Electrochemical behaviour of Mn3+/Mn2+, Co3+/Co2+ and Ce4+/Ce4+ redox mediators in methanesulfonic acid

The redox behaviour of Mn³⁺/Mn²⁺, Co³⁺/Co²⁺ and Ce⁴⁺/Ce³⁺ mediators commonly used in indirect oxidation of organic compounds were evaluated in methane sulfonic acid on a glassy carbon working electrode employing cyclic voltammetry. Manganic methanesulfonate exhibits higher instability in dilute methanesulfonic acid. The solid MnO₂ formed during disproportionation on the glassy carbon electrode further affects the reproducibility. Cobaltic methanesulfonate formation occurs only at oxygen evolution region rendering the overall oxidation process less efficient. Ceric methane sulfonate formation is highly efficient over a wide acid concentration range. Ceric methanesulfonate can also be employed over a wide temperature range to oxidize different aromatic compounds.     

邻氨基苯磺酸生产装置技术改造

通过改进生产工艺与设备,提高了装置生产能力和产品质量指标,达到了降本增效的目的。     

Embedding poly(styrene sulfonic acid) into PVDF matrix—a new type of proton electrolyte membrane

Hydrophilic polymer segments, consisting of styrene sulfonic acid (SSA) units, were uniformly embedded into hydrophobic poly(vinylidene fluoride) (PVDF) matrix through the mediation of poly(methyl methacrylate) (PMMA) segments, with which SSA segments form a copolymer. Discrete domains (∼100 nm) assembled by the SSA segments have been identified throughout the matrix of the membrane, which was prepared through blending of the copolymer P(MMA-SSA) and the PVDF. The thermal stability of the SSA was largely boosted in such hydrophobic environment. This unique matrix structure offers proton conductivity of as high as 10⁻³ S/cm at a low SSA equivalent (0.6 mmol -SO₃H/g of membrane), which is accompanied with a low level of water uptake (26%) at ambient temperature. Using this type of polymer membrane as electrolyte, the electrochemical cell possesses obvious capacitive resistance when the membrane is in the anhydride form according to the impedance analysis. However, the capacitive character vanishes when the membrane is hydrated; this response is attributed to the existence of highly dispersed SSA domains in the membrane. This work also analyzes the impedance spectra of the membranes at different hydrated states or with different SSA contents by using an equivalent electrical circuit.     

新型阻垢剂IA-SSS-MA聚合物的合成与表征

以衣康酸(IA)、苯乙烯磺酸钠(SSS)和马来酸酐(MA)为单体,以水为溶剂,过硫酸铵作引发剂,合成了衣康酸-苯乙烯磺酸钠-马来酸酐(IA-SSS-MA)三元聚合物阻垢剂,考察了单体配比、反应温度、引发剂量、滴加时间等对聚合物阻碳酸钙垢效果的影响,结果表明:当单体配比为IA∶SSS∶MA=5∶1∶0.25(摩尔比),反应温度100℃,引发剂量占单体总量13%,滴加时间为5 h,阻碳酸钙垢效果最好,阻垢率达到98.11%。     

丙烯酰胺与2-丙烯酰胺基-2-甲基丙磺酸反相乳液聚合的研究

采用Span-80为乳化剂，白油为分散介质，（NH4）2S2O8-Na2SO3为引发剂，研究了丙烯酰胺（AM）与2-丙烯酰胺基-2-甲基丙磺酸（AMPS）的反相乳液共聚反应，合成出了高相对分子质量的共聚物。讨论了引发剂用量、乳化剂用量、水油比、单体浓度等因素对共聚物相对分子质量的影响。引发剂用量为单体质量的0．2‰，乳化剂为油相的6．7％，水油比为1：1．5，单体浓度为37．5％时可获得高相对分子质量的共聚物，且聚合反应平稳易控制。     

