcohol and definite volume of dimethyl sulphate were added to the residue so as to thoroughly endcap the unreacted carboxyl groups.The reaction proceeded with continuous stirring for another 24 h at 60℃.The methyl alcohol in the reaction mixture was then removed.The crude product was purified by butanone/toluene reprecipitation
and dried at room temperature.Further more
the product must be purified three times using petroleum ether and deionized waters at 80℃ to get the purified product.The purified product was dried in a vacuum oven to remove the trapped solvent at 40℃ for 24 h.The final product is white power.The structure of the comblike copolymer was characterized by Fourier transform infrared spectroscopy (FTIR)
which showed that the characteristic absorption of CO in anhydride at 1851 cm-1 and 1786 cm-1 disappeared
and the absorption of a saturated cyclic five-member anhydride(OC—O—CO)also disappeared.While a strong characteristic absorption of an ether group at 1152 cm-1 is shown.This is an evidence that appreciable amount of the anhydride has been esterified and the product is an ester of poly(ethylene glycol)mono.The structure of P(MMA-co-MAh)-g-PEGME polymer was further examined by 13C-NMR
1H-NMR and H
C-COSP spectra.The FTIR and NMR spectra indicated that the comb-like P(MMA-co-MAh)-g-PEGME copolymer was successful synthesized.The thermal properties of P(MMA-co-MAh)-g-PEGME were studied by thermogravimetric analysis (TGA)and differential scanning calorimetry (DSC).The TGA indicated that the thermal stability of P(MMA-co-MAh)-g-PEGME polymer was littler lower than that of P(MMA-co-MAh)copolymer.The decomposition temperature of the comblike polymer P(MMA-co-MAh)-g-PEGME is 325.9℃.The thermal stability of comb-like P(MMA-co-MAh)-g-PEGME copolymer and the P(MMA-co-MAh)copolymer are both better than that of the pure PMMA polymer.The DSC curves showed that the comb like polymer P(MMA-co-MAh)-g-PEGME had two glass transition temperatures(Tg)
the one glass transition of the main-chains
which was at around 120℃
and the other was about 32℃
which can be considered as the glass transition of the sidechains.The sidechains can move at room temperature
which will help to transfer and expand the electro active material.
SYNTHESIS AND SELF-ASSEMBLY OF POLY(N-ISOPROPYLACRYLAMIDE)-b-POLY(ε-BENZYLOXYCARBONYL-L-LYSINE)-b-POLY(ETHYLENE GLYCOL)
The Synthesis of a MMA/MAh Copolymer and Properties of the CopolymerBased Gel Polymer Electrolytes
SYNTHESIS OF WATER_SOLUBLE,COMB_LIKE POLY(ACRYLIC ACID)-g-POLY[(ETHYLENE GLYCOL)METHYL ETHER] COPOLYMERS AND THE CRYSTALLIZATION BEHAVIOR OF PEG SIDE CHAINS
SYNTHESIS OF AMPHIPHILIC DIBLOCK COPOLYMERS MPEG-b-Phe AND THEIR SELF-ASSEMBLY IN WATER