基于超支化聚乙烯亚胺构筑新型功能高分子材料
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摘要
本论文以商品化的含有大量氨基基团的超支化聚乙烯亚胺(HPEI)为原料,制备了多种功能性高分子材料,分别用做可回收再利用的原子转移自由基聚合(ATRP)的大分子配体、染料吸附剂、小粒径金纳米粒子模板和大粒径金纳米粒子稳定剂等方面,具体内容如下:
1、大分子配体的制备及在ATRP中的应用
Fe_3O_4磁性纳米粒子表面通过HPEI修饰改性后,得到具有磁性的适用于ATRP的大分子配体MNP-HPEI,在甲基丙烯酸甲酯(MMA)的ATRP聚合反应中,MNP-HPEI与CuCl/CuBr2络合形成的催化体系能够较好地控制MMA聚合的反应速率、分子量和分散度,并且该催化体系通过磁场可以回收利用多次。
2、功能性多臂星状聚合物的制备、表征及应用在以改性HPEI为大分子引发剂的甲基丙烯酸羟乙酯(HEMA)的ATRP聚合反应中,通过聚合反应条件的优化,制备出了一系列可控性好的以HPEI为核、聚甲基丙烯酸羟乙酯(PHEMA)为臂的功能性多臂星状聚合物HPEI-b-PHEMA。HPEI-b-PHEMA能够以固体颗粒的形式吸附水溶液的阴离子染料甲基橙和刚果红,吸附能力与HPEI核的大小、PHEMA臂的长短及臂数都有着紧密的联系。此外,以HPEI-b-PHEMA为模板,可以制备出稳定的、粒径在2-10nm之间可调的小粒径金纳米粒子(AuNP),通过对比实验证明,具有多氨基的HPEI核和含有大量羟基的PHEMA壳的同时存在,对AuNP的粒径控制及稳定性是非常重要的。
3、两亲性超支化聚合物在稳定大粒径AuNP方面的应用棕榈酸改性HPEI后得到具有核壳结构的两亲性HPEI-C16超支化聚合物,其中,只有高取代度的HPEI-C16能够有效地将直径约为18nm的AuNP从水相转移至氯仿相。与棕榈酸改性的线形聚乙烯亚胺(LPEI-C16)相比,相转移AuNP所需HPEI-C16聚合物的量更少,并且稳定性更好。HPEI-C16和LPEI-C16稳定的AuNP都能异相催化NaBH4还原4-硝基酚,HPEI-C16稳定的AuNP催化速率慢于LPEI-C16稳定的AuNP,但其重复催化次数远高于LPEI-C16稳定的AuNP。
In this dissertation, the commercially available hyperbranched polyethylenimine (HPEI) polymers having a large number of amino groups were used as the main raw materials to prepare several kinds of functional polymeric materials,such as recoverable and reusable macroligands suitable for atom transfer radical polymerization (ATRP), solid sorbent for dyes, template for small-diametered gold nanoparticles (AuNP) and stabilizers for large-diametered AuNP The detail was as follows:
1. Preparation of macroligands and their application in ATRP
Magnetic macroligand MNP-HPEI for ATRP was prepared through the surface modification of Fe3O4 magnetic nanoparticle with HPEI In the ATRP of methyl methacrylate (MMA), the catalytic system based on the complex of MNP-HPEI with CuCl/CuBr_2 could control the polymerization rate of MMA, molecular weight and polydispersity in good mode Furthermore, the catalytic systemcould be recovered and reused several times through magnetic field
2 Preparation, characterization and application of functional multiarm star polymers
Macroinitiators derived from HPEI were used to initiate the ATRP of 2-hydroxylethyl methacrylate (HEMA), resulting in functional multiarm star polymerwith HPEI as core and poly(2-hydroxylethyl methacrylate) (PHEMA) as arms After optimization of the polymerization condition, a series of HPEI-b-PHEMAmultiarm star polymers with controlled molecular weight and relatively narrow polydispersity could be obtained HPEI-b-PHEMA polymers in the solid state could adsorb the anionic Methyl Orange and Congo Red dyes from water The adsoption capacities were related closely with the size of HPEI core, the length and number of PHEMA arms Moreover, stable small AuNPs with diameter in the range of 2-10nm could be prepared with HPEI-b-PHEMA as template Compared with the control experiments, it could be concluded that the integration of the plenty of amino groups of HPEI core and the hydroxyl groups of PHEMA arms was the key to control the size of AuNPs and stabilize the AuNPs for long time
3 The application of amphiphilic hyperbranched polymers in stabilizing large AuNPs
Core-shell type amphiphilic hyperbranched HPEI-C16 polymers were prepared through the modification of HPEI with palmitic acid Among these HPEI-C16 polymers, only those with high degree of substitution could effectively transfer 18nm diametered AuNPs from water into chloroform phase Compared with the linear polyethylenimine modified with plamitic acid (LPEI-C16), less HPEI-C16 polymers were required for the completely extraction of AuNPs from water into chloroform phase Moreover, the AuNPs stabilized by HPEI-C16 polymers in chloroform were more stable AuNPs stabilized by both HPEI-C16 and LPEI-C16 could heterogeneously catalyze the NaBH4 reduction of 4-nitrophenol The catalytic rate of AuNPs stabilized by HPEI-C16 polymers was slower than that of AuNPs stabilized by LPEI-C16 polymers;however, the AuNPs stabilized by HPEI-C16 polymers could be recycled more times