甲烷磺酸电镀Sn-Pb合金添加剂研究

介绍了国内外磺酸型Sn-Pb合金电镀添加剂近十年的研究历程现况并根据各组分的化学结构及其在电镀中所体现出的性质将添加剂分为Sn^2 离子稳定剂、光亮剂及分散剂三类。最后列出了新研制的甲烷磺酸Sn-Pb合金电镀添加剂的主要性能及具体工艺配方。     

杯[4]芳烃磺酸钠催化合成乙酸正丁酯

以杯[4]芳烃磺酸钠为催化剂,以乙酸与正丁醇为原料,通过酯化反应合成乙酸正丁酯,考察了催化剂用量、原料配比和反应时间对酯化反应的影响,产品进行折光指数检测。结果表明,杯[4]芳烃磺酸钠作为催化剂,乙酸物质的量为0.1mol,醇酸物质的量比为1.2,催化剂质量为1g,反应时间为4h时,酯化率可达81.41%,杯[4]芳烃磺酸钠可以重复使用多次。     

C／T iO 2复合材料的制备及光催化性能的研究

采用溶胶-凝胶法制得了C/TiO2复合光催化剂,并采用X射线衍射（XRD）﹑扫描电子显微镜（ SEM ）﹑紫外光谱等方法对复合材料进行了表征。以1-萘胺-4-偶氮对苯磺酸为模型化合物评价了C/TiO2复合材料的光催化性能,考察了降解时间、初始浓度和催化剂投加量等因素对降解率的影响。研究表明,在1-萘胺-4-偶氮对苯磺酸初始浓度为2×10-5 mol/L,催化剂投加量为1．0 g/L时,光催化反应5 h后,1-萘胺-4-偶氮对苯磺酸的降解率达到85．41％。     

两亲性共聚物P(MMA-co-AMPS)对聚偏氟乙烯超滤膜性能的影响

以2-丙烯酰胺基-2-甲基丙磺酸(AMPS)为亲水单体,甲基丙烯酸甲酯(MMA)为疏水单体,偶氮二异丁腈(AIBN)为引发剂,采用自由基共聚合法制得了两亲性共聚物P(AMPS-co-MMA);以两亲性共聚物P(AMPS-co-MMA)与聚偏氟乙烯(PVDF)共混,通过相转变法制备PVDF/P(MMA-co-AMPS)超滤膜。利用傅里叶变换红外光谱、热失重法表征无规共聚物的组成和热稳定性能。并通过扫描电子显微镜,傅里叶变换红外光谱、吸水率测试、表面润湿性测试,探讨了不同单体摩尔比对PVDF/P(MMA-co-AMPS)超滤膜的结构及性能的影响。结果表明,单体AMPS与MMA间发生自由基聚合生成两亲性共聚物P(AMPS-co-MMA)。PVDF/P(MMA-co-AMPS)超滤膜表面多孔,内部有大孔,存在相对致密皮层和多孔的支撑层。当2-丙烯酰胺基-2-甲基丙磺酸和甲基丙烯酸甲酯的摩尔比为2∶1时,PVDF/P(MMA-co-AMPS)超滤膜吸水率和表面润湿性能最好。     

手性樟脑磺酸的合成及表征

以樟脑粉为原料合成了消旋樟脑磺酸;采用l-苯甘氨酸为拆分剂,经拆分、纯化分离得到了手性樟脑磺酸。合成消旋樟脑磺酸的适宜工艺条件为：反应时间25 h,浓硫酸的滴加速度0.5～1.0 mL/min,反应温度10℃,消旋樟脑磺酸的收率85.6%,熔点195～201℃。拆分的适宜工艺条件为：物料比n（dl-樟脑磺酸）∶n（l-苯甘氨酸）=1∶0.95,d-樟脑磺酸拆分收率64%,熔点194～196℃,[α]2D0=＋23°（C=5,H2O）;l-樟脑磺酸拆分收率90.8%,熔点197～198℃,[α]2D0=-22.5°（C=5,H2O）。样品经熔点、旋光率、红外光谱等检测方法,证明与目标产物一致。