嵌段、星形及超支化聚合物的合成与性能
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摘要
嵌段共聚物具有特殊的物理化学特性,作为热塑性弹性体、表面活性剂、表面修饰剂、分散剂和聚合物共混的增溶剂等有着广泛的应用前景,已受到了学术界和工业界的广泛关注。活性自由基聚合技术的发展,为嵌段聚合物的合成提供了更多的手段,很多新型的结构规整、分子量和分子量分布可控的嵌段聚合物不断被人们合成出来。
嵌段共聚物在选择性溶剂中自组装可以形成高分子胶束。聚合物胶束在药物缓释、分离、催化和纳米材料方面具有潜在的应用前景,引起人们的浓厚兴趣。通过物理包埋、静电作用或化学键联等方法,将不溶性药物与聚合物胶束相结合,可以增加药物的溶解性,延长药物的体内循环时间,控制药物定时定点释放,在医药学领域得到了广泛的应用。在化学键联法中,要求用于连接载药胶束与药物的化学键具有环境响应特性,目前可以选择的这类化学键还十分有限,这一领域还有待更多的研究。
聚合物胶束的聚集形态与其应用密切相关,目前除常见的球形胶束外,已经可以得到棒状、层状、碗形、管状、囊泡及其他多种具有复杂的复合结构的胶束。通过改变嵌段聚合物的自组装条件,控制形成的聚合物胶束的形态已有很多报道,但目前的研究工作大多集中在亲溶剂段较短的嵌段聚合物自组装形成的平头胶束上,研究星形胶束的形态多样性的报道还很少。
近年来在常规制备聚合物胶束的方法的基础上,出现了许多利用聚合物的特殊性质或聚合物分子间的特殊相互作用,实现高分子胶束化的新方法。两种含有相同嵌段长度并带有相反电荷的聚电解质链段的两亲性聚合物,通过静电相互作用,共同自组装形成复合胶束据我们所知还没有报道过。
星形聚合物是一类具有简单支化结构和特殊性能的聚合物,无论采用先臂后核还是先核后臂的路径合成星形聚合物,核或臂都要通过一个单独的步骤预先合成,或者需要分多步投入反应原料,这给工业规模的制备带来不便。一步法合成星形聚合物使核的形成与臂的生长能通过“一锅”反应来实现,不需要中间产物的分离与纯化,也不需要分两步加入反应原料,可以使星形聚合物的合成更为简单、有效。
静电纺丝技术是目前大规模制备纳米纤维最合适的方法,近几年来已经用于几十种不同的聚合物,并且通过溶胶-凝胶法配制溶液,适用范围已经扩大到无机物领域。但目前人们研究所用的聚合物还仅限于均聚物、共混聚合物和嵌段聚合物等,因而对具有特殊性能的超支化聚合物的静电纺丝的研究是一项很有意义的工作。
据此,本文的主要工作和取得的研究成果摘要如下:
1)以单端带有C-Br键的聚环氧乙烷(PEO-Br)作为大分子引发剂,引发丙烯酸缩酮甘油酯(SA)的ATRP,合成了PEO-b-PSA的嵌段聚合物,研究了这一聚合反应的活性特征,进一步通过脱去缩酮保护基将聚丙烯酸缩酮甘油酯嵌段(PSA)转化为聚丙烯酸甘油酯嵌段(PGA)。以具有荧光特性的1-醛基芘(Pyrene-CHO)做为药物模型,通过与PGA上邻-二羟基的缩合反应连到嵌段聚合物PEO-b-PGA的PGA上,所得的聚合物在选择性溶剂中自组装,形成以疏水的PGA-Py为核,亲水的PEO为壳的聚合物胶束。用荧光跟踪研究了芘在不同pH值(1.0,5.0和7.4)缓冲溶液中,从聚合物胶束中的释放动力学。研究结果表明,双亲水性嵌段聚合物PEO-b-PGA,可与含有羰基的药物,通过缩酮键连接并自组装形成酸敏感性载药胶束,在药物缓释领域具有潜在的应用前景。