1、大分子配体的制备及在ATRP中的应用
Fe_3O_4磁性纳米粒子表面通过HPEI修饰改性后,得到具有磁性的适用于ATRP的大分子配体MNP-HPEI,在甲基丙烯酸甲酯(MMA)的ATRP聚合反应中,MNP-HPEI与CuCl/CuBr2络合形成的催化体系能够较好地控制MMA聚合的反应速率、分子量和分散度,并且该催化体系通过磁场可以回收利用多次。
2、功能性多臂星状聚合物的制备、表征及应用在以改性HPEI为大分子引发剂的甲基丙烯酸羟乙酯(HEMA)的ATRP聚合反应中,通过聚合反应条件的优化,制备出了一系列可控性好的以HPEI为核、聚甲基丙烯酸羟乙酯(PHEMA)为臂的功能性多臂星状聚合物HPEI-b-PHEMA。HPEI-b-PHEMA能够以固体颗粒的形式吸附水溶液的阴离子染料甲基橙和刚果红,吸附能力与HPEI核的大小、PHEMA臂的长短及臂数都有着紧密的联系。此外,以HPEI-b-PHEMA为模板,可以制备出稳定的、粒径在2-10nm之间可调的小粒径金纳米粒子(AuNP),通过对比实验证明,具有多氨基的HPEI核和含有大量羟基的PHEMA壳的同时存在,对AuNP的粒径控制及稳定性是非常重要的。
3、两亲性超支化聚合物在稳定大粒径AuNP方面的应用棕榈酸改性HPEI后得到具有核壳结构的两亲性HPEI-C16超支化聚合物,其中,只有高取代度的HPEI-C16能够有效地将直径约为18nm的AuNP从水相转移至氯仿相。与棕榈酸改性的线形聚乙烯亚胺(LPEI-C16)相比,相转移AuNP所需HPEI-C16聚合物的量更少,并且稳定性更好。HPEI-C16和LPEI-C16稳定的AuNP都能异相催化NaBH4还原4-硝基酚,HPEI-C16稳定的AuNP催化速率慢于LPEI-C16稳定的AuNP,但其重复催化次数远高于LPEI-C16稳定的AuNP。
In this dissertation, the commercially available hyperbranched polyethylenimine (HPEI) polymers having a large number of amino groups were used as the main raw materials to prepare several kinds of functional polymeric materials,such as recoverable and reusable macroligands suitable for atom transfer radical polymerization (ATRP), solid sorbent for dyes, template for small-diametered gold nanoparticles (AuNP) and stabilizers for large-diametered AuNP The detail was as follows:
1. Preparation of macroligands and their application in ATRP
Magnetic macroligand MNP-HPEI for ATRP was prepared through the surface modification of Fe3O4 magnetic nanoparticle with HPEI In the ATRP of methyl methacrylate (MMA), the catalytic system based on the complex of MNP-HPEI with CuCl/CuBr_2 could control the polymerization rate of MMA, molecular weight and polydispersity in good mode Furthermore, the catalytic systemcould be recovered and reused several times through magnetic field
2 Preparation, characterization and application of functional multiarm star polymers
Macroinitiators derived from HPEI were used to initiate the ATRP of 2-hydroxylethyl methacrylate (HEMA), resulting in functional multiarm star polymerwith HPEI as core and poly(2-hydroxylethyl methacrylate) (PHEMA) as arms After optimization of the polymerization condition, a series of HPEI-b-PHEMAmultiarm star polymers with controlled molecular weight and relatively narrow polydispersity could be obtained HPEI-b-PHEMA polymers in the solid state could adsorb the anionic Methyl Orange and Congo Red dyes from water The adsoption capacities were related closely with the size of HPEI core, the length and number of PHEMA arms Moreover, stable small AuNPs with diameter in the range of 2-10nm could be prepared with HPEI-b-PHEMA as template Compared with the control experiments, it could be concluded that the integration of the plenty of amino groups of HPEI core and the hydroxyl groups of PHEMA arms was the key to control the size of AuNPs and stabilize the AuNPs for long time
3 The application of amphiphilic hyperbranched polymers in stabilizing large AuNPs
Core-shell type amphiphilic hyperbranched HPEI-C16 polymers were prepared through the modification of HPEI with palmitic acid Among these HPEI-C16 polymers, only those with high degree of substitution could effectively transfer 18nm diametered AuNPs from water into chloroform phase Compared with the linear polyethylenimine modified with plamitic acid (LPEI-C16), less HPEI-C16 polymers were required for the completely extraction of AuNPs from water into chloroform phase Moreover, the AuNPs stabilized by HPEI-C16 polymers in chloroform were more stable AuNPs stabilized by both HPEI-C16 and LPEI-C16 could heterogeneously catalyze the NaBH4 reduction of 4-nitrophenol The catalytic rate of AuNPs stabilized by HPEI-C16 polymers was slower than that of AuNPs stabilized by LPEI-C16 polymers;however, the AuNPs stabilized by HPEI-C16 polymers could be recycled more times
引文
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