改进型聚丙烯酸系高效减水剂的合成

根据分子结构设计原理,合成了一种改进型聚丙烯酸系高效减水剂(PC-C),对影响减水剂性能的几个关键因素进行了探讨,并用红外光谱表征了其分子结构。通过正交实验获得了最佳的合成参数:乙烯基磺酸钠(SVS):丙烯酸(AA):丙烯酸聚乙二醇单酯(PEA)=1.5:5:3,过硫酸铵(APS)用量为单体总质量的3%;同时研究了减水剂侧链和掺量对分散性能的影响。结果表明:采用甲氧基聚乙二醇(MPEG)作为接枝侧链合成减水剂的分散能力优于采用聚乙二醇(PEG)合成的减水剂;PC-C低掺量即可发挥高分散性能,分散保持性能随掺量的增加而得以提高。     

影响St-MMA-MA无皂乳液胶粒性质的因素丙烯酸浓度及加料方式的影响

以苯乙烯、甲基丙烯酸甲酯为主单体,丙烯酸为功能单体合成了三元无皂乳液共聚胶粒。用ＴＥＭ观测了胶粒形态、大小及其分布;以电导滴定法测定了胶粒表面－ＣＯＯＨ的密度。考察了不同的聚合阶段加入不同量的丙烯酸对所得胶粒形态、大小及其表面－ＣＯＯＨ的密度的影响。结果表明：在聚合前加入丙烯酸,随着丙烯酸浓度的增大,胶粒粒径减小、分散系数增大;在成核后期滴加丙烯酸,胶粒粒径较大且随丙烯酸浓度增大粒径变化不大而分散     

SBS亲水性接枝共聚物的合成及表征

采用自由基接枝共聚的方法合成了亲水性ＳＢＳ接枝丙烯酸共聚物,同时进行了结构表征。该共聚物易于分散在水中,并形成亚微米级球形微粒     

有机胺催化制备单分散二氧化硅纳米球形颗粒

基于Stber方法,在以正硅酸乙酯为硅源及乙醇和水为共溶剂的条件下,利用不同结构的小分子有机胺为催化剂成功地制备出了一系列单分散SiO_2纳米颗粒.扫描电镜和透射电镜的表征结果表明,所合成的SiO_2颗粒呈现实心球的形貌,其粒径分布范围在几纳米到500nm之间.同时,实验表征结果也进一步说明,通过选用不同结构的小分子有机胺作催化剂能对SiO_2颗粒的粒径和形貌进行有效地调控.此外,本文作者还对小分子有机胺催化制备不同粒径和形貌SiO_2颗粒的作用机理进行了初步的讨论.     

pH敏感的金纳米颗粒的制备及表征

利用立方硅氧烷(odaaps)作为保护剂合成了金纳米颗粒,利用紫外-可见(UV-vis)吸收光谱、透射电镜(TEM)对纳米颗粒进行了表征。通过改变纳米溶胶的pH值,从而改变立方硅氧烷上羧基的存在形式,控制纳米颗粒表面的电荷,实现金纳米颗粒的可逆聚集与分散;当将其pH值降低至2.5时,颗粒能够完全沉淀,加碱调节其pH与原始值(pH=9)一致时,聚集的颗粒会自动重新分散形成溶胶,其具有与起始一致的高分散性。     

单分散纳米金尺寸的分步晶种生长控制

以聚乙烯吡咯烷酮(poly(vinylpyrrolidone), PVP)为保护剂, 硼氢化钠为还原剂, 合成了尺寸为(1.9±0.4) nm的单分散金胶体, 再以其作为一级晶种, 并分别用抗坏血酸和PVP为还原剂和保护剂, 通过改变各步晶种尺寸和氯金酸与晶种的摩尔比分步逐级合成了尺寸为3.2、4.7、6.3、8.0、10.3、14.0 nm的系列金纳米颗粒. 以LaMer模型为基础, 对分步晶种生长过程中影响金胶体产物尺寸分布(单分散性)的主要因素进行了讨论. 缓慢加入抗坏血酸并降低氯金酸对晶种的相对量对于单分散金纳米颗粒的控制合成有决定性作用. 快速加入抗坏血酸会因二次成核而导致金颗粒尺寸分布范围变宽.     