2)用PEO-Br作为大分子引发剂,以ATRP法合成了环氧乙烷和甲基丙烯酸对硝基苯酚酯的嵌段共聚物(PEO-b-PNPMA),研究了聚合物PEO_(113)-b-PNPMA_(28)在选择不同的共溶剂(四氢呋喃、二甲亚砜和硝基甲烷)和选择性溶剂(甲醇、乙醇和水)时的稀溶液自组装行为,通过TEM观察到具有球形、棒状、囊泡、花椰菜形、双连续棒状等不同形态的星形聚集体。测试了所用的不同溶剂的临界选择性溶剂含量和PNPMA富集相溶剂含量,具有乙醇＞甲醇＞水,四氢呋喃＞硝基甲烷＞二甲亚砜的相对大小顺序。以此为基础讨论了这些不同形态的聚集体可能的形成机理。研究结果表明,采用改变共溶剂或选择性溶剂的方法,可以很方便地使成壳链段相对较长的两亲性嵌段聚合物形成的星形胶束,如平头胶束一样呈现多样的形态。
3)以对二溴苄(DBX)引发苯乙烯和甲基丙烯酸对硝基苯酚酯(NPMA)相继进行ATRP,合成了三嵌段聚合物PNPMA-b-PS-b-PNPMA。利用PNPMA嵌段易于水解和被氨基取代的特点,以相同PNPMA链长的三嵌段共聚物分别进行水解反应及与2-氨基吡啶的取代反应,制备了具有相反电荷的阴离子型PMAA-b-PS-b-PMAA和阳离子型PNPMAAm-b-PS-b-PNPMAAm两种三嵌段共聚物。将这两种三嵌段共聚物以等摩尔比混合,在水中自组装形成了碗形的聚集体结构,讨论了这种结构可能的形成机理。这些由聚电解质复合物自组装形成的聚集体,在微反应器和药物释放等领域具有潜在的应用前景。
4)合成了双乙烯基的2,7-二亚甲基-1,4,6-三氧杂螺环烷,作为给电子单体和交联剂,与吸电子单体马来酸酐(MAh)或过量的丙烯酸甲酯(MA)形成电荷转移络合物(CTC)共同聚合,尝试了用ATRP和RAFT方法一步法合成星形聚合物。在ATRP共聚合中,由于螺环交联剂与MA不能有效组成CTC,因而不能优先聚合而成核,它们的共聚合反应主要产生均聚物。在RFAT共聚合中,在S-1-十二烷基-S'-(α,α'-甲基-α”-乙酸)三硫代碳酸酯链转移剂存在下,摩尔比2:1的MAh和螺环交联剂,与过量MA进行共聚合成了星形聚合物。对聚合反应初期反应混合物的核磁共振氢谱跟踪结果证实了我们假定的聚合机理,即MAh与螺环交联剂形成CTC,并优先聚合形成了交联的带有多个转移基团的核,继而引发MA单体均聚形成了星形聚合物。可以预见,这种方法还可以方便地扩展到其他单体的聚合上,因而我们找到了一条比较简单的一步法合成星形聚合物的路线。
5)通过三元胺单体2-氨基乙基哌嗪(AEPZ)和等摩尔的二乙烯基单体胱胺双丙烯酰胺(CBA)进行迈克尔加成反应,获得了主链上含有三级胺、端基为一级胺的超支化聚(酰胺-胺)。对超支化聚(酰胺-胺)的甲醇溶液进行静电纺丝可制备聚合物纤维,研究了聚合物溶液浓度、外加电压和接收距离对电纺纤维的形态的影响。在荧光显微镜下观察,这种聚合物纤维可在不同波长的激发光作用下发出蓝色、绿色和红色的荧光。这种可以光致发光的聚合物纤维在显示领域有着潜在的应用前景。
Recently, block copolymers have attracted considerable attention because of their unique behaviors and potential applications, such as thermoplastics, surfactants, modifiers, dispersants, and tackifier etc. With the development of living radical polymerizations, such as SFRP, ATRP, RAFT and Iniferter, a large number of novel well-defined block copolymers with controlled molecular weights and narrow molecular weight distributions were prepared.
