微滴乳液聚合制备PDMS/SiO2纳米复合材料

采用超声分散的方法,以少量八甲基环四硅氧烷(D₄)对硅溶胶粒子进行表面接枝改性。然后在改性硅溶胶存在下,以十二烷基苯磺酸(DBSA)为乳化剂兼催化剂进行D₄的微滴乳液聚合,得到聚硅氧烷(PDMS)/二氧化硅(SiO₂)纳米复合乳液。采用FTIR、TGA、纳米粒度仪、TEM和拉力机分别对样品进行了表征。结果表明:采用超声分散的方法,能够有效地实现硅溶胶粒子的表面改性。通过微滴乳液聚合得到的复合乳胶粒是聚合物包覆二氧化硅粒子的核壳结构形态。SiO₂的引入提高了有机硅复合膜力学性能,增强了热稳定性。     

纳米SiO2／氟改性聚丙烯酸酯复合乳液的制备

以正硅酸乙酯为前驱物,采用溶胶一凝胶法原位制备纳米Si02粒子,然后通过细乳液聚合制得纳米Si02／氟改性聚丙烯酸酯复合乳液。采用傅里叶变换红外光谱（FTIR）和动态光散射（DLS）对产物进行了表征。研究了含氟单体和纳米Si02用量对复合乳胶膜性能的影响。结果表明：随着氟含量的增加,乳胶膜的水接触角增加,吸水性降低;体系中加入纳米Si029可以降低聚合物乳胶膜的吸水率。     

微乳液-溶胶凝胶法制备TiO2纳米光催化剂及结构表征

在TX-100／正己烷／正己醇／水（pH-9）微乳液环境中进行溶胶凝胶过程制备纳米TiO2粉体。研究在微乳液环境中发生稳定的溶胶凝胶过程的操作条件,并采用XRD、TG—DSC、FTIR、SEM、BET等手段对煅烧前后的TiO2粉体材料进行了结掏表征;研究结果表明在合适的操作条件下,该方法可以制备出12-26nm范围内粒径分布窄,平均孔径为47．6nm,BET比表面积为70．51m2／g,单一的锐钛矿型TiO2纳米微粒。     

细乳液聚合制备聚丙烯腈/纳米SiO2复合粒子

由含甲基丙烯酸-3-三甲氧基硅烷(MPS)改性纳米SiO2的丙烯腈细乳液聚合制备聚丙烯腈/纳米SiO2复合粒子.研究了纳米SiO2的改性及含量、十二烷基硫酸钠(SDS)乳化剂和十六烷(HD)助乳化剂浓度对细乳化液滴粒径的影响.结果表明,直接采用未改性纳米SiO2,细乳化后出现双峰分布,纳米SiO2粒子未有效进入单体液滴;用10%MPS改性纳米SiO2后,细乳化液滴呈单峰分布.随着纳米SiO2粒子含量的增加,细乳化液滴的平均粒径增大,分布变宽.含纳米SiO2粒子的细乳化液滴体的平均粒径随SDS浓度和HD浓度增大而减小.透射电镜观察发现,细乳液聚合产物的连续相中无纳米SiO2粒子分布,复合粒子呈非规整结构,纳米SiO2>粒子在聚丙烯腈基体中基本呈初级粒子分布.     

原位乳液聚合法制备超易分散纳米氧化锌

采用溶胶-凝胶法制得纳米氧化锌（ZnO）溶胶,将ZnO溶胶分散于乙酸乙烯酯单体中,通过原位乳液聚合法对纳米粒子进行表面有机修饰,制备出超易分散纳米氧化锌,ZnO在聚乙酸乙烯酯中显示出优异的分散性和稳定性。     

两步反相微乳液法原位制备纳米SiO2/聚甲基丙烯酸甲酯复合微粒

采用两步反相微乳液法原位聚合制备纳米SiO2／聚甲基丙烯酸甲酯(polymethylmethacrylate,PMMA)复合微粒。首先,通过混合2个分别增溶有2种反应物的微乳液,制备纳米SiO2粒子;然后,向混合后的微乳液中滴加单体及引发剂,通过单体的原位聚合反应得到SiO2,PMMA复合微粒。通过相图研究：确定了微乳液法制备复合微粒时初始组分的用量。通过透射电子显微镜、红外光谱、热重分析、X射线光电子能谱等手段对复合微粒进行了表征。结果表明：聚合后的PMMA包覆在SiO2表面．复合微粒的平均粒径为30nm．分散性良好。复合微粒中不能被抽提出来的聚合物占10．08％,这部分聚合物以Si-O-C键形式接枝在SiO2表面。     

细乳液聚合制备纳米SiO2／含氟丙烯酸酯复合乳液及其性能研究

采用溶胶-凝胶法,以正硅酸乙酯为前驱物,在丙烯酸酯单体为油相介质中原位生成纳米SiO2粒子,并通过细乳液聚合,制备出纳米Si02／含氟丙烯酸酯复合乳液。研究了含氟单体和SiO2的用量对复合乳胶膜性能的影响,并采用FT-IR,DSL等分析手段对产物进行了表征。结果表明：该乳液具有良好的稳定性,粒径分布较窄。当（甲基丙烯酸十二氟庚酯）FA与SiO2的用量分别为6％和5．5％时,乳胶膜表现出良好的疏水性能,对水的接触角达到了102．7°,吸水性降低到6．9％。     

