三羟甲基丙烷三丙烯酸酯-苯乙烯沉淀聚合高产率制备高交联单分散聚合物微球

以三羟甲基丙烷三丙烯酸酯(TMPTA)-苯乙烯(St)为单体,偶氮二异丁腈(AIBN)为自由基引发剂,通过在乙醇中的沉淀聚合可制得高交联单分散P(TMPTA-St)聚合物微球.对单体转化率,微球以及可溶性低聚物的产率进行了测试.结果表明,使用10 wt%至60 wt%的交联剂TMPTA进行聚合可获得单分散微球,产率在50%左右.增加TMPTA用量可提高微球产率和单体转化率.增加引发剂AIBN用量对提高微球产率也有促进作用,但同时可溶性低聚物产率也增加.向乙醇中加入水作为反应介质结合适当增加AIBN用量可使单体转化率达到98%,微球产率高于90%.对实验结果进行了解释,对聚合机理进行了讨论.     

冰冻人血清中尿酸标准物质复制的定值EI北大核心CSCD

为了满足该标准物质的需求,进行了第二次尿酸血清标准物质的复制。针对复制的尿酸血清标准物质,基于单四极杆质谱的液相色谱-同位素稀释质谱法(LC-IDMS),用乙腈沉淀法去除蛋白质,BEH C18色谱柱和电喷雾离子源负离子模式(ESI^(-)),同位素稀释的单点校准法进行定值、均匀性检验、稳定性检验以及不确定度评定等研究。此定值方法经过CCQM-K109(血清中尿酸分析)国际关键比对进行验证。复制的2种不同浓度水平尿酸(肾病患者和正常人)血清标准物质的定值结果分别为(73.5±1.3)μg/g,(47.5±1.1)μg/g,其均匀性和稳定性评估结果良好。     

无机与有机混合物的含量分析——以探究鼻可乐成分为例

在化学实验课堂上,以生活中常见药品作为实验对象更能激发起学生对化学学习的兴趣。鼻可乐是一种常见的市售洗鼻剂,主要成分为氯化钠、柠檬酸与柠檬酸钠,是一种典型的无机物与有机物的混合体系。本文设计了对鼻可乐的组成进行定量分析的方法,并且通过实验验证其合理性,以期为鼻可乐成分分析实验进入高校分析化学实验课堂提供指导方法。学生通过该实验不仅能掌握恒重坩埚、沉淀滴定等实验基本操作方法,而且能更好地理解定量分析数据的方法。     

Facile synthesis and characterization of β-cobalt hydroxide/hydrohausmannite/ramsdellitee/spertiniite and tenorite/cobalt manganese oxide/manganese oxide as novel nanocomposites for efficient photocatalytic degradation of methylene blue dye

In this paper, our research team has synthesized new nanocomposites by simple precipitation/ignition method and using low-cost chemicals. Hence, β-cobalt hydroxide/hydrohausmannite/ramsdellitee/spertiniite and tenorite/cobalt manganese oxide/manganese oxide new nanocomposites were synthesized by precipitation of Mn(II)/Co(II)/Cu(II) solution using sodium hydroxide and ignition of precipitate at 700 °C for 3 hrs, respectively. The synthesized nanocomposites were characterized using different instruments such as energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), field emission scanning electron microscope (FE-SEM), transmission electron microscope (TEM), nitrogen gas sorption analyzer, and UV–vis spectrophotometer. Energy dispersive X-ray analysis revealed that the nanocomposite formed as a result of precipitation consists of copper, cobalt, manganese, and oxygen where the weight percentages are equal to 31.73, 27.01, 17.26, and 24 %, respectively. Also, the nanocomposite formed as a result of ignition consists of copper, cobalt, manganese, and oxygen where the weight percentages are equal to 31.26, 23.87, 14.56, and 30.31 %, respectively. Transmission electron microscope revealed that the nanocomposites formed as a result of precipitation and ignition consist of polyhedral and spherical shapes with an average diameter of 34.50 and 28.56 nm, respectively. The synthesized nanocomposites were used as new photocatalysts for the efficient degradation of methylene blue dye. 0.05 g of the synthesized nanocomposites degrade 100 % of 50 mL of 15 mg/L of methylene blue dye solution within 25 min in the presence of H₂O₂ under UV light.     