Polymer micelles, formed by self-assembly of block copolymers in selective solvent, have been extensively investigated for their potential applications in drug delivery, separation, catalysis and nanomaterials fields. For example, Hydrophobic drugs loaded by polymer micelles with physically entrapment or chemically conjugation are improved their water solubility and bioavailability. The drug-loaded micelles prolong their circulation in body and release selectively their payload in tumor tissue or within cells. However, the "smart" stimuli-responsive linkages, which are used to link drug and micelle in chemically conjugation method, are still limited.
The applications of polymer micelles are related to their morphologies. Beside frequently observed spherical core-shell micelles, Many other morphologies have been obtained, such as rod, worm-like, vesicle, lamellae and other complicated aggregates. These morphologies were usually prepared from crew-cut micelles by controlling the preparation conditions until now. There are few reports on the multiple morphologies of star micelles.
Polyion complex micelle, a novel micelle with its unique behaviors, is formed by a pair of opposite charged polymers in aqueous solution. The charged polymers used are usually homo-polyelectrolytes and double hydrophilic block copolymers consist of a polyelectrolyte block and a nonionic hydrophilic block such as PEO. The self-assemly of the mixture, which is composed of a pair of amphiphilic block copolymers with opposite charge and equal length, has not been researched.
Star polymer is a class of simplest branched polymer, which is usually prepared by "arm-first" and "core first" approach. No matter which approach is used in the literature, two steps are needed to get a star polymer. Either the core or the arms should be synthesized in a separate step; at least chemicals were added step by step. Therefore, a simple way of synthesis is highly appreciated.
Electrospinning is a very suitable method to obtained nanofibers. Many kinds of polymers, such as homopolymers, block copolymers and polymer blends, had been used to prepare nanofibers by electrospinning. In addition, inorganic nanofibers were fabricated by this method in recent years. The research of electrospinning of functional hyperbranched polymer is still an outgoing challenge.
All these facts are the origin and impetus of this thesis. The main results obtained in this thesis are as follows:
1) A new type of double hydrophilic block copolymer, poly(ethylene oxide) (PEO)-block-poly(glycerol monoacrylate) (PGA) have been synthesized via atom transfer radical polymerization of solketal acrylate (SA) using PEO-Br as macro-initiator, and subsequent hydrolysis of the acetal-protecting group. A hydrophobic fluorescent compound, 1-pyrenecarboxaldehyde, was used as a model drug, which was covalently bound to the PEO-b-PGA block copolymer via a pH-sensitive acetal linkage. The kinetics of the pyrene release was studied in THF/aqueous buffers at pH 1.0, pH 5.0 (close to pH in endosomes) and 7.4 (pH of blood plasma) by fluorescent spectroscopy. The results demonstrate that the double hydrophilic block copolymer PEO-b-PGA is a promising candidate for potential application as pH-sensitive carrier for carbonyl-containing hydrophobic drugs.
2) Novel amphiphilic block copolymers, poly(ethylene oxide)-b-poly(p-nitrophenyl methacrylate) (PEO-b-PNPMA) with controlled molecular weights and narrow molecular weight distributions were successively synthesized by ATRP of NPMA, using PEO-Br as macro-initiator. Self-assembling of the diblock copolymer PEO_(113)-b-PNPMA28 in the different solvent mixtures yielded various morphologies of star micelle-like aggregates, such as spheres, vesicles, cauliflower-like aggregates and rod-like aggregates, which were determined by the nature of the common solvents and the selective solvents. Thus the critical selective solvent contents and the solvent contents in PNPMA-rich phase were measured, and they have the following orders, ethanol>methanol>water, and THF>CH_3NO_2>DMSO. Based on this, the probable self-assembling mechanism was discussed. This method is convenient for preparation of multiple morphological star micelle-like aggregates in solution, especially from amphiphilic block copolymers with long shell block.
