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1.
以丙烯酰胺(AM)和丙烯酸(AA)单体的水溶液为分散相,失水山梨醇单油酸脂(Span80)/聚氧乙烯失水山梨醇脂肪酸脂(Tween80)/异辛烷为分散介质,分别以N,N′-亚甲基双丙烯酰胺(MBA)、过硫酸铵/亚硫酸氢钠((NH4)2S2O8/NaHSO3)为交联剂和氧化还原引发剂,在30℃进行反相微乳液聚合制备了一系列不同单体摩尔百分数的P(AM-co-AA)微凝胶.通过傅立叶红外光谱、浊度法、透射电镜(TEM)和动态光散射(DLS)等测试手段分别对微凝胶特征官能团的存在、pH敏感性、微观形态、粒径大小及粒径分布等进行表征分析.结果表明,共聚物中存在AM和AA结构单元;样品的TEM照片显示在原料中AA的摩尔百分数为60%时,P(AM-co-AA)微凝胶粒子的数均粒径为90 nm左右,呈现非规则球形;DLS结果表明,P(AM-co-AA)微凝胶与PAM微凝胶相比具有较宽的粒径分布,且随原料中AA摩尔百分数增加,粒径分布逐渐变宽;P(AM-co-AA)微凝胶具有良好的pH敏感性,敏感pH值与AA的解离常数有关,通过调节pH值可以迅速控制自身体积的溶胀与收缩.  相似文献   

2.
PNI PAM/CS微凝胶的性质测定   总被引:1,自引:0,他引:1  
以N-异丙基丙烯酰胺(NIPAM)、壳聚糖(CS)为单体,N,N-亚甲基双丙烯酰胺(MBA)为交联剂,制备了PNIPAM/CS微凝胶.测定了不同单体配比对微凝胶体积相转变温度(VPTT)的影响和25℃不同pH条件下微凝胶液浊度及粒径的变化.研究表明,PNIPAM/CS微凝胶具有温敏性;并且随着pH的增大,微凝胶粒径先变小后变大,显示pH敏感性;浊度法测定结果与粒径测定一致.  相似文献   

3.
pH响应性阳离子型微凝胶的制备及性质研究   总被引:1,自引:0,他引:1  
孙桂香  张明祖  许杨  陆一鸣  倪沛红 《化学学报》2009,67(14):1685-1690
以甲基丙烯酸-(N,N-二甲氨基)乙酯(DMAEMA)和丙烯酸乙酯(EA)为共聚单体, 二甲基丙烯酸乙二醇酯(EGDMA)为交联剂, 采用半连续乳液聚合法, 制备了具有pH响应性的阳离子型微凝胶, 并研究不同聚合条件对所合成的微凝胶性质的影响. 利用透射电子显微镜(TEM)、激光粒度分析仪和流变仪对微凝胶进行一系列表征. 研究了介质pH值对微凝胶的形态、平均粒径、zeta电位、溶液浊度(透光率)的影响, 以及NaCl盐溶液对微凝胶分散体系稳定性的影响. 结果表明, 这类阳离子型微凝胶体系具有良好的pH响应性, 在pH=7左右发生相转变. 此外, 研究表明不同浓度NaCl溶液对微凝胶的稳定性有一定影响, 临界絮凝浓度约为1.3 mol•L-1.  相似文献   

4.
以无机粘土为交联剂制备了具有温度、pH双重敏感特性的羧甲基纤维素钠/聚(N-异丙基丙烯酰胺)/粘土半互穿网络纳米复合水凝胶(CMC/PNIPA/Clay semi-IPN),并通过红外和透射电镜对其结构和形态进行了表征。在酸性(pH=1.2)和20℃条件下,分别研究了温度和不同pH缓冲液对该凝胶溶胀度的影响,测定了复合水凝胶的力学性能。结果表明:水凝胶中的粘土被剥离成单片层,且均匀分散在凝胶网络中,起交联剂的作用,而CMC以线性大分子的形态存在;CMC/PNIPA/Clay具有良好的温度、pH双重敏感特性;凝胶的断裂伸长率>1 000%。  相似文献   

5.
交联核壳结构PBA/PS和PBA/PMMA纳米微球的制备与应用   总被引:1,自引:0,他引:1  
考察了聚丙烯酸丁酯/聚苯乙烯(PBA/PS)以及聚丙烯酸丁酯/聚甲基丙烯酸甲酯(PBA/PMMA)交联核壳结构纳米高分子微球的制备方法,并对其在尼龙复合材料中的应用进行了初步研究.结果表明,通过交联剂的引入使粒子核层和壳层内部均形成了高度交联的结构,可以限制亲水性较小的聚苯乙烯(PS)壳层向粒子内部迁移的趋势;制备出的微球平均粒径为40~50 nm,粒径分布很窄.采用饥饿态加料方式加入第二单体不仅可以使微球具有较高的产率和凝胶率,而且可以使其具有更理想的核壳结构和更窄的粒径分布.此外,将合成出的PBA/PMMA核壳粒子对尼龙6基体进行复合的结果表明,由于该微球表面与尼龙6基体之间具有较强的界面相互作用且微球具有较大的形变能力,可以在基体中形成良好的分散,在保持材料强度的同时有效地提高了其刚性和韧性.  相似文献   

