三直链烷基苯磺酸钠的合成及其表面活性的研究

为了研究三直链烷基苯磺酸钠的分子结构与表面活性之间的关系,以对二氯苯为原料,经交叉耦合反应、傅-克酰基化反应、黄鸣龙还原反应、磺化反应以及中和反应等步骤,合成了5种不同烷基链长的三直链烷基苯磺酸钠,产物的收率为45%~53%,用两相滴定法测定产物的纯度均大于99.5%,并用核磁共振氢谱和碳谱对产物进行了结构鉴定。用Wilhelmy-Plate法测定了三直链烷基苯磺酸钠水溶液的表面性质,发现直链烷基苯磺酸钠疏水链碳数增加,临界胶束浓度CMC减小;相同疏水碳原子的化合物,短侧链碳数少的化合物CMC低;长侧链碳数保持不变,两个短侧链碳数由4个增加至8个,临界胶束浓度下的表面张力γcmc由32.44mN/m降低至28.97mN/m;而短侧链碳数保持不变,长侧链碳数由7个增加至11个,γcmc变化不明显。     

长链烷基苯磺酸钠Gemini表面活性剂的合成和表面活性

以脂肪酸、苯酚、乙二醇为原料,经酰化反应、酯化反应、Fries重排、氢化还原反应、磺化以及中和反应等步骤,合成出3种长链烷基苯磺酸钠Gem in i表面活性剂。用IR、1HNMR和ESI-MS对产物进行了结构鉴定。以W ilhelmy-p late法测定了30℃时它们在水溶液中的临界胶束浓度(CMC)和临界胶束浓度下的表面张力(γCMC)。纯水溶液中其临界胶束浓度(CMC)为10-4~10-5mol/L,γCMC为35~37 mN/m;随着苯环上长链烷基碳数(n=8、10、12)的增加,CMC分别为5.94×10-4、1.53×10-5、0.46×10-5mol/L;γCMC分别为36.9、34.4、34.4 mN/m。结果表明,此类表面活性剂具有比较好的表面活性。     

食品接触材料中全氟烷基磺酸类化合物的HPLC-MS/MS测定

研究食品接触材料中全氟烷基磺酸类化合物的检测方法和该类化合物的残留水平。样品采用甲醇超声提取,液相色谱-质谱联用测定,以C18为分离柱,甲醇-5mmol/L乙酸铵溶液为梯度洗脱淋洗液,同位素内标法定量,内标物为13C标记的PFOS。该方法的检出限为0.5μg/kg,线性范围为0.5～10μg/kg,方法的平均回收率为91.1%～112.8%。结果证明,该方法准确、快速,可成功应用于16种食品接触材料实样的检测。     

SiW12/NaY固体杂多酸催化剂的微波合成及LAS降解性能研究

以微波辐射方法合成了NaY分子筛、二氧化锆和二氧化钛不同载体负载磷钨酸、磷钼酸、硅钨酸不同杂多酸的固体酸催化剂,用Hammett指示剂与紫外光谱相结合的方法测定固体杂多酸催化剂的酸度,发现SiW12/NaY酸性最强。单因子实验研究了制备条件对SiW12/NaY固体酸催化剂酸活性的影响,正交试验探讨了影响SiW12/NaY固载杂多酸活性四个因素的大小顺序为:烧结时间>烧结功率>浸泡浓度>浸泡时间,催化剂制备的优化条件为:硅钨酸水溶液浓度0.10 mol/L,浸泡时间30 h,微波功率750 W,烧结时间40 min,制得的催化剂酸度最高。应用0.050 g SiW12/NaY固载硅钨酸催化剂降解150 mg/L,pH值为3的十二烷基苯磺酸钠(LAS)溶液60 min,LAS降解率由76%提高到94.5%。固载硅钨酸催化剂对LAS的降解率明显提高。     