3) Triblock copolymers PNPMA-b-PS-b-PNPMA with 146 St units and 8, 20 and 36 NPMA units were prepared by ATRP of St using dibromoxylene as initiator, and following ATRP of NPMA. The anionic copolymer PMAA-b-PS-b-PMAA was synthesized by the hydrolysis of the PNPMA-b-PS-b-PNPMA, and the cationic copolymer PNPMAAm-b-PS-b-PNPMAAm was prepared by the amino substitution of the same PNPMA-b-PS-b-PNPMA. Equal mole of PMAA-b-PS-b-PMAA and PNPMAAm-b-PS-b-PNPMAAm both having the same chain lengths were mixed and dissolved in common solvent THF with 20% deionized water, and the solution was dialyzed against water to induce the copolymers self-assembly to form aggregates. Polydisperse spheres were observed containing an asymmetrically placed single void space, which has broken through the surface (so-called bowl-shaped aggregates).The possible mechanism was discussed. These bowl-shaped aggregates are promising candidates for nano reactor or drug carrier.
4) 2,7-dimethylene-1,4,6-trioxaspiro[4, 4]nonane with two vinyls was prepared to be used as electron-donor and crosslinker. The ATRP of this crosslinker and excess methylacrylate (used as electron-accpetor) was proved to mainly form homopolymers. With the chain-transfer agent S-1-Dodecyl-S'-(α,α'-dimethyl-α"-acetic acid)trithiocarbonate, the copolymerization of the spiro hydrocarbon, maleic anhydride (Mah) and MA by RAFT method produced star PMA. The molecular weights of obtained polymers measured by GPC were much higher than that of the linear polymers with the same monomer conversion. Samples taken with different time intervals in the polymerization initial stage were analyzed by ~1H NMR spectroscopy. The results demonstrated the possible mechanism. Charge transfer complexes of spiro hydrocarbon and Mah were formed, and first consumed in the initial stage, which produce a core with many chain-transfer groups on its surface. Then MA monomers were polymerized onto the core to form star polymers. This method can be expanded to other monomers. It is a simply way to prepare star polymers by one-pot.
5) Hyperbranched Poly(amidoamine) was obtained by the Michael addition polymerization of N,N'-cystaminebisacrylamide (CBA) and 1-(2-aminoethyl) piperazine (AEPZ). The electrospinning of hyperbranched Poly(amidoamine)s in methanol solution was performed. The effects of solution concentration, added voltage and accepting distance on the morphology of the obtained fibers were discussed. These polymer fibers could emit blue, green or red photoluminescence when excited by lights of different wavelength. The colorful photoluminescent fibers have potential applications in display field.