6.
CS/TPP纳米微胶囊的制备及其载药性能   总被引:5,自引:0,他引:5  
利用离子凝胶法, 以三聚磷酸钠(TPP)为交联剂, 由壳聚糖(CS)制备了CS/TPP纳米微胶囊. 用红外光谱仪、扫描电镜和粒径分析仪进行了表征, 并以牛血清蛋白(BSA)作为模型药物, 考察了所制备的CS/TPP纳米微胶囊的包载和缓释性能. 结果表明, CS/TPP纳米微胶囊的红外光谱相对于CS和TPP的红外光谱发生了很大变化, 说明CS和TPP通过正负电荷吸引聚合成囊; 粒径分析表明, 离子凝胶法可以得到粒径约430 nm的均匀分散的壳聚糖纳米微胶囊, 经冷冻干燥后粒径变为300 nm左右; 微胶囊包封率最高可达79.74%, 模型药物的持续释放时间可达7 d以上.  相似文献   

7.
天然高分子具有良好的生物相容性和生物可降解性,因此用天然高分子制备的微凝胶更适合于生物医学领域的应用。羟丙基纤维素(HPC)是一种具有温度敏感性的纤维素衍生物,可通过不同的方法制备为微凝胶,然而现有方法制备的HPC微凝胶都不能完全降解。我们采用一种新方法制备HPC微凝胶。首先通过NaIO4处理将醛基引入HPC。红外光谱检测证明了醛基的生成。氧化后的HPC仍具温敏性,其最低临界溶解温度(LCST)保持不变;当加热到LCST以上时,HPC分子通过疏水相互作用聚集成纳米小球;再加入交联剂己二酸二酰肼,通过醛基与胺基之间的反应,使纳米小球共价交联得到HPC微凝胶。电镜研究表明HPC微凝胶呈球形,粒径在100~300nm之间。浊度和光散射研究表明HPC微凝胶仍具温敏性。细胞毒性实验表明我们制备的微凝胶几乎没有细胞毒性。由于HPC及交联剂己二酸二酰肼均可生物降解,预期我们制备的微凝胶也能很好地降解,并有望应用于生物医学领域。  相似文献   

8.
报道了一种采用光化学方法一步合成磁性纳米凝胶的方法. 在亲水性Fe3O4磁流体中, 以甲基丙烯酸2-羟基乙酯(HEMA)为单体, N,N-亚甲基双丙稀酰胺(MBA)为交联剂, 紫外光辐照下原位聚合制备了聚(甲基丙烯酸2-羟基乙酯)(PHEMA)磁性纳米凝胶. 运用红外光谱(FTIR)和热重分析(TGA)检测了磁性凝胶的化学组成, 得出其磁含量高达90%; 磁性测量表明凝胶呈现超顺磁性; 扫描电子显微镜(SEM)和透射电子显微镜(TEM)观测了其表面形貌和粒径, 通过光子相关光谱(PCS)得出其平均水合粒径及粒径分布, 发现外壳层凝胶有大的溶胀能力. 通过单体浓度、光照时间对磁性纳米凝胶粒径的影响研究, 发现可以调控磁性纳米凝胶的平均水合粒径在55.4~144.5 nm范围内变化, 并对可能的包敷机制进行了探索.  相似文献   

9.
以含双硫键的N,N-二(3-羧基丙烯酰)胱胺(BCCy)为交联剂,在1-(3-二甲氨基丙基)-3-乙基碳二亚胺盐酸盐/N-羟基琥珀酰亚胺(EDC/NHS)的催化下将壳聚糖(CS)交联,在水溶液中制备了纳米微凝胶。通过红外、元素分析、纳米粒度仪和扫描电镜等对其结构和形貌进行了表征,考察了pH和还原性环境对粒径的影响。对抗癌药物喜树碱(CPT)进行了负载,考察了载药粒子在还原性环境中对药物的控释性能。结果表明:随交联剂用量的增加,纳米微凝胶的粒径减小。该纳米微凝胶具有较好的生物相容性、较显著的pH和还原敏感性。  相似文献   

