2,2'-亚甲基双(4-叔丁基苯基)磷酰氯的制备及表征

以2,2'-亚甲基-双(4-叔丁基苯)酚和三氯氧磷为原料,通过滴加缚酸剂和催化剂三乙胺,反应生成了2,2'-亚甲基双(4-叔丁基苯基)磷酰氯。主要研究了加料顺序、时间、温度和溶剂量对反应产物和收率的影响。当滴加三乙胺,加入25 mL溶剂,反应时间2 h和反应温度为45℃时收率可以达到68%。对产物进行了傅里叶红外变换光谱仪(FTIR)、核磁共振仪(NMR)、质谱仪(MS)和差式扫描量热分析(DSC)表征,各项检测表明,合成的产物为2,2'-亚甲基双(4-叔丁基苯基)磷酰氯。     

The effect of triethylamine on the hydrodechlorination of chlorophenols on Pd/C at low temperature

The hydrodechlorination (HDC) of chlorophenols on 5 wt.% Pd/C catalyst was investigated at low temperature under ordinary pressure by using triethylamine (Et₃N) as a base additive. The inhibition effect of Et₃N on the HDC existed obviously and can be efficiently reduced by stepwise addition of Et₃N. For the first time, the high activity of Pd/C for HDC of chlorophenols was observed at 258 K.     

AKD生产中三乙胺的回收和利用

从副产物三乙胺盐酸盐中回收三安对降低ＡＫＤ生产成本至关重要。采用了物理和化学相结合的方法使回收三乙胺的含水量低于０．１％,满足了ＡＫＤ生产的要求。     

相转移催化法合成乙酸苄酯

对用相转移催化法合成乙酸苄酯工艺进行了改进,使用三乙胺作催化剂,三乙胺可回收,增加水解、脱醛步骤,使合成的产品不含氯、纯度高、香气好,具有较高的工业实用价值.     

Enhanced triethylamine sensing performance of superfine NiO nanoparticles decoration by two-dimensional hexagonal boron nitride

The novel two-dimensional hexagonal boron nitride (h-BN) decorated nickel oxide (NiO) heterojunction was successfully synthesized by a facile solvothermal precipitation method combining with heat treatment. SEM and TEM analysis were used to corroborate the average size (~8 nm) and overall distribution of superfine NiO nanoparticles on h-BN. XRD, FT-IR and XPS characterization confirmed the configuration of highly crystallinity and p-n heterojunction as well as the presence of surface oxygen vacancy defects. Gas sensing test results revealed that the decoration of h-BN could significantly enhanced triethylamine (TEA) sensing property of NiO. The main contribution of such remarkable results lies in NiO nanoparticles that are close to Debye length scale were embedded on vacancy defects of functionalized h-BN nanosheets, which can optimize sensitivity and selectivity by taming two-dimensional (2D) interfacial electronic effects that strongly affect nonmetal-support interaction between grain boundaries. Meanwhile, the formation of p-n Schottky nanoscale heterojunction between NiO and h-BN can significantly enlarge resistance variation and efficiently promoted the adsorbed triethylamine molecules to oxidize into NO₂, H₂O, and CO₂. Our work highlights the important role of coupling functionalized h-BN in gas sensors, which can also provide a valuable avenue in boosting the sensing performance.     

Ultrahigh sensitive and selective triethylamine sensor based on h-BN modified MoO3 nanowires

In this work, a novel structure of 1D MoO₃ nanowires wrapped by 2D hexagonal boron nitride (h-BN) was synthesized via a simple solvothermal method with subsequent annealing process for triethylamine (TEA) detection. The samples were characterized by XPS, SEM, HRTEM and N₂ adsorption-desorption. Gas sensing performance test results illuminate that the typical 2 wt% h-BN/MoO₃ sensor possesses an ultrahigh response (8616) toward 500 ppm TEA. The promoted sensing performance of TEA may be caused by the forming of heterojunction between h-BN and MoO₃, the increased specific surface area of h-BN modification, providing a highly active sites for the adsorption of TEA gas, which greatly enhance the response of the sensor. The adsorption energy of a single oxygen molecule on MoO₃ (0 1 0) surface was calculated by DFT, indicating the most stable site is the terminal oxygen position (Top O-1), with an adsorption energy of ?2.075 eV. This work provides an inspiration to design highly efficient TEA gas sensor on basis of h-BN/MoO₃ nanocomposites.     

一种超高密度存储材料的四极质谱分析

三乙胺-四氰-p-醌二甲烷(TEA(TCNQ)2)单晶样品是一种可以用来进行超高密度信息存储研究的有机复合物材料.在扫描隧道显微镜(STM)针尖和TEA(TCNQ)2样品间加电压脉冲,可以在TEA(TCNQ)2样品表面形成规则排列的直径为纳米级孔洞阵列.为了阐明孔洞形成的机理,使用四极质谱计对其进行了残气分析.在负高压脉冲刻蚀TEA(TCNQ)2样品,测量到放出气体为TEA的86u主峰,证实了STM脉冲刻蚀形成的孔洞阵列主要是由于TEA(TCNQ)2气化分解的结果.测量TEA(TCNQ)2样品在不同热处理温度时的放气质谱,发现TEA(TCNQ)2样品在110℃时大量放出TEA气体.     

Influence of the temperature on the formation of a phenolic resol resin catalyzed with amine

The influence of the condensation temperature on the phenolic resol resin prepolymer formation was studied by liquid chromatography and carbon nuclear magnetic resonance (¹³C NMR) spectroscopy. Four resols catalyzed with triethylamine and with initial pH=8.0 and F/P=1.8 were synthesized at 60, 80, 95 °C, and reflux (98-102 °C). On increasing the condensation temperature, reactant consumption rates and first formed addition products increased, condensation times decreased as well. Prepolymer synthesized at refluxing temperatures showed higher formaldehyde addition onto ortho positions with respect to the other resols. Different types of phenolic rings connecting bonds were observed: para, para and ortho, para bridges as well as ether bonds were detected. No ortho, ortho bonds were observed for the condensation with the catalyst used. ¹³C NMR measurements did not show qualitative differences between prepolymers. Anyway, residual phenol and formaldehyde concentrations and the amount of free unreacted ortho and para positions decreased with temperature.     

冷芯盒法的现状与展望

根据所用硬化气体的种类对冷芯盒法进行归类 ,叙述了冷芯盒法的工艺特点 ,适用范围及其应用现状 ,并对其发展前景进行了探讨。     

N-苄氧羰基-L-丝氨酸苄酯的合成研究与改进

摘要：以苄氧羰基氯、L -丝氨酸为原料,合成了N -苄氧羰基-L-丝氨酸。通过正交实验考察了反应温度、pH、原料的摩尔比、相转移催化剂对N -苄氧羰基-L-丝氨酸收率的影响。优化反应条件后N-苄氧羰基-L-丝氨酸收率为93.2%。N -苄氧羰基-L-丝氨酸和苄溴反应生成了目标产物-N-苄氧羰基-L-丝氨酸苄酯,重点探讨了酯化过程中缚酸剂、原料的投料顺序及产品后处理对目标产物得率的影响。选择具有催化作用的三乙胺为缚酸剂,用10%的亚硫酸氢钠对产品进行后处理使得N-苄氧羰基-L-丝氨酸苄酯的纯度达98.5%。通过红外、核磁、熔点、旋光度等对目标产品进行了结构表征, 用高效液相色谱对产品的纯度进行了测定。