柠檬酸铋合成新工艺研究

针对现有柠檬酸铋制备工艺合成时间长、能耗高、产品纯度不高等不足,介绍了一种常温下制备柠檬酸铋的新工艺。新工艺制备时间短,制备的柠檬酸铋产品质量好,合成过程产生的废水可循环利用,废气经碱液循环吸收可生产硝酸钠副产品。     

Physicochemical investigation of the decomposition products of ammonium metal carboxylates: ammonium ferric citrate hydrate

The thermal decomposition up to 400 °C of ammonium ferric citrate hydrate, of unknown structure and formula weight, was studied by thermogravimetry, differential thermal analysis, infrared (IR) spectroscopy and X-ray diffractometry. The possible identities of the formula weight and the intermediate products of calcination are discussed. The results revealed that the parent material is amorphous and contains two moles of water and two moles of ammonia. Decomposition takes place via six weight-loss processes, three endothermic (90–230 °C) and three exothermic (240–298 °C), leading eventually to the formation of Fe₂O₃. The intermediate solid products are mainly unstable amorphous oxycarbonates, as indicated by X-ray and IR spectroscopies. The gas-phase decomposition products identified by IR spectroscopy are NH₃, CO₂, CO, CH₃COCH₃, CH₄ and NH₄OH. Surface area measurement and scanning electron microscopy showed that Fe₂O₃, the final product at 400 °C, hada surface area of 40 m²/g and good crystalline and porous character.     

柠檬酸三丁酯、乙酰柠檬酸三丁酯的合成进展

概述了柠檬酸酯增塑剂中两个主要品种柠檬酸三丁酯和乙酰柠檬酸三丁酯的催化合成进展。介绍了固体超强酸、稀土固体酸,杂多酸等催化剂的催化效果和特点。指出高效,无毒,无公害的催化剂的是今后研究的重点。     

蒙脱土负载［C14mim］+有机阳离子催化合成柠檬酸三丁酯

通过咪唑基离子液体和蒙脱土在甲苯溶液中的离子交换反应，将热稳定性高的咪唑基有机阳离子［C₁₄mim］⁺交换吸附进入蒙脱土片层间，制备了蒙脱土负载的有机阳离子固体催化剂［C₁₄mim］⁺/MMT。利用XRD和TGA对催化剂的结构与性能进行了表征和测定，研究了蒙脱土负载有机阳离子固体催化剂的催化性能，初步考察了其稳定性及再次使用效率。研究结果表明，［C₁₄mim］⁺/MMT在合成无毒增塑剂柠檬酸三丁酯的酯化反应中表现出较高的催化活性，可循环使用。与未负载的C₁₄mimBF₄相比，［C₁₄mim］⁺/MMT具有催化活性高、稳定性好和易分离的特点。     

煅烧温度对多组分SrFe_(0.5)CoO_(3-δ)氧化物结构的影响(英文)

采用柠檬酸法合成了多组分的SrFe_(0.5)CoO_(3-δ)氧化物,并分析了锻烧温度对样品结构的影响。实验结果显示不同锻烧温度后所得样品主要由钙钛矿结构的SrFe_(0.5)Co_(0.5)O_3构成,随着锻烧温度的降低,样品的杂相减少,而钙钛矿结构的SrFe_(0.5)Co_(0.5)O_3相衍射峰的强度也有所降低,锻烧温度为1200℃时所得样品由高纯钙钛矿结构的SrFe_(0.5)Co_(0.5)O_3晶相构成。随着锻烧温度的降低,无规则形态结构样品的粒子尺寸随之降低。     

Electrolyte composition and removal mechanism of Cu electrochemical mechanical polishing

The optimization of electrolytes and the material removal mechanisms for Cu electrochemical mechanical planarization （ECMP） at different pH values including 5-methyl-1H-benzotriazole （TTA）, hydroxyethylidenediphosphoric acid （HEDP）, and tribasic ammonium citrate （TAC） were investigated by electrochemical techniques, X-ray photoelectron spectrometer （XPS） analysis, nano-scratch tests, AFM measurements, and polishing of Cu-coated blanket wafers. The experimental results show that the planarization efficiency and the surface quality after ECMP obtained in alkali-based solutions are superior to that in acidic-based solutions, especially at pH=8. The optimal electrolyte compositions （mass fraction） are 6% HEDP, 0.3% TTA and 3% TAC at pH=8. The main factor affecting the thickness of the oxide layer formed during ECMP process is the applied potential. The soft layer formation is a major mechanism for electrochemical enhanced mechanical abrasion. The surface topography evolution before and after electrochemical polishing （ECP） illustrates the mechanism of mechanical abrasion accelerating electrochemical dissolution, that is, the residual stress caused by the mechanical wear enhances the electrochemical dissolution rate. This understanding is beneficial for optimization of ECMP processes.     

