微波辅助合成3,4-二氨基苯甲酸

以对氨基苯甲酸为原料,在微波辐射下经乙酰化、硝化、水解及还原反应制得3,4-二氨基苯甲酸(Ⅰ),总收率为67．6%(未用微波辐射时为40．7%),反应时间由6 h缩短为1 h,并探讨了合成条件。在n(p- H2NC6H4COOH):n(Ac2O)=1:2,微波功率800 w的条件下,回流5 min,对乙酰胺基苯甲酸(Ⅱ)的收率为93．8%;n(Ⅱ):n(Ac2O)=1:2,使用过量乙酸酐,在冰水浴中滴完浓硝酸后,在微波功率800 W,回流3 min后,4-乙酰氨基-3-硝基苯甲酸(Ⅲ)的收率为85．3%;在微波功率800 W条件下,Ⅲ与过量的w(KOH)= 50%乙醇溶液,回流5 min,3-硝基-4-氨基苯甲酸(Ⅳ)的收率为93．1%;在Ⅳ的乙醇溶液中,在回流温度下滴加w[(NH4)2S]=9%硫化铵溶液,然后,在微波功率800 W条件下,回流5 min,可得90．8%的目标产物Ⅰ。用IR、1H NMR对化合物Ⅰ～Ⅳ进行了表征。     

甲醇气相羰化合成醋酸甲酯的产物分析

以热导池为检测器,分别采用8/100间苯二甲酸+GDX-103、Porapak-Q分析甲醇气相羰化的液相产物和气相产物,确定了气相色谱分析的操作条件,测定了各组分的校正因子,并应用于甲醇绿色羰化合成醋酸甲酯的催化剂评选,得到了满意的结果。     

Fabrication and frequency response of a complex ultrasonic transducer for multilayer evaluation

To characterize the thickness of a corrosive fluid system's coated facilities, such as pipes, tubes, tanks, and structural members, a complex ultrasonic transducer capable of measuring multilayered parts was fabricated and the time and frequency responses were evaluated. The target transducer was constructed with two active dual elements made from tape-cast PbNb₂O₆ sheets and an additional thin-film active element made from sol–gel spin-coated Pb(Zr_0.52Ti_0.48)O₃ films. After adjusting the properties of each active element, a complex transducer was assembled after matching the impedance of each element and considering the minimal interference between the active layers. The impulse response of the assembled complex transducer shows excellent characteristics. Moreover, the assembled transducer's capability of accurately measuring the thickness assures that it can be directly applied to related industries.     

Effect of chemical phosphorylation on solubility of buffalo milk proteins

Buffalo milk proteins (casein, co-precipitate or whey protein concentrate) were phosphorylated with phosphorus oxychloride (POCl₃) at three different pH values (5.0, 7.0 and 9.0). The solubilities of phosphorylated milk proteins were examined over the pH range 3.0–9.0 in water and ionic (0.1 m NaCl or 10–70 mm Ca²⁺) systems. The solubilities of buffalo milk proteins decreased at pH 3.0, while there was an increase in the solubilities of casein and co-precipitate near their isoelectric points upon phosphorylation. Solubilities of these phosphorylated milk proteins were pH dependent in 0.1 m NaCl but there was a decrease in their solubilities with increase in calcium ion concentration. This alteration could be due to the shifting of isoionic points of phosphorylated buffalo milk proteins towards acidic pH.     

