甲磺酸铜催化合成草酸二异戊酯

制备了甲磺酸铜催化剂,对其结构进行了IR和热重分析,并用于催化草酸和异戊醇的酯化反应。结果表明,甲磺酸铜具有催化活性高、稳定,易分离,重复使用性能优良,对环境友好的特点。最佳酯化工艺条件为:n(异戊醇):n(草酸)=2．8:1,w(甲磺酸铜)=0．3％,以过量的异戊醇为带水剂,回流反应2．0 h,酯化率可达到96．8％。     

甲基磺酸镧催化缩醛化反应性能的研究

以正辛醛和乙二醇为原料,甲基磺酸镧为催化剂,合成了正辛醛缩乙二醇。采用正交实验法考察了影响收率的因素。其最优条件为,正辛醛∶乙二醇∶催化剂∶带水剂为1m o l∶1.2m o l∶7.5g∶75mL,反应在回流温度下进行,反应时间3.0h,收率可达87.2%。用此方法合成了其它三种缩醛,同样获得满意结果。证明甲基磺酸镧对缩醛化反应具有较高的催化活性。     

Cation Effect on the Binary and Ternary Phase Behaviors of Double-Tailed Methanesulfonate Amphiphiles

A series of symmetrical dialkyl methanesulfonate amphiphiles [DiC _n CHSO ₃ ] _m M (n = 6, 7, 8) with different counter cations (M^m+ = H⁺, Li⁺, Na⁺, K⁺, Cu²⁺, Zn²⁺, Mg²⁺, Ca²⁺, Sc³⁺) were synthesized in five steps. Their solubility and critical micelle concentration (CMC) in water were determined highlighting a huge effect of the chain length and the nature of the cation. The hydrophilic–lipophilic balance of the surfactants were assessed with the phase inversion temperature (PIT)-slope method based on the deviation from the PIT of the reference C₁₀E₄/n-octane/0.01 M NaCl_(aq) emulsion through addition of increasing amounts of the dialkyl methanesulfonates. The hydrophilicity of the surfactants was thus ranked in terms of dPIT/dx_sulfonate. A “cation” scan with the [DiC ₆ CHSO ₃ ] _m M /benzene/water systems at f_w = 0.5 was finally performed confirming the hydrophilicity ranking obtained with the PIT-slope method. It revealed that the [DiC ₆ CHSO ₃ ] ₂ Mg behaves as a “Balanced Surfactant” able to form spontaneously a three-phase microemulsion system (Winsor III) just in the presence of water and oil, in the same way as the catalytic surfactant dimethyldioctylammonium molybdate, which has the same PIT-slope.     

取代2-四氢萘酮的一步合成新方法研究

本文介绍了一步法制备取代2-四氢萘酮的新方法,与常规合成方法相比,该法具有明显的优点:不需要先将羧酸转化成酰氯,避免了三氯化铝以及含氯溶剂的应用,并使催化剂得以循环利用。因此,该方法安全、环保,有望取代常规的付-克反应在工业上的应用。     

高纯度甲基磺酸亚锡生产新工艺

研究了用锡和甲基磺酸反应直接生产电镀用的纯甲基磺酸亚锡的新工艺，其产品纯度达到99．5％以上，并研究了提高设备利用率和生产效率的措施，设备利用率可提高2．28倍，建成的150t/a甲基磺酸亚锡生产装置，其产品产量、质量均达到了预期效果。该工艺无毒无害无三废排放。     

隔膜电解法合成电镀级甲基磺酸亚锡

研究了隔膜电解法合成甲基磺酸亚锡的工艺。考察了电流密度、阴极酸质量浓度、阳极酸质量浓度、稳定剂的加入量、浓缩温度等因素对产品的影响。在电流密度1.8 A/dm2、常温反应60 h,阴极酸质量浓度180 g/L、阳极酸质量浓度180 g/L、浓缩温度80℃以下的条件下,锡的直收率92%以上,电流效率95%以上。     

甲基磺酸盐体系电镀铅–锡–铜合金工艺

研究了甲基磺酸盐体系电镀Pb–Sn–Cu三元合金工艺参数对镀层成分和外观的影响,确定了最佳的工艺条件:Pb2+95~105g/L,Sn2+9~13g/L,Cu2+2~3g/L,甲基磺酸140g/L,添加剂A3~5g/L,添加剂B6~7g/L,电流密度2.5A/dm2,温度19~23°C。在此工艺下以不锈钢片为基材镀Pb–Sn–Cu合金45min,所得镀层色泽均匀,结晶细致,膜层厚度为11.2μm,镀层中Sn含量为7.44%~7.52%,Cu含量为2.19%~2.26%,符合Pb–Sn–Cu三元合金镀层成分的要求。     

食用香料柠檬醛缩1,2-丙二醇的新法合成

以柠檬醛和1,2-丙二醇为原料,甲基磺酸铜为催化剂,合成了柠檬醛缩1,2-丙二醇。考察了影响收率的因素。其最优条件为:柠檬醛∶1,2-丙二醇:催化剂∶带水剂为1mol:1.4mol∶24mmol∶100mL,反应在回流温度下进行,反应时间2.0h。收率可达88.6%。     

Anodic behavior of gold in 1-butyl-3-methylimidazolium methanesulfonate ionic liquid with chloride anion

The anodic behavior of gold has been investigated in presence of chloride and/or water in 1-butyl-3-methylimidazolium methanesulfonate (BMI CH₃SO₃) ionic liquid (IL). The cyclic voltammetry (CVs) in presence of chloride ions shows two waves attributed to the oxidation of the gold electrode which occurs under two steps: the first one is attributed to the electrochemical dissolution of gold into to gold(I), while the second one is attributed to an overlap of the chloride oxidation step as well as the oxidation of Au(I) to Au(III). Furthermore the determination of water and chloride content in IL allowed observing that the passive layer induced by water could be removed under chloride. Thanks to those results we were able to clarify the conditions of gold recovering in this kind of electrolyte.     

甲烷磺酸铝催化合成氯乙酸酯的性能研究

合成了甲烷磺酸铝,用热重和红外对其进行表征。并以甲烷磺酸铝为催化剂,研究其催化氯乙酸与异丙醇酯化反应中各种因素对酯化率的影响。反应条件为:醇酸摩尔比1.2∶1,催化剂摩尔分数1.0%(以酸的摩尔数计),反应时间2.5h,反应温度80～85℃,环己烷5mL作为带水剂,酯化率可达96.8%,反应后催化剂经过简单的相分离就可重复使用。与AlCl3·6H2O、Al2(SO4)3·18H2O及其它Lewis酸进行比较,甲烷磺酸铝的催化活性最好。用甲烷磺酸铝作催化剂合成其它氯乙酸酯,酯化率均在96.0%以上。