Copolymeric nano/microgels of N-isopropylacrylamide and carboxyalkyl methacrylamides: Effect of methylene chains and the ionization state of the weak acids on size and sensitivity to pH and temperature

ABSTRACT

We prepared nano/microgels by precipitation copolymerization of N-isopropylacrylamide (NIPAAm), and one of three different carboxyalkyl methacrylamides [methacryloylamido hexanoic acid (M₅), 8-methacryloylamido octanoic acid (M₇), and 11-methacryloylamido undecanoic acid (M₁₀)], either in the acid forms or as carboxylates (potassium salts). The hydrodynamic diameter (Dh) of the nano/microgels prepared with the carboxylates was smaller (≈100 nm for M₁₀ copolymers), compared to the size of homopolymeric NIPAAm microgels prepared by dispersion polymerization (around 600 nm), indicating that the carboxylates act as surfactants reducing the size of the seeds during the polymerization process. These materials presented a swollen-shrunken transition temperature (T _tr) similar to the T _tr of the homopolymeric NIPAAm microgels, without pH sensitivity. On the other hand, the copolymeric microgels prepared from the acid form of the comonomers have a similar or bigger size than NIPAAm microgels. For these copolymers, the T _tr can be tuned by the type and proportion of acid comonomer used and present pH sensitivity. This is important for biomedical applications such as positive temperature control release. Polyelectrolyte titration demonstrates that the nano/microgels prepared with the carboxylates behave as hard spheres, while the microgels prepared with the weak acid behave as porous materials.     

Improved performance of porous LiFePO4/C as lithium battery cathode processed by high energy milling comparison with conventional ball milling

Porous LiFePO₄ is synthesized and coated with amorphous carbon by using high energy nano-mill (HENM) processed solid-state reaction method. FeCl₃ (38%) containing water solution which is originated from pickling of steel scrap (waste liquid) is used as a source material in this study. The result indicates that LiFePO₄ powders are well coated with the amorphous carbon. HENM process successfully produces the porous LiFePO₄ with homogeneously distributed pores and a well networked carbon web, which delivers an enhanced electrochemical rate capability. HENM process is incorporated as an effective route for reducing particle size, distributing particle homogeneously and averting agglomeration of particles of precursor in this study. X-ray diffraction, scanning electron microscopy with elemental mapping, transmission electron microscopy with selected area (electron) diffraction, Raman spectroscopy, cyclic voltammetry, and galvanostatic charge/discharge are employed to characterize the final product. Electrochemical measurement shows that the synthesized LiFePO₄/C composite cathode delivers an initial discharge capacity of 161 mAhg⁻¹ at 0.1C-rate between 4.2 and 2.5 V. Remarkably, the cathode delivers 101.9 mAhg⁻¹ at high charge/discharge rate (10 C).     

原位沉析法制备磁性氧化铁羟基磷灰石/壳聚糖棒材

首先通过化学沉淀法制备磁性氧化铁羟基磷灰石(Fe3O4/HA),然后以壳聚糖(CS)为基体,利用原位沉析法将Fe3O4/HA与CS复合,制得磁性Fe3O4/HA/CS复合材料.经XRD、粒径分布和PPMS测试,结果表明了Fe3O4/HA复合物的生成.系统研究了磁性Fe3O4/HA/CS棒材力学性能的影响因素,最终确定Fe3O4与HA质量比为3∶17,磁性Fe3O4/HA与CS质量比为9∶91时,棒材的力学性能最优,弯曲强度可达到87.0 MPa,弯曲模量1.57 GPa.     

沉淀法制备EPDM-g-MAH/CaCO_3复合材料及其性能的表征

提供了三元乙丙橡胶(EPDM)交联的一种方法.以二甲苯为溶剂,溶液法制备马来酸酐(MAH)接枝EPDM,然后向溶液中加入适量碳酸钙(CaCO3),与已接枝的马来酸酐(MAH)反应.待反应完全后,滴加丙酮作为沉淀剂,沉淀物真空干燥,制得EPDM-g-MAH/CaCO3弹性体复合材料.溶解、溶胀及拉伸性能测试结果表明,复合材料样品已形成有效的交联,且材料的抗张强度、断裂伸长率和模量均得到较大幅度的提高,当CaCO3含量达到体系总重的20%时,复合材料呈现最佳力学性能.上述实验结果是因为碱性的CaCO3的Ca2+可以与接枝在EPDM上的MAH发生配合反应,进而成为EPDM的交联中心,形成有效交联,从而促进了EPDM机械性能的提高,ATR-FTIR和TGA的测试结果被用于证实上述观点.     

乙酸中沉淀聚合制备窄分散聚二乙烯基苯微球

在沉淀聚合中利用含无毒的乙酸溶剂合成出窄分散交联聚二乙烯基苯(PDVB-55)微球,用扫描电镜(SEM)对其表面形态和粒度进行了表征,结果显示PDVB-55微球均匀且互相分离,平均粒径是2.69μm.X射线光电能谱(XPS)分析表面化学组成显示,微球表面有大量残余双键.     

花椰菜状碳酸钙的"一步法"制备及表征

以碱土金属锶的硝酸盐为添加剂, 采用“一步法”制备了大小均一、 分散性良好的花椰菜状碳酸钙粒子. 考察了反应温度、 反应时间等因素对碳酸钙结晶行为的影响, 确定了最佳反应条件. 利用扫描电子显微镜(SEM)、 X射线衍射仪(XRD)、 X射线能谱仪(EDAX)等对所得产物的结构和性能进行了表征, 并探讨了其反应原理.