嵌段共聚物在选择性溶剂中自组装可以形成高分子胶束。聚合物胶束在药物缓释、分离、催化和纳米材料方面具有潜在的应用前景,引起人们的浓厚兴趣。通过物理包埋、静电作用或化学键联等方法,将不溶性药物与聚合物胶束相结合,可以增加药物的溶解性,延长药物的体内循环时间,控制药物定时定点释放,在医药学领域得到了广泛的应用。在化学键联法中,要求用于连接载药胶束与药物的化学键具有环境响应特性,目前可以选择的这类化学键还十分有限,这一领域还有待更多的研究。
聚合物胶束的聚集形态与其应用密切相关,目前除常见的球形胶束外,已经可以得到棒状、层状、碗形、管状、囊泡及其他多种具有复杂的复合结构的胶束。通过改变嵌段聚合物的自组装条件,控制形成的聚合物胶束的形态已有很多报道,但目前的研究工作大多集中在亲溶剂段较短的嵌段聚合物自组装形成的平头胶束上,研究星形胶束的形态多样性的报道还很少。
近年来在常规制备聚合物胶束的方法的基础上,出现了许多利用聚合物的特殊性质或聚合物分子间的特殊相互作用,实现高分子胶束化的新方法。两种含有相同嵌段长度并带有相反电荷的聚电解质链段的两亲性聚合物,通过静电相互作用,共同自组装形成复合胶束据我们所知还没有报道过。
星形聚合物是一类具有简单支化结构和特殊性能的聚合物,无论采用先臂后核还是先核后臂的路径合成星形聚合物,核或臂都要通过一个单独的步骤预先合成,或者需要分多步投入反应原料,这给工业规模的制备带来不便。一步法合成星形聚合物使核的形成与臂的生长能通过“一锅”反应来实现,不需要中间产物的分离与纯化,也不需要分两步加入反应原料,可以使星形聚合物的合成更为简单、有效。
静电纺丝技术是目前大规模制备纳米纤维最合适的方法,近几年来已经用于几十种不同的聚合物,并且通过溶胶-凝胶法配制溶液,适用范围已经扩大到无机物领域。但目前人们研究所用的聚合物还仅限于均聚物、共混聚合物和嵌段聚合物等,因而对具有特殊性能的超支化聚合物的静电纺丝的研究是一项很有意义的工作。
据此,本文的主要工作和取得的研究成果摘要如下:
1)以单端带有C-Br键的聚环氧乙烷(PEO-Br)作为大分子引发剂,引发丙烯酸缩酮甘油酯(SA)的ATRP,合成了PEO-b-PSA的嵌段聚合物,研究了这一聚合反应的活性特征,进一步通过脱去缩酮保护基将聚丙烯酸缩酮甘油酯嵌段(PSA)转化为聚丙烯酸甘油酯嵌段(PGA)。以具有荧光特性的1-醛基芘(Pyrene-CHO)做为药物模型,通过与PGA上邻-二羟基的缩合反应连到嵌段聚合物PEO-b-PGA的PGA上,所得的聚合物在选择性溶剂中自组装,形成以疏水的PGA-Py为核,亲水的PEO为壳的聚合物胶束。用荧光跟踪研究了芘在不同pH值(1.0,5.0和7.4)缓冲溶液中,从聚合物胶束中的释放动力学。研究结果表明,双亲水性嵌段聚合物PEO-b-PGA,可与含有羰基的药物,通过缩酮键连接并自组装形成酸敏感性载药胶束,在药物缓释领域具有潜在的应用前景。
2)用PEO-Br作为大分子引发剂,以ATRP法合成了环氧乙烷和甲基丙烯酸对硝基苯酚酯的嵌段共聚物(PEO-b-PNPMA),研究了聚合物PEO_(113)-b-PNPMA_(28)在选择不同的共溶剂(四氢呋喃、二甲亚砜和硝基甲烷)和选择性溶剂(甲醇、乙醇和水)时的稀溶液自组装行为,通过TEM观察到具有球形、棒状、囊泡、花椰菜形、双连续棒状等不同形态的星形聚集体。测试了所用的不同溶剂的临界选择性溶剂含量和PNPMA富集相溶剂含量,具有乙醇＞甲醇＞水,四氢呋喃＞硝基甲烷＞二甲亚砜的相对大小顺序。以此为基础讨论了这些不同形态的聚集体可能的形成机理。研究结果表明,采用改变共溶剂或选择性溶剂的方法,可以很方便地使成壳链段相对较长的两亲性嵌段聚合物形成的星形胶束,如平头胶束一样呈现多样的形态。
3)以对二溴苄(DBX)引发苯乙烯和甲基丙烯酸对硝基苯酚酯(NPMA)相继进行ATRP,合成了三嵌段聚合物PNPMA-b-PS-b-PNPMA。利用PNPMA嵌段易于水解和被氨基取代的特点,以相同PNPMA链长的三嵌段共聚物分别进行水解反应及与2-氨基吡啶的取代反应,制备了具有相反电荷的阴离子型PMAA-b-PS-b-PMAA和阳离子型PNPMAAm-b-PS-b-PNPMAAm两种三嵌段共聚物。将这两种三嵌段共聚物以等摩尔比混合,在水中自组装形成了碗形的聚集体结构,讨论了这种结构可能的形成机理。这些由聚电解质复合物自组装形成的聚集体,在微反应器和药物释放等领域具有潜在的应用前景。
4)合成了双乙烯基的2,7-二亚甲基-1,4,6-三氧杂螺环烷,作为给电子单体和交联剂,与吸电子单体马来酸酐(MAh)或过量的丙烯酸甲酯(MA)形成电荷转移络合物(CTC)共同聚合,尝试了用ATRP和RAFT方法一步法合成星形聚合物。在ATRP共聚合中,由于螺环交联剂与MA不能有效组成CTC,因而不能优先聚合而成核,它们的共聚合反应主要产生均聚物。在RFAT共聚合中,在S-1-十二烷基-S'-(α,α'-甲基-α”-乙酸)三硫代碳酸酯链转移剂存在下,摩尔比2:1的MAh和螺环交联剂,与过量MA进行共聚合成了星形聚合物。对聚合反应初期反应混合物的核磁共振氢谱跟踪结果证实了我们假定的聚合机理,即MAh与螺环交联剂形成CTC,并优先聚合形成了交联的带有多个转移基团的核,继而引发MA单体均聚形成了星形聚合物。可以预见,这种方法还可以方便地扩展到其他单体的聚合上,因而我们找到了一条比较简单的一步法合成星形聚合物的路线。
5)通过三元胺单体2-氨基乙基哌嗪(AEPZ)和等摩尔的二乙烯基单体胱胺双丙烯酰胺(CBA)进行迈克尔加成反应,获得了主链上含有三级胺、端基为一级胺的超支化聚(酰胺-胺)。对超支化聚(酰胺-胺)的甲醇溶液进行静电纺丝可制备聚合物纤维,研究了聚合物溶液浓度、外加电压和接收距离对电纺纤维的形态的影响。在荧光显微镜下观察,这种聚合物纤维可在不同波长的激发光作用下发出蓝色、绿色和红色的荧光。这种可以光致发光的聚合物纤维在显示领域有着潜在的应用前景。
