Mesoporous poly(styrene-co-maleic anhydride)/silica hybrid materials have been prepared. The synthesis was achieved by the HCl-catalyzed sol-gel reactions of tetraethyl orthosilicate (TEOS) and styrene-maleic anhydrid...Mesoporous poly(styrene-co-maleic anhydride)/silica hybrid materials have been prepared. The synthesis was achieved by the HCl-catalyzed sol-gel reactions of tetraethyl orthosilicate (TEOS) and styrene-maleic anhydride copolymer in the presence of 3-aminopropyl triethoxysilane (APTES) as a coupling agent and citric acid as a nonsurfactant template or pore-forming agent, followed by ethanol extraction. Characterization results from nitrogen sorption isotherms and powder X-ray diffraction indicate that polymer-modified mesoporous materials with large specific surface areas (e.g. 900 m(2)/g) and pore volumes (e.g. 0.6 cm(3)/g) could be prepared. As the citric acid concentration is increased, the specific surface areas, pore volumes and pore diameters of the hybrid materials increase.展开更多
Supercritical carbon dioxide （scCO2） was used as a reaction medium in synthesizing amphiphilic graft copolymers composed of poly（styrene-co-maleic anhydride） （SMA） backbones and methoxyl poly（ethylene glycol） ...Supercritical carbon dioxide （scCO2） was used as a reaction medium in synthesizing amphiphilic graft copolymers composed of poly（styrene-co-maleic anhydride） （SMA） backbones and methoxyl poly（ethylene glycol） （MPEG） side chains via esterification. The synthesized copolymers were characterized by Fourier transform infrared spectroscopy （FTIR）, gel permeation chromatography （GPC）, IH-NMR, thermo-gravimetric analysis （TGA） and differential scanning calorimetric analysis （DSC）. The gelation phenomenon was suppressed effectively by tuning reaction conditions. The influences of scCO2 temperature and pressure on the conversion of anhydride were investigated. It was found that the highest conversion ratio occurred at 80~C under a constant pressure of 14 MPa or 26 MPa. With the increase of scCO2 pressure, the conversion ratio increased first, and then leveled off. The conversion ratio of anhydride could be controlled by regulating the reaction conditions. It was also revealed that using low molecular weight MPEG brought a high conversion ratio of anhydride.展开更多
The comblike polymers based on poly (styrene-co-maleic anhydride) backbone with poly (ethylene glycol) methyl ether as side chains were synthesized and characterized by H-1 NMR. with the result compared with that of 1...The comblike polymers based on poly (styrene-co-maleic anhydride) backbone with poly (ethylene glycol) methyl ether as side chains were synthesized and characterized by H-1 NMR. with the result compared with that of 1R. It is found that it is both feasible and simple to synthesize this kind of compounds with the help of H-1 NMR.展开更多
本文以丁二酸、丁二酸酐和1,4-丁二醇为原料,以自制的微孔钛硅分子筛为聚合催化剂,制备了高相对分子质量的聚丁二酸丁二醇酯。考察了原料物质的量比、酯化时间、酯化温度对酯化反应的影响,以及缩聚时间、缩聚温度、分子筛种类和用量对...本文以丁二酸、丁二酸酐和1,4-丁二醇为原料,以自制的微孔钛硅分子筛为聚合催化剂,制备了高相对分子质量的聚丁二酸丁二醇酯。考察了原料物质的量比、酯化时间、酯化温度对酯化反应的影响,以及缩聚时间、缩聚温度、分子筛种类和用量对聚丁二酸丁二醇酯性能的影响。结果表明,当丁二酸、丁二酸酐和丁二醇的物质的量比为0.5:0.5:1.3,酯化温度为150℃,反应2.5 h酯化率达到95.2%;当以制备的钛硅分子筛为缩聚催化剂,其用量为酯化产物总质量的1%,缩聚温度为220℃,反应3 h,产物聚丁二酸丁二醇酯的特性粘度可以达到2.0 d L/g,相对分子质量可以达到12.9万g/mol以上。展开更多
基金Project supported by the National Natural Science Foundation of China (No. 29874002) and the Outstanding Young Scientist Award from National Natural Science Foundation of China (No. 29825504)
文摘Mesoporous poly(styrene-co-maleic anhydride)/silica hybrid materials have been prepared. The synthesis was achieved by the HCl-catalyzed sol-gel reactions of tetraethyl orthosilicate (TEOS) and styrene-maleic anhydride copolymer in the presence of 3-aminopropyl triethoxysilane (APTES) as a coupling agent and citric acid as a nonsurfactant template or pore-forming agent, followed by ethanol extraction. Characterization results from nitrogen sorption isotherms and powder X-ray diffraction indicate that polymer-modified mesoporous materials with large specific surface areas (e.g. 900 m(2)/g) and pore volumes (e.g. 0.6 cm(3)/g) could be prepared. As the citric acid concentration is increased, the specific surface areas, pore volumes and pore diameters of the hybrid materials increase.
基金financially supported by the 973 Program of China(No.2009CB623402)the Fundamental Research Funds for the Central Universities(MOE Engineering Research Center of Membrane and Water Treatment Technology, Grant no.KYJD09011)+1 种基金the 863 Program of China(No.2009AA062902)Zhejiang Provincial Sci & Tech Plan of China(No.2010C31028)
文摘Supercritical carbon dioxide （scCO2） was used as a reaction medium in synthesizing amphiphilic graft copolymers composed of poly（styrene-co-maleic anhydride） （SMA） backbones and methoxyl poly（ethylene glycol） （MPEG） side chains via esterification. The synthesized copolymers were characterized by Fourier transform infrared spectroscopy （FTIR）, gel permeation chromatography （GPC）, IH-NMR, thermo-gravimetric analysis （TGA） and differential scanning calorimetric analysis （DSC）. The gelation phenomenon was suppressed effectively by tuning reaction conditions. The influences of scCO2 temperature and pressure on the conversion of anhydride were investigated. It was found that the highest conversion ratio occurred at 80~C under a constant pressure of 14 MPa or 26 MPa. With the increase of scCO2 pressure, the conversion ratio increased first, and then leveled off. The conversion ratio of anhydride could be controlled by regulating the reaction conditions. It was also revealed that using low molecular weight MPEG brought a high conversion ratio of anhydride.
文摘The comblike polymers based on poly (styrene-co-maleic anhydride) backbone with poly (ethylene glycol) methyl ether as side chains were synthesized and characterized by H-1 NMR. with the result compared with that of 1R. It is found that it is both feasible and simple to synthesize this kind of compounds with the help of H-1 NMR.
文摘本文以丁二酸、丁二酸酐和1,4-丁二醇为原料,以自制的微孔钛硅分子筛为聚合催化剂,制备了高相对分子质量的聚丁二酸丁二醇酯。考察了原料物质的量比、酯化时间、酯化温度对酯化反应的影响,以及缩聚时间、缩聚温度、分子筛种类和用量对聚丁二酸丁二醇酯性能的影响。结果表明,当丁二酸、丁二酸酐和丁二醇的物质的量比为0.5:0.5:1.3,酯化温度为150℃,反应2.5 h酯化率达到95.2%;当以制备的钛硅分子筛为缩聚催化剂,其用量为酯化产物总质量的1%,缩聚温度为220℃,反应3 h,产物聚丁二酸丁二醇酯的特性粘度可以达到2.0 d L/g,相对分子质量可以达到12.9万g/mol以上。