种子乳液聚合法制备纳米SiO_2/苯丙复合乳液

采用种子乳液聚合工艺,用经硅烷偶联剂改性后的纳米SiO2原位合成了纳米SiO2/苯丙复合乳液。通过正交实验确定了最佳原料配比和聚合工艺条件,并对复合乳液性能进行了分析与表征。结果表明,当功能单体的用量为单体总量的5%、阴离子乳化剂十二烷基硫酸钠(SDS)与非离子乳化剂辛基苯基聚氧乙烯醚(OP-10)质量比为1颐1、复合乳化剂总量3%、纳米SiO2含量为单体总量的1.5%、聚合温度为80℃时,可制备具有良好综合性能的复合乳液,其涂膜耐水性、硬度、附着力等均优于普通苯丙乳液。该复合乳液乳胶粒粒度呈单峰分布,平均粒径为101nm,具有核/壳结构。     

原位乳液聚合制备的聚丙烯酸丁酯/纳米SiO2复合粒子的形貌和形成机理

通过吸附于水相分散纳米SiO2粒子表面的2,2'-偶氮(2-脒基丙烷)二氢氯化物(AIBA)的引发作用,进行丙烯酸丁酯(BA)的原位乳液聚合,制备聚丙烯酸丁酯(PBA)/纳米SiO2复合乳胶粒.分别采用透射电镜观察复合粒子的形貌,高速离心分离/超声分散和氢氟酸腐蚀表征复合胶乳中PBA乳胶粒与纳米SiO2粒子的结合程度.发现有纳米SiO2粒子聚集于复合乳胶粒表面,复合粒子表面粗糙,呈"草莓形"结构;当复合粒子中SiO2质量分率为14.6%～22.6%时,60%左右的纳米SiO2富集于复合粒子表面,30%左右被包覆在复合粒子内部,另有少量游离于水相.采用原位乳液聚合得到的复合粒子中纳米SiO2与聚合物的结合牢度远大于以AIBA为引发剂合成的PBA乳液与纳米SiO2分散液直接混合所能达到的结合牢度.认为在原位乳液聚合过程中,由于纳米SiO2粒子表面锚固的PBA量的不同,引起SiO2粒子的亲水/亲油性和与PBA的相容性也不相同,导致出现以上的SiO2的分布特性和复合粒子形貌.     

微乳液聚合在钻井液中的研究进展

概述了微乳液的结构,形成机理以及微乳液聚合的基本原理。简单介绍了正相微乳液聚合、反相微乳液聚合以及双连续相微乳液聚合的研究,综述了微乳液聚合产品在钻井液中的应用。探讨了微乳液聚合存在的一些问题,并对今后的发展前景进行了展望。     

细乳液聚合制备改性硅溶胶／聚丙烯酸酯复合乳液

常温下一步法制备改性硅溶胶,并通过细乳液聚合制备改性硅溶胶／聚丙烯酸酯复合乳液。考查了温度对聚合速率和单体转化率的影响以及不同乳化剂含量下聚合过程中乳胶粒粒径的变化情况;测试了乳胶膜的吸水率,并用接触角法表征了乳胶膜的表面自由能。     

High‐molecular‐weight polyurethanes prepared by one‐step miniemulsion polymerization

Through one‐step miniemulsion polymerization, hydrophobic polyurethane (PU) dispersions were prepared, with hexadecane (HD) as costabilizer in the oil phase and sodium dodecyl sulfate (SDS) as surfactant in the water phase. The oil phase, including isophorone diisocyanate, poly(oxytetramethylene) glycol, a costabilizer HD, a chain extender 1,4‐butanediol, a crosslinking agent trimethylol propane, and a catalyst dibutyltin dilaurate (SnDBL), was dispersed in the water phase containing SDS. The influences of experimental parameters, such as SnDBL, NCO/OH equivalents, and concentrations of surfactant, were discussed. The particle size and the molecular weight of PU polymer were measured by light scattering and gel permeation chromatography, respectively. With the addition of SnDBL and higher NCO/OH ratio, PU films with higher molecular weights were produced. The chemical structure of the PU polymer was identified by Fourier transform infrared spectrometer, and the adsorption of urethane group was observed. Thermal gravimetric analysis was used to characterize the thermal stability of PU. Furthermore, mechanical property was also investigated and characterized by tensile strength and elongation at break. With a higher NCO/OH ratio and the existence of SnDBL, the tensile strength of PU films was significantly increased. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2008     