10.
阳离子化热响应微凝胶的合成及在二氧化硅矿化中的应用   总被引:1,自引:0,他引:1  
采用无皂乳液聚合技术,在亚甲基双丙烯酰胺(MBA)为交联剂的情况下,N-异丙基丙烯酰胺(NIPAM)与甲基丙烯酰氧乙基三甲基氯化铵(DMC)发生共聚,生成具有阳离子功能化的热响应微凝胶poly-(NIPAM-co-DMC).TEM研究表明该微凝胶粒子的粒径约为200 nm左右,具有规则的球形形态.DLS和1H-NMR研究证实了微凝胶粒子的最低临界溶液温度(LCST)在34℃左右.进一步以此微凝胶为模板,在中性条件下,以四甲氧基硅烷(TMOS)为硅源,在此模板上仿生沉积S iO2,生成poly(NIPAM-co-DMC)/S iO2杂化纳米粒子.FTIR、TEM、1H-NMR及TGA等研究表明S iO2在聚合物模板上发生了沉积.能谱分析进一步证明了S iO2主要分布在杂化纳米粒子的壳层区域.另外,当矿化反应温度高于微凝胶的LCST值时,体系生成了具有明显核壳结构的异形杂化粒子.  相似文献   

11.
A novel pH- and temperature-sensitive nanocomposite microgel based on linear Poly(acrylic acid) (PAAc) and Poly(N-isopropylacrylamide) (PNIPA) crosslinked by inorganic clay was synthesized by a two-step method. First, PNIPA microgel was prepared via surfactant-free emulsion polymerization by using inorganic clay as a crosslinker, and then AAc monomer was polymerized within the PNIPA microgel. The structure and morphology of the microgel were confirmed by FTIR, WXRD and TEM. The results indicated that the exfoliated clay platelets were dispersed homogeneously in the PNIPA microgels and acted as a multifunctional crosslinker, while the linear PAAc polymer chains incorporated in the PNIPA microgel network to form a semi-interpenetrating polymer network (semi-IPN) structure. The hydrodynamic diameters of the semi-IPN microgels ranged from 360 to 400 nm, which was much smaller than that of the conventional microgel prepared by using N,N′-methylenebis(acrylamide) (MBA) as a chemical crosslinker, the later was about 740 nm. The semi-IPN microgels exhibited good pH- and temperature-sensitivity, which could respond independently to both pH and temperature changes.  相似文献   

12.
Adopting inorganic clay (hectorite) and MBA as physical and chemical cross‐linking agents, respectively, PNIPAM microgels were synthesized by SFEP. The chemical structure and morphology of the microgels were confirmed by FTIR, WXRD, and SEM. The temperature‐sensitivity of the microgels was investigated by DLS and UV spectrophotometers. The results inferred that clay platelets dispersed in an aqueous medium were fully exfoliated and could act as a kind of multifunctional cross‐linking agent and significantly reduced the hydrodynamic diameters of the microgels. In fact, the hydrodynamic diameters of the PNIPAM microgels with clay as cross‐linker ranged from 154 to 322 nm which was much smaller than that using MBA as chemical cross‐linker, the later was in the range of 284–808 nm on heating from 5 to 50 °C.

  相似文献   


13.
通过γ 射线辐照技术 ,在稀水溶液中实现了N ,N′ 亚甲基双丙烯酰胺 (Bis)与 4 乙烯基吡啶 (4 VP)的无皂乳液共聚 ,得到平均流体力学半径 (Rh)为 5 6~ 15 2nm的一系列微凝胶 ,并通过红外光谱、热分析、透射电镜进行了表征 .通过测定Rh、吸光度、凝胶比 ,研究了与Bis共聚的单体及比例、剂量和剂量率对微凝胶合成的影响 .结果表明 ,微凝胶的大小可以通过吸收剂量、单体相对含量的改变来进行控制 .最后 ,对微凝胶的形成机理进行了初步探讨 .  相似文献   

14.
以N-异丙基丙烯酰胺(NIPAM)、甲基丙烯酸(MAA)为单体,N,N-亚甲基双丙烯酰胺(MBA)为交联剂,制备了温敏性聚(N-异丙基丙烯酰胺)(PNIPAM)和具有温度、pH敏感性的聚(N-异丙基丙烯酰胺-co-甲基丙烯酸)(PNIPAM-MAA)微凝胶。通过测定不同温度和pH条件下微凝胶浊度变化,表征微凝胶的温度及pH敏感性,描述了NaCl浓度和pH对微凝胶体积相转变温度的影响。同时,测定了微凝胶的临界聚沉浓度及临界絮凝温度,表征了微凝胶的稳定性,讨论了影响微凝胶的稳定性因素。  相似文献   