玻璃微珠的表面化学镀银及红外辐射性能研究

采用化学镀方法在玻璃微珠表面镀银,考察了预处理条件、反应温度和反应时间等因素对玻璃微珠表面镀银的影响,并通过扫描电镜和X-射线衍射分析仪,对镀银后玻璃微珠的表面形貌和结构进行了观察和表征。将镀银玻璃微珠用于涂料中,考察了玻璃微珠在涂料中的应用及其红外辐射率的变化,探讨了化学镀条件对涂料红外辐射率的影响,结果表明,在控制反应温度和浓度的条件下,可使镀银玻璃微珠的红外辐射率由原来的1.02降为0.70,将其应用于涂料后,涂层的红外辐射率为0.80。     

羧酸系列集油剂的水面集油性能

研究了十二烷酸、十四烷酸、十六烷酸和十八烷酸在淡水中的集油能力。结果表明，这4种羧酸在淡水表面的表面膜压随其分子中碳数的增加而增大。其中后两者的表面膜压高达45～50mN／m，显著高于各类油膜膜压，满足集油剂对表面活性物质膜压的要求。4种脂肪羧酸在淡水中使柴油油膜的收缩率在1min时达到最大值，分别为80．0％、81．8％、83．8％和88．2％。它们的己醇、正庚醇、正辛醇、仲辛醇溶液的集油持续性，总体上随羧酸分子碳数增加而增大。其中十六烷酸和十八烷酸集油能力非常接近，它们的正庚醇、正辛醇和仲辛醇溶液使柴油膜面积收缩率在120h后仍保持在66．0％～70．2％。该类集油剂毒性低，易为生物降解，有实际应用前景。     

11B and 15N solid state NMR investigation of a boron nitride preceramic polymer prepared by ammonolysis of borazine

A poly(aminoborazine), precursor for hexagonal boron nitride (h-BN) obtained by reaction of borazine B₃N₃H₆ with ammonia, and its pyrolysis derivatives have been extensively characterised by ¹⁵N and ¹¹B MAS NMR. The various B and N sites have been identified according to their first neighbouring atoms, as well as to the second ones in the case of ¹⁵N, and have also been quantified. This study demonstrates that a suitable choice of NMR techniques together with the use of isotopic enrichment can lead to a large improvement in spectral resolution, which allows a better understanding of such complex BN preceramic polymer structures and permits to follow the polymer-to-ceramic transformation.     

Comparison of Lactic Acid Productivities at High Substrate Conversions in a Continuous Two-stage Fermenter With Cell Recycle Using Different Kinetic Models

The steady-state performance of a two-stage recycle fermenter with two different types (I and II) of configurations for staging was investigated numerically for the continuous production of lactic acid. In Type I the bleed broth withdrawn from the first stage is supplied to the second fermenter, and in Type II both filtrate and bleed broth from the first stage are introduced to the second stage. Using four different kinetic models taken from the literature, the effects of operating parameters on the overall lactic acid productivities and the overall substrate conversions are examined. At moderate conversions, productivities for Type I operation are found to be higher than those for Type II and for the single-stage system. In the case of high conversions close to complete consumption, Type II operation is more efficient than the Type I and single-stage systems. For 99% conversion and 40 kg m^-3 substrate feed concentration, productivities for Type II are predicted to be 14-74% higher compared to those for the single-stage system at the same bleed ratios.     

Ni catalyst promotion of a Cis-selective Pd catalyst for canola oil hydrogenation

A Ni catalyst was added to a cis-selective Pd catalyst in an attempt to further improve the Pd catalyst's cis-selectivity and activity for canola oil hydrogenation. The system was tested under reaction conditions known to be suitable for cis-selective hydrogenation with the Pd catalyst (50 ppm Pd, 70 °C, and 5.2 MPa). Although inactive on its own under these conditions, the addition of 100 ppm Ni increased the hydrogenation activity (from 2.12 to 2.49 10⁻² min⁻¹). Further addition of Ni up to 1000 ppm resulted in no further improvements in activity. The trans isomer contents of the oils hydrogenated with Pd and the Pd/Ni systems were similar. The level of conjugated dienes decreased rapidly during hydrogenation with both Pd alone and with the Pd/Ni combination and no changes in conjugation were detected in the presence of the Ni catalyst alone. The increased activity of the Pd/Ni system over Pd alone was attributed to adsorption of catalyst poisons from the oil by Ni.