Polyamide 6/silica nanocomposites prepared by in situ polymerization

A polyamide 6 (PA 6)/silica nanocomposite was obtained through a novel method, in situ polymerization, by first suspending silica particles in ϵ-caproamide under stirring and then polymerizing this mixture at high temperature under a nitrogen atmosphere. The silicas were premodified with aminobutyric acid prior to the polymerization. The effects of the addition of unmodified and modified silicas on the dispersion, interfacial adhesion, isothermal crystallization, and mechanical properties of PA 6 nanocomposites were investigated by using scanning electron microscopy, dynamic mechanical analysis, differential scanning calorimetry, and mechanical tests, respectively. The results show that the silicas dispersed homogeneously in the PA 6 matrix. The addition of silicas increases the glass transition temperature and crystallization rate of PA 6. The mechanical properties such as impact strength, tensile strength, and elongation at break of the PA 6/modified silica nanocomposites showed a tendency to increase and decrease with increase of the silica content and have maximum values at 5% silica content, whereas those of the PA 6/unmodified silica system decreased gradually. © 1998 John Wiley & Sons, Inc. J Appl Polym Sci 69: 355–361, 1998     

Optimizing nitroxide-mediated miniemulsion polymerization processes

Living/controlled radical polymerizations provide significant advantages in the control of polymer resin microstructure compared to conventional radical polymerization. Advances in our ability to tailor polymer microstructure will enable improvements in coatings properties and possible new applications of coating technologies. Adapting living radical polymerizations to heterogeneous media such as aqueous-based miniemulsion polymerization presents several challenges related to maintaining the livingness (the fraction of chains that are still “living” at the end of polymerization) of the polymer chains and also developing a commercially viable process. We have studied the nitroxide-mediated polymerization of styrene in miniemulsion, with the intent of maintaining a high degree of livingness by balancing the rates of biradical termination and disproportionation. We can now achieve >95% monomer conversion in less than three hours, while maintaining polydispersities ∼1.3. Monomer conversion can be dramatically increased from about 60–95% by changing the concentration of sodium dodecylbenzenesulfonate (SDBS) surfactant. Conversions in Dowfax 8390 stabilized miniemulsions showed no comparable dependency. Reasons for this potentially commercially important effect are under investigation.     

Synthesis of polypyrrole/indium tin oxide nanocomposites via miniemulsion polymerization

Polypyrrole/indium tin oxide nanocomposites were synthesized via in situ miniemulsion polymerization of pyrrole monomer in the presence of indium tin oxide nanoparticles. Different nanocomposites were synthesized by different loadings of nano indium tin oxide. The morphology and nanoparticles distribution of the nanocomposites were characterized by electron microscopy. The results of XRD and TEM analysis showed that indium tin oxide nanoparticles were well placed in the polymeric structure of latex. FTIR analysis was used for the characterization of synthesized polypyrrole and its nanocomposites. TGA analysis was performed to investigate the thermal behavior of pristine polypyrrole and its nanocomposites. Conductivities of nanocomposites were measured by 4-point probe method and compared to the neat polymer.     

细乳液聚合制备含氟丙烯酸酯聚氨酯共聚物

采用细乳液聚合法,制备了稳定的含氟丙烯酸酯聚氨酯细乳液。用FT-IR表征了丙烯酸酯聚氨酯预聚体及其共聚物的结构组成;考查了细乳液的稳定性;用透射电子显微镜(TEM)观察了乳胶粒的形态;用接触角法表征了乳胶膜对水和正十六烷的接触角。     

助乳化剂及其对细乳液聚合的影响

细乳液聚合由于在体系中引进了助乳化剂,是一种新型的乳液聚合,助乳化剂是细乳液聚合中的重要组成部分。介绍了细乳液聚合的特点、助乳化剂在细乳液聚合中的作用;较详细地分析了助乳化剂对细乳液聚合的影响;指出了目前助乳化剂存在的缺陷,强调开发多种类、多功能助乳化剂的重要性。     

Emulsion and miniemulsion polymerization of isobornyl acrylate

Isobornyl acrylate, a highly hydrophobic monomer, was batch‐polymerized in both emulsion and miniemulsion recipes. Surfactant levels above and below the critical micelle concentration were used, as were two different initiator types: ionic (potassium persulfate) and nonionic (t‐butyl hydroperoxide) Samples were analyzed for degree of conversion, molecular weight, and particle size. The effects of reaction type (emulsion versus miniemulsion), surfactant level, type of initiator (ionic versus nonionic) of the polymer properties are discussed. Issues of monomer transport across the aqueous phase, and mechanisms of nucleation, especially at very low surfactant concentrations are discussed. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 103: 819–833, 2007     

Thermal storage nanocapsules by miniemulsion polymerization

Paraffin wax was nanoencapsulated by miniemulsion polymerization. Low solid content batch polymerizations were carried out and the influence of paraffin wax/methyl methacrylate ratio on polymeriztion kinetics, phase change properties, and thermal stability were investigated. Paraffin concentration controls the nucleation mechanism and nanocapsules particle size. The latent heat capacity increases as the content of encapsulated paraffin wax increases. The maximum amount of encapsulated paraffin wax achieved under the experimental conditions was 60 wt %, presenting a latent heat capacity of 140.3 J/g. Moreover, the encapsulated systems present in all cases better thermal stability than pure paraffin wax. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013