Recently, block copolymers have attracted considerable attention because of their unique behaviors and potential applications, such as thermoplastics, surfactants, modifiers, dispersants, and tackifier etc. With the development of living radical polymerizations, such as SFRP, ATRP, RAFT and Iniferter, a large number of novel well-defined block copolymers with controlled molecular weights and narrow molecular weight distributions were prepared.
Polymer micelles, formed by self-assembly of block copolymers in selective solvent, have been extensively investigated for their potential applications in drug delivery, separation, catalysis and nanomaterials fields. For example, Hydrophobic drugs loaded by polymer micelles with physically entrapment or chemically conjugation are improved their water solubility and bioavailability. The drug-loaded micelles prolong their circulation in body and release selectively their payload in tumor tissue or within cells. However, the "smart" stimuli-responsive linkages, which are used to link drug and micelle in chemically conjugation method, are still limited.
The applications of polymer micelles are related to their morphologies. Beside frequently observed spherical core-shell micelles, Many other morphologies have been obtained, such as rod, worm-like, vesicle, lamellae and other complicated aggregates. These morphologies were usually prepared from crew-cut micelles by controlling the preparation conditions until now. There are few reports on the multiple morphologies of star micelles.
Polyion complex micelle, a novel micelle with its unique behaviors, is formed by a pair of opposite charged polymers in aqueous solution. The charged polymers used are usually homo-polyelectrolytes and double hydrophilic block copolymers consist of a polyelectrolyte block and a nonionic hydrophilic block such as PEO. The self-assemly of the mixture, which is composed of a pair of amphiphilic block copolymers with opposite charge and equal length, has not been researched.
Star polymer is a class of simplest branched polymer, which is usually prepared by "arm-first" and "core first" approach. No matter which approach is used in the literature, two steps are needed to get a star polymer. Either the core or the arms should be synthesized in a separate step; at least chemicals were added step by step. Therefore, a simple way of synthesis is highly appreciated.
Electrospinning is a very suitable method to obtained nanofibers. Many kinds of polymers, such as homopolymers, block copolymers and polymer blends, had been used to prepare nanofibers by electrospinning. In addition, inorganic nanofibers were fabricated by this method in recent years. The research of electrospinning of functional hyperbranched polymer is still an outgoing challenge.