Adherence rates to ferric citrate as compared to active control in patients with end stage kidney disease on dialysis

Introduction: Oral phosphate binders are the main stay of treatment of hyperphosphatemia. Adherence rates to ferric citrate, a recently approved phosphate binder, are unknown. Methods: We conducted a post‐hoc analysis to evaluate whether adherence rates were different for ferric citrate vs. active control in 412 subjects with end stage kidney disease (ESKD) who were randomized to ferric citrate vs. active control (sevelamer carbonate and/or calcium acetate). Adherence was defined as percent of actual number of pills taken to total number of pills prescribed. Findings: There were no significant differences in baseline characteristics including gender, race/ethnicity, and age between the ferric citrate and active control groups. Baseline phosphorus, calcium, and parathyroid hormone levels were similar. Mean (SD) adherence was 81.4% (17.4) and 81.7% (15.9) in the ferric citrate and active control groups, respectively (P = 0.88). Adherence remained similar between both groups after adjusting for gender, race/ethnicity, age, cardiovascular disease (CVD), and diabetic nephropathy (mean [95% CI]: 81.4% [78.2, 84.6] and 81.5% [77.7, 85.2] for ferric citrate and active control, respectively). Gender, race/ethnicity, age, and diagnosis of diabetic nephropathy did not influence adherence to the prescribed phosphate binder. Subjects with CVD had lower adherence rates to phosphate binder; this was significant only in the active control group. Discussion: Adherence rates to the phosphate binder, ferric citrate, were similar to adherence rates to active control. Similar adherence rates to ferric citrate are notable since tolerance to active control was an entry criteria and the study was open label. Gender, race/ethnicity, nor age influenced adherence.     

柠檬酸根对纳米Fe_3O_4/PVA磁性复合膜性能的影响

采用化学共沉淀法制备了添加柠檬酸根前后的纳米Fe_3O_4粉体材料,用流延成膜法制备了添加柠檬酸根前后的Fe_3O_4/聚乙烯醇(PVA)复合膜。用红外光谱分析仪、古埃磁天平法、振动样品磁强计、自制磁致变形设备、发射扫描电子显微镜对添加柠檬酸根前后的纳米Fe_3O_4/PVA复合膜的结构及性能进行了表征和分析。结果表明:添加柠檬酸根纳米Fe_3O_4制备的Fe_3O_4/PVA复合膜磁化率更大、磁性能更好、磁致变形性能更大、分散性好。     

Liquid–liquid equilibria of aqueous two-phase systems composed of TritonX-100 and sodium citrate or magnesium sulfate salts

Liquid–liquid phase diagrams of surfactant-based aqueous two-phase systems (ATPS) composed of TritonX-100, as a non-ionic surfactant, and two different salts have been studied at 298.15 K. The salts used were an inorganic salt, magnesium sulfate (MgSO₄), and an organic salt, sodium citrate (Na₃C₆H₅O₇). The results show that the salt MgSO₄ is more capable of inducing ATPS formation than the salt Na₃C₆H₅O₇. The experimental liquid–liquid equilibrium data were correlated using a modified virial model. Good agreement was obtained with the experimental data.     

Fe(Ⅲ)-过氧化氢-亚硝酸盐催化BSA蛋白硝化的影响研究

采用分光光度法研究了不同pH Hepes缓冲液中Fe(Ⅲ)-过氧化氢-亚硝酸盐催化牛血清白蛋白(BSA)发生蛋白质硝化的情况.实验结果表明:在Hepes缓冲液中,EDTA-Fe(Ⅲ)及柠檬酸铁均能够催化过氧化氢-亚硝酸盐引起BSA的硝化.在EDTA-Fe(Ⅲ)-过氧化氢-亚硝酸盐体系中,BSA的硝化程度随pH的升高而依次增强,亚硝酸盐含量随pH值的升高而降低,说明碱性环境有利于EDTA-Fe(Ⅲ)-过氧化氢-亚硝酸盐催化BSA发生蛋白质硝化;而在柠檬酸铁-过氧化氢-亚硝酸盐体系中,BSA的硝化程度随pH的升高而依次降低,亚硝酸盐含量随pH值的升高而升高,说明酸性环境有利于柠檬酸铁-过氧化氢-亚硝酸盐催化BSA发生蛋白质硝化.进一步研究表明:EDTA-Fe(Ⅲ)催化过氧化氢-亚硝酸盐发生蛋白质硝化作用强于柠檬酸铁.