CdS/BiVO4复合半导体制备及其光催化性能

采用水热法以BiVO_4纳米片为基体原位生长CdS晶体,得到CdS/BiVO_4复合光催化剂,利用XRD、SEM、UV-Vis DRS等方法对材料进行了表征,通过降解亚甲基蓝对样品的光催化性能进行评价。结果表明,BiVO_4为方形片状颗粒,其表面附着棒状CdS纳米颗粒,分散较好。CdS/BiVO_4复合光催化剂表现出较高的光催化活性,在可见光照射下,利用CdS/BiVO_4光催化降解亚甲基蓝,60 min后的降解率达94.79%,相比于纯相BiVO_4和CdS有显著提高,且对多种有机染料均有良好的降解效果,重复使用性较好。机理研究发现,超氧自由基(·O_2~-)是CdS/BiVO_4光催化降解亚甲基蓝的主要活性物种。     

单分散球状纳米金颗粒的合成*

综述了近年来单分散球状金纳米颗粒的合成研究进展。分析了球状单分散金纳米颗粒的应用前景,介绍了单分散球状金纳米颗粒的主要合成方法如种子生长、回流熟化、尺寸选择沉淀分级以及电泳法等,评述了各种方法的优缺点。最后提出了单分散球状金纳米颗粒合成的一些问题,并展望了单分散球状金纳米颗粒的研究和发展方向。     

水脱型UV防护油墨的制备及性能研究

通过将环氧树脂E44、丙烯酸、2-丙烯酰胺-2-甲基丙磺酸反应,合成了一种改性环氧丙烯酸树脂。将改性的环氧丙烯酸树脂作为主体树脂,复配活性单体、引发剂、助剂、填充料等进行混合、分散、研磨,制备得到热水脱膜UV防护油墨。将该树脂与其他丙烯酸树脂进行性能对比,并进一步探究不同活性单体、膜层厚度与光固化能量对防护油墨的性能影响。实验表明,该树脂具有较好的热水脱膜性能,当采用活性单体二乙二醇二甲基丙烯酸酯,膜层厚度为30?m及固化能量为1 500 mJ/cm2时,防护油墨综合性能最佳。     

从含氢硅油制取水性氟硅聚合物

在无溶剂的条件下, 通过硅氢加成法将烯丙基聚氧乙烯聚氧丙烯醚, 氟化丙烯酸烷基酯接枝共聚到甲基含氢硅油侧链, 成功地合成了一系列有机氟硅聚合物. 通过高速剪切乳化法可制得不同质量投料比时的水性氟硅聚合物水分散物. 采用FTIR, ¹H NMR和TEM对有关产物和乳液进行了结构分析, 并进一步系统研究了水分散物表面张力, 流变性等性能, 结果表明: 质量分数为2.0%的水性氟硅聚合物水分散物的表面张力降低至22.00～26.00 N/m, 其黏度随着剪切速率的增大有剪切变稠现象发生, 且不同质量投料比时, 其粒子粒径大小及形状也有较大差别.     

“核-壳”结构微交联聚苯乙烯微粒的合成与表征

本文用复合乳液聚合方法合成了粒径70—160nm的窄分散、微交联聚苯乙烯微粒,透射电子显微镜观测表明该微粒具有核-壳结构。用薄层色谱、透射电镜结合凝胶色谱、粘度等方法对该微粒进行了结构表征并探讨了影响微粒结构的主要因素。实验结果表明:双烯A用量为苯乙烯单体Ⅰ重量的1—4％,第一阶段聚合两小时后,滴加苯乙烯单体Ⅱ进行壳层聚合,合成的微粒含8.0—15.0％的线性聚苯乙烯,壳层主要由与核连接的聚苯乙烯链构成。     

Comparative study between core-shell and interpenetrating network structure polyurethane/polyacrylate composite emulsions