适用于高矿化度油藏的醇（酚）聚氧烯基醚磺酸盐合成进展

醇（酚）聚氧烯基醚磺酸盐具有优良的耐盐、耐高温水解、HLB值可调及配伍性能,在高矿化度油藏开采领域具有广泛的应用潜力。本文介绍了几种常见醇（酚）聚氧烯基醚磺酸盐表面活性剂的结构,分析了其在高矿化度、高二价离子油藏中的作用特征,综述了亚硫酸盐磺化工艺、磺烷基化工艺和硫酸酯基团转化等磺化工艺,并从原料性能、收率、反应路线及工艺流程等角度对各工艺进行了分析比较,总结了各工艺路线的优、缺点,指出如能对基团转化过程中的水解程度加以控制,以脂肪醇聚氧乙烯醚硫酸钠为原料的硫酸酯基团转化工艺具有较好的工业应用前景。     

纺织品中全氟辛烷磺酸及全氟辛酸的测定及其研究进展

全氟辛烷磺酸(PFOS)和全氟辛酸(PFOA)等化合物是应用广泛但对环境有持久污染的有机物.开展纺织品中PFOS和PFOA检测方法的研究是保护环境和人类健康,提升纺织产品质量的迫切要求.简述了PFOS和PFOA的各种检测方法和复杂样品的前处理技术,指出应研究有关纺织品中PFOS和PFOA快速、精确的测定方法,并尽快建立...     

Synthesis and Characterization of Novel Aryl Alkyl Sulfonates Based on Nonylphenol

A series of nonylphenol-substituted alkyl sulfonates (C _x NPAS, x = 8, 10, 12, 14, 16) with two hydrocarbon chains and two different hydrophilic groups has been synthesized from α-olefins and nonylphenol. The respective products have a “pseudo-gemini” surfactant structure. The structures of the C _x NPAS have been characterized by IR, UV, ¹H nuclear magnetic resonance, electrospray ionization mass spectrometry, and elemental analysis. The effects of carbon chain length of the obtained surfactants on properties such as the critical micelle concentrations (CMC) in aqueous solutions, surface tension at the CMC (γ _CMC), and efficiency of adsorption at the water/air interface (pC ₂₀) have been determined. The γ _CMC of the surfactants first decreased and then increased with increasing length of the carbon chain x, and reached a minimum of 29.25 mN/m at x = 10, which is much lower than that of α-olefin sulfonate (AOS) (33.52 mN/m). The CMC decreased and pC ₂₀ increased with increasing x. The introduction of the hydroxyl group is responsible for multiple molecular conformations at the water/air interface and leads to a greater molecular area A _min and smaller Γ_max than those of AOS.     

LC-MS/MS法测定清洗剂中全氟辛磺酸类物质总量

样品采用液液分配经甲醇提取,提取液经浓缩定容后,用液相色谱-质谱/质谱仪采用多反应监测(MRM)进行检测。通过PFOS类物质共有的特征离子作为检测目标离子进行定性,外标法测定PFOS类物质的总含量。PFOS标液在0.01~1.0μg/mL范围内浓度与响应值有良好的线性关系。方法的检测低限是0.01 mg/kg,回收率为76.5%~110.0%,相对标准偏差为5.69%~15.75%。     

Photocatalytic degradation of aromatic sulfonates present in industrial percolates

Photocatalytic treatment in the presence of aqueous TiO₂ suspensions was applied to an aqueous percolate containing various hydrophilic aromatic pollutants, in particular naphthalene sulfonates. A preliminary feasibility study was accomplished on standards of pure compounds, for which a degradation rate trend inversely proportional to the sulfonation degree was found, demonstrating the important role played by the substrate adsorption on semiconductor particles. The evolution of primary processes, the abatement of TOC and the release of sulfate were monitored. Further experiments performed on samples of percolates taken from an abandoned industrial site demonstrated the suitability of photocatalysis for the effective destruction and mineralization of the investigated contaminants in these complex matrices after a few hours irradiation.     

Bismuth(III) Bromide‐Catalysed Substitution of Benzyl Alcohols with Arylsulfonylmethyl Isocyanides: An Unexpected Access to Sulfinates

A bismuth(III) bromide‐catalysed direct substitution of benzyl alcohols with arylsulfonylmethyl isocyanides affords sulfinates under mild acidic conditions. An unforeseen reversed reactivity was observed in this highly selective formation of sulfinates instead of the formation of the usually favoured sulfones. Cytotoxicity tests (in vitro) indicated that the sulfinates exhibit antibiotic activity against a human leukaemia cell line HL‐60, which would widen the structural diversity of this antitumour target and confirm the perspectives of further investigations.