All these facts are the origin and impetus of this thesis. The main results obtained in this thesis are as follows:
1) A new type of double hydrophilic block copolymer, poly(ethylene oxide) (PEO)-block-poly(glycerol monoacrylate) (PGA) have been synthesized via atom transfer radical polymerization of solketal acrylate (SA) using PEO-Br as macro-initiator, and subsequent hydrolysis of the acetal-protecting group. A hydrophobic fluorescent compound, 1-pyrenecarboxaldehyde, was used as a model drug, which was covalently bound to the PEO-b-PGA block copolymer via a pH-sensitive acetal linkage. The kinetics of the pyrene release was studied in THF/aqueous buffers at pH 1.0, pH 5.0 (close to pH in endosomes) and 7.4 (pH of blood plasma) by fluorescent spectroscopy. The results demonstrate that the double hydrophilic block copolymer PEO-b-PGA is a promising candidate for potential application as pH-sensitive carrier for carbonyl-containing hydrophobic drugs.
2) Novel amphiphilic block copolymers, poly(ethylene oxide)-b-poly(p-nitrophenyl methacrylate) (PEO-b-PNPMA) with controlled molecular weights and narrow molecular weight distributions were successively synthesized by ATRP of NPMA, using PEO-Br as macro-initiator. Self-assembling of the diblock copolymer PEO_(113)-b-PNPMA28 in the different solvent mixtures yielded various morphologies of star micelle-like aggregates, such as spheres, vesicles, cauliflower-like aggregates and rod-like aggregates, which were determined by the nature of the common solvents and the selective solvents. Thus the critical selective solvent contents and the solvent contents in PNPMA-rich phase were measured, and they have the following orders, ethanol>methanol>water, and THF>CH_3NO_2>DMSO. Based on this, the probable self-assembling mechanism was discussed. This method is convenient for preparation of multiple morphological star micelle-like aggregates in solution, especially from amphiphilic block copolymers with long shell block.
3) Triblock copolymers PNPMA-b-PS-b-PNPMA with 146 St units and 8, 20 and 36 NPMA units were prepared by ATRP of St using dibromoxylene as initiator, and following ATRP of NPMA. The anionic copolymer PMAA-b-PS-b-PMAA was synthesized by the hydrolysis of the PNPMA-b-PS-b-PNPMA, and the cationic copolymer PNPMAAm-b-PS-b-PNPMAAm was prepared by the amino substitution of the same PNPMA-b-PS-b-PNPMA. Equal mole of PMAA-b-PS-b-PMAA and PNPMAAm-b-PS-b-PNPMAAm both having the same chain lengths were mixed and dissolved in common solvent THF with 20% deionized water, and the solution was dialyzed against water to induce the copolymers self-assembly to form aggregates. Polydisperse spheres were observed containing an asymmetrically placed single void space, which has broken through the surface (so-called bowl-shaped aggregates).The possible mechanism was discussed. These bowl-shaped aggregates are promising candidates for nano reactor or drug carrier.
4) 2,7-dimethylene-1,4,6-trioxaspiro[4, 4]nonane with two vinyls was prepared to be used as electron-donor and crosslinker. The ATRP of this crosslinker and excess methylacrylate (used as electron-accpetor) was proved to mainly form homopolymers. With the chain-transfer agent S-1-Dodecyl-S'-(α,α'-dimethyl-α"-acetic acid)trithiocarbonate, the copolymerization of the spiro hydrocarbon, maleic anhydride (Mah) and MA by RAFT method produced star PMA. The molecular weights of obtained polymers measured by GPC were much higher than that of the linear polymers with the same monomer conversion. Samples taken with different time intervals in the polymerization initial stage were analyzed by ~1H NMR spectroscopy. The results demonstrated the possible mechanism. Charge transfer complexes of spiro hydrocarbon and Mah were formed, and first consumed in the initial stage, which produce a core with many chain-transfer groups on its surface. Then MA monomers were polymerized onto the core to form star polymers. This method can be expanded to other monomers. It is a simply way to prepare star polymers by one-pot.
5) Hyperbranched Poly(amidoamine) was obtained by the Michael addition polymerization of N,N'-cystaminebisacrylamide (CBA) and 1-(2-aminoethyl) piperazine (AEPZ). The electrospinning of hyperbranched Poly(amidoamine)s in methanol solution was performed. The effects of solution concentration, added voltage and accepting distance on the morphology of the obtained fibers were discussed. These polymer fibers could emit blue, green or red photoluminescence when excited by lights of different wavelength. The colorful photoluminescent fibers have potential applications in display field.
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