Anionic aqueous polyurethane dispersion was prepared by using carboxyl acid group to make the polyurethane dispersible, and then nanograde core-shell and crosslinked IPN structure polyurethane/polyacrylate composite latex (PUA) were synthesized by soap-free emulsion polymerization method with polyurethane dispersion as seed. FTIR, DSC, dynamic light scattering, TEM, ESCA, TGA, electronic tensile machine were employed to investigate the structures and properties of the composite latex and their polymers. Meanwhile the core-shell composite PUA emulsion and the crosslinked IPN composite PUA emulsion were compared. The results showed that the particle morphology of PUA composite emulsion is inverted core-shell structure with polyacrylate as the core and with polyurethane as the shell. The morphology of the crosslinked PUA emulsion was multi-core structure. The surface in core-shell PUA contains rich PU phase. The phase structure of the crosslinked PUA is more uniform. Three transition temperatures are observed for the core-shell composite PUA, two transitions are observed for the film from the crosslinked PUA. The TGA curves of core-shell PUA and crosslinked PUA exhibit two stages, the first stage corresponds to the thermal decomposition of hard segments in seed polyurethane; the second stage corresponds to the decomposition of soft segments in PUA and decomposition of polyacrylate. With the increase of glycidyl methacrylate (GMA) amounts in PUA composite emulsions, the tensile strength of the PUA films as well as the average diameter of the PUA composite emulsion particles increase, the elongation at break of the PUA films decreases.     

Facile synthesis and performance of polypyrrole-coated sulfur nanocomposite as cathode materials for lithium/sulfur batteries

In situ chemical oxidation polymerization of pyrrole on the surface of sulfur particles was carried out to synthesize a sulfur/polypyrrole （SIPPy） nanocomposite with core-shell structure. The composite was characterized by elemental analysis, X-ray diffraction, scanning/transmission electron microscopy, and electrochemical measurements. XRD and FTIR results showed that sulfur well dispersed in the core-shell structure and PPy structure was successfully obtained via in situ oxidative polymerization of pyrrole on the surface of sulfur particles. TEM observation revealed that PPy was formed and fixed to the surface of sulfur nanoparticle after polymerization, developing a well-defined core-shell structure and the thickness of PPy coating layer was in the range of 20-30 nm. In the composite, PPy worked as a conducting matrix as well as a coating agent, which confined the active materials within the electrode. Consequently, the as prepared SIPPy composite cathode exhibited good cycling and rate performances for rechargeable lithium/sulfur batteries. The resulting cell containing SIPPy composite cathode yields a discharge capacity of 1039 mAh·g^-1 at the initial cycle and retains 59% of this value over 50 cycles at 0.1 C rate. At 1 C rate, the SIPPy composite showed good cycle stability, and the discharge capacity was 475 mAh·g^-1 after 50 cycles.     

Fe_3O_4/P(NaUA-St-BA)核-壳纳米磁性复合粒子的合成与表征

以表面包敷有反应型的表面活性剂NaUA(十一烯酸钠)的Fe3O4磁性胶体粒子为种子,运用无皂乳液聚合方法原位制备出Fe3O4P(NaUAStBA)核壳纳米磁性复合粒子.Fe3O4磁性胶体粒子的粒径为10nm左右.IR和TG结果分析表明,苯乙烯、丙烯酸酯和NaUA在Fe3O4粒子的表面发生了聚合反应,形成P(NaUAStBA);TEM和激光粒度分析仪测试结果显示,Fe3O4P(NaUAStBA)复合粒子具有核壳结构而且粒子分布均匀、平均粒径60nm;TG测试的结果表明,NaUA在Fe3O4粒子的包覆率为13.83%,P(NaUAStBA)共聚物的包覆率71.85%;振动样品磁强仪(VSM)测试的磁滞回线则表明由无皂乳液聚合得到的Fe3O4P(NaUAStBA)复合粒子具有超顺磁性,可避免磁性微球在磁场中的团聚.另外,合成的磁性胶乳可稳定存放数月.     