15.
We report a microfluidic approach to generating capsules of biopolymer hydrogels. Droplets of an aqueous solution of a biopolymer were emulsified in an organic phase comprising a cross-linking agent. Polymer gelation was achieved in situ (on a microfluidic chip) by diffusion-controlled ionic cross-linking of the biopolymer, following the transfer of the cross-linking agent from the continuous phase to the droplets. Gelation was quenched by collecting particles in a large pool of cross-linking agent-free liquid. The structure of microgels (from capsules to gradient microgels to particles with a uniform structure) was controlled by varying the time of residence of droplets on the microfluidic chip and the concentration of the cross-linking agent in the continuous phase. We demonstrated the encapsulation of a controlled number of polystyrene beads in the microgel capsules. The described approach was applied to the preparation of capsules of several polysaccharides such as alginate, kappa-carrageenan, and carboxymethylcellulose.  相似文献   

16.
A new method, adopting inorganic clay (synthetic hectorite) as a physical cross-linker, was used to prepare poly(N-isopropylacrylamide) (PNIPAM) microgels via surfactant-free emulsion polymerization. The effect of hectorite content on the temperature-sensitivity of PNIPAM microgels was investigated by means of DLS, UV/Vis and DSC. It was found that, in the absence of surfactant, with increasing hectorite content, the particle size tends to decrease to 300 nm at room temperature, while increases as weight ratio (WR) of hectorite and N-isopropylacrylamide (NIPAM) exceeds 21%. Furthermore, with increasing WR from 7% to 21%, the volume phase transition temperature of PNIPAM microgels has little shift, while decreases slightly when WR increases up to 28%.  相似文献   

17.
We used soft microgels made of poly(N-isopropylacrylamide) (pNIPAM) of variable cross-linking degrees and the same colloidal size to stabilize oil-in-water Pickering emulsions. The extent of droplet flocculation increased and the resistance of the emulsions to mechanical stresses decreased as the cross-linking density was augmented. Large flat films were separating the droplets, and we could measure the adhesion angle at the junction with the free interfaces through several microscopy methods. The size of the flat films and the values of the angles were reflecting strong adhesive interactions between the interfaces as a result of microgel bridging. In parallel, cryo-SEM imaging of the thin films allowed a precise determination of their structure. The evolution of the adhesion angle and of the film structure as a function of microgels cross-linking density provided interesting insights into the impact of particle softness on film adhesiveness and emulsion stability. We exploited our main findings to propose a novel route for controlling the emulsions end-use properties (flocculation and stability). Owing to particle softness and thermal sensitivity, the interfacial coverage was a path function (it depended on the sample "history"). As a consequence, by adapting the emulsification conditions, the interfacial monolayer could be trapped in a very dense and rigid configuration, providing improved resistance to bridging flocculation and to flow-induced coalescence.  相似文献   

18.
高浓度丙烯酸酯类微凝胶分散液的制备及性质   总被引:3,自引:1,他引:3  
用微乳液聚合方法合成了浓度高达30wt%的丙烯酸酯类微凝胶,研究了乳化剂用量和微乳液浓度对微凝胶粒径及分布的影响,以及交联剂用量对微凝胶二甲苯分散液的流变行为的影响。利用制备的微凝胶对高固体份羟基丙烯酸树脂进行了改性。实验结果表明,微凝胶改性的树脂具有显著的切力变稀现象。  相似文献   

19.
pH-responsive microgels are cross-linked polymer colloids that swell when the pH approaches the pK a of the particles. In this work, we present a comprehensive investigation of pH-triggered particle swelling and gel formation for a range of microgels containing methacrylic acid (MAA). The microgels investigated have the general composition poly(A/MAA/X), where A and X are the primary co-monomer and cross-linking monomer, respectively. The primary co-monomers were methyl methacrylate (MMA), ethyl acrylate (EA) or butyl methacrylate. The cross-linking monomers were either butanediol diacrylate (BDDA) or ethyleneglycol dimethacrylate (EGDMA). The microgels were studied using scanning electron microscopy, photon correlation spectroscopy (PCS) and dynamic rheology measurements. Gel phase diagrams were also constructed. The particles swelled significantly at pH values greater than approximately 6.0. It was shown that poly(EA/MAA/X) microgels swelled more strongly than poly(MMA/MAA/X) microgels. Furthermore, greater swelling occurred for particles prepared using EGDMA than BDDA. Concentrated dispersions of all the microgels studied exhibited pH-triggered gel formation. It was found that the fluid-to-gel transitions for the majority of the six microgel dispersions investigated could be explained using PCS data. In those cases, gelation was attributed to a colloidal glass transition. Interestingly, the microgels that were considered to have the highest hydrophobic content gelation occurred under conditions where little particle swelling was evident from PCS. The data presented show that gelled poly(EA/MAA/BDDA) and poly(MMA/MAA/EGDMA) microgel dispersions have the strongest elasticities at pH = 7.  相似文献   

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