The polyurethane/polyacrylate soap-free emulsion formation: effects of hydrophilic polyurethane

The vinyl group terminated water-borne polyurethanes (WPU) with different DMPA content were prepared. Subsequently the core-shell polyurethane/polyacrylate (PUA) composite emulsions were synthesized by soap-free emulsion copolymerization. The WPU as sole surfactant was used in copolymerization, and the lowest surface tension could be achieved to 38.8?mN m^?1. Furthermore, the final conversion of acrylic monomer was reached to 98% in the case of WPU reactive seed. The FTIR-ATR indirectly confirmed the core-shell structure of PUA, simultaneously combined with DSC results found that the compatibility of WPU and PA was enhanced by growing grafting efficiency. The TEM results further indicated that the amount of DMPA in WPU had a great significant role in polymerization and final morphology structure. The PUA composite particles changed from scattered structure, core-shell structure to multi-core structure with increasing DMPA content. Correspondingly, the reinforcing and toughening effects were also found in PUA films with the increase content of DMPA by tensile testing.     

Preparation of Polypyrrole/Poly(methyl methacrylate) Core-Shell Nanoparticles in Four-Component Microemulsion Media

Electrically conductive polypyrrole (PPy)/poly(methyl methacrylate) (PMMA) core-shell nanoparticles were synthesized by two-step microemulsion polymerization. PPy core particles were prepared in a four-component microemulsion system, which was formed with surfactant cetyltrimethyl ammonium bromide (CTAB), cosurfactant n-pentanol, water, and pyrrole. Ferric chloride and iodine was added as the oxidant and the dopant, respectively. Then the PPy nanoparticles were coated with PMMA to prepare PPy/PMMA core-shell nanoparticles. The morphology of PPy/PMMA core-shell nanoparticles was characterized with transmission electron microscopy (TEM). Fourier transform infrared (FTIR) spectroscopy was used to characterize the structure of the samples. The electrical conductivities of samples were studied by a Hall effect testing instrument. Despite being coated with a layer of insulation, the conductivity of the composite PPy/PMMA core-shell nanoparticles could still reached to 7.856 × 10^?1 S/cm.     

pH值和前驱体用量对核壳结构PSt/SiO2复合微球结构形态的影响

首先通过无皂乳液聚合法制得表面含羧基、粒径为360 nm的单分散聚苯乙烯(PSt)种子乳液,并在EtOH/H2O混合介质中用γ-氨丙基三乙氧基硅烷(KH-550)对其进行改性,制得表面含有活性硅乙氧基并带有正电荷的改性PSt乳胶粒,然后再加入原硅酸乙酯(TEOS)进行共水解与共缩聚反应,制备出了核壳结构PSt/SiO2...     

Preparation and characterization of silver/TiO2 composite hollow spheres

Silver-coated poly(methyl acrylic acid) (PSA) core-shell colloid particles were prepared by an in situ chemical reduction method. Crystalline silver/titania composite hollow spheres were obtained by coating the as-prepared PSA/silver particles with an amorphous titania layer and subsequently calcining in Ar atmosphere. SEM and TEM investigation indicated that the size of the as-prepared PSA/silver and PSA/silver/TiO(2) core-shell particles and silver/titania composite hollow particles was fairly uniform and the wall thickness of the hollow spheres was in the range of 40-80 nm. UV-vis absorption spectra were recorded to investigate their optical properties.     

核壳结构Beta/MCM-22双微孔复合分子筛的合成与表征

以Beta分子筛为晶核,通过二步水热晶化法成功制备了形态良好的Beta/MCM-22核壳结构复合分子筛。采用X射线衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)及N2吸附-脱附技术等对分子筛进行了表征。结果表明,复合分子筛形态规整,Beta与MCM-22分别作为核壳而共生;Beta/MCM-22复合分子筛孔结构性质介于MCM-22、Beta分子筛之间。在酸性分布上,复合分子筛的中强酸及B酸所占比例显著增加(CB/CL=13.8)。通过Ar-H2等离子体对Beta分子筛进行处理,使其表面能提高并使表面正电荷富集、硅羟基增加,这是形成良好Beta/MCM-22核壳结构的内在原因。     

超声法制备硫化铅/二氧化硅核壳结构亚微米粒子

0 引言 纳米微粒具有的小尺寸效应,表面效应、量子尺寸效应及宏观量子隧道效应等导致纳米粒子的热、磁、光、敏感特性和表面稳定性等不同于常规粒子,这就使得它具有广阔的应用前景.