用磷酸铝分子筛和硅磷酸铝分子筛作催化剂合成丙酸戊酯的研究

用新型磷酸铝分子筛和硅磷酸铝分子筛作催化剂,对丙酸和正戊醇液—固相酯化反应进行了研究.考察了合成条件及用不同方法制备的催化剂对醇产率的影响,当醇酸摩尔比为1.2∶1、催化剂用量为0.6～1.0g/mol丙酸、带水剂环己烷用量为5.0ml/mol丙酸,反应温度为140～160"C时,5hr酯化反应的酯产率大于98％.同时对酯产物的物理常数进行了测定,实测值与文献值相符.     

In vitro protein synthesis and α amylase activity in F cells from hepatopancreas ofPalaemon serratus (Crustacea; Decapoda)

In crustaceans, all the steps in the assimilation of food take place in the hepatopancreas. To facilitate the study of this organ, a method for the dissociation of cell types was developed. The hepatopancreas of the prawnPalaemon serratus was mechanically dissociated and the cells separated by Percoll density-gradient centrifugation. The E and R cells had similar densities of around 1.05 g/ml. The F cells were separated into two distinct fractions with densities of 1.075 and 1.082 g/ml. The B cells sedimented at a density of 1.12 g/ml. The ratio between the two populations of F cells was found to vary during the intermolt cycle while B cells disappeared after the molt. When the density gradient fractions were incubated with³H-leucine, incorporation was highest in the F cell fractions. Measurements of -amylase activity, indicated that the two populations of F cells may be derived from the same cell type.     

Improvement in hydrogen storage performance of Mg by mechanical grinding with molten salt etching Ti3C2Clx

Mg-based materials are currently a hot research topic as hydrogen storage materials due to their considerable theoretical hydrogen storage capacity. However, the kinetic performance of hydrogen absorption and desorption of Mg is too slow and requires high temperature, which seriously hinders the application of this material. MXene is a new type of two-dimensional material with significant role in improving thermodynamics and kinetics. In this experiment, a two-dimensional layered MXene containing Cl functional group was prepared by molten salt etching using the Ti-containing MAX phase as the raw material. Then different ratios of Ti₃C₂Cl_x were uniformly dispersed onto the surface of Mg by high energy ball milling. The samples were characterized by hydrogen absorption and desorption kinetics, SEM, XRD, XPS, and DSC to investigate the effect of Ti₃C₂Cl_x on the hydrogen absorption and desorption performance of Mg. The onset hydrogen absorption temperature can be reduced to room temperature and the hydrogen release temperature is reduced by 200 ​°C by doping Ti₃C₂Cl_x. And there is also 5.4 ​wt% hydrogen storage in the isothermal hydrogen absorption test at 400 ​°C. The results of DSC demonstrate that the E_a of Mg+15 ​wt% Ti₃C₂Cl_x was reduced by 12.6% compared to pristine Mg. The ΔH is almost invariable. The results of XPS show that the presence of multivalent Ti promotes electron transfer and thus improves the conversion between Mg²⁺/Mg and H⁻/H. This study provides a guideline for further improving the hydrogen absorption and desorption performance of Mg-based hydrogen storage materials.     

3—己烯—1—醇及其酯类的合成和香气研究

介绍了叶醇(cis-3-己烯-1-醇)及其异构体的实用合成路线。由顺反混合(或全反式)3-己烯-1-醇制备了一系列羧酸酯,研究了这些化合物的结构与香气的关系,从中发现一些有实用价值的新香料。     

Sex pheromone of the pine sawflyDiprion pini (Hymenoptera: Diprionidae): Chemical identification,synthesis and biological activity

The main component of the sex pheromone secretion of femaleDiprion pini L. (Hymenoptera: Diprionidae) from insects collected both in Finland and in France has been identified as athreo-3,7-dimethyl-2-tridecanol (8 ng per female) stereoisomer by GC-MS and synthesis. The secretion also contains lower and higher homologues in small amounts (1–4% of the main component). Combined gas chromatographic-electroantennographic detection showed activity in both natural and esterified extracts (acetates and propionates); the esters of the main component gave the largest responses. The acetates and propionates of the eight stereoisomers of 3,7-dimethyl-2-tridecanol were synthesized from enantiomerically highly enriched (>99% ee) building blocks. The stereochemistry of the main component was established to be (2S,3R,7R)-3,7-dimethyl-2-tridecanol by GC analysis of the natural material. It was purified by liquid chromatography prior to the GC analysis of both its pentafluorobenzoates and its isopropylcarbamates on a non-chiral polar column (ECD) and a chiral column (NPD), respectively. Field tests demonstrated that both the acetate and propionate of the main component (100 g of each applied on cotton roll dispensers) were active in attracting males, with or without the presence of several of the minor compounds. Experiments with smaller amounts of the acetate and the propionate (1 g in France and 50 g in Finland) demonstrated that the propionate was more active than the acetate, and that it also caught more males than a blend of the two compounds.     

苯甲醛缩氨基硫脲Cu(I)、Zn(Ⅱ)配合物的直接电化学合成

用电化学金属阳极氧化法在非水溶剂中合成了苯甲醛缩氨基硫脲（ＨＬ）与Ｃｕ（Ｉ）、Ｚｎ（Ⅱ）配合物,通过元素分析、红外光谱、紫外光谱、磁矩、摩尔电导等对配合物进行了表征。     

2,3-二羟基哌嗪与几种氨基化合物的缩合反应研究

由乙二胺与乙二醛的缩合物２,３－二羟基哌嗪,分别与甲酰胺、脲和乙二胺反应,制得２,４,７,９,１１,１４－六氮杂三环［８,４,０,０３,８］十四烷六盐酸盐四水合物（１）,２,５,７,９－四氮杂双环［４,３,０］壬－８－酮二盐酸盐－水合物（２）和２,５,７,１０－四氮杂双环［４,４,０］癸烷（３）。化合物１为未见文献报道的新化合物。化合物２的合成工艺条件优化后,反应得率与文献［１］相比有一定提高。化合物３的合成,由于将反应分为低温和高温两个缩合阶段,使反应得率提高到７７．５％。     

微波合成PMMA胶乳粒子

在常压微波辐照下合成聚甲基丙烯酸甲酯（ＰＭＭＡ）单分散的胶体微粒。体系中未加表面活性剂和稳定剂,在透射电镜下观察粒子的形状和直径大小,并得出在引发剂浓度一定的条件下,微粒的体积与单体的浓度呈现线性关系,为我们合成一定大小的超细微粒提供了选择的条件。功力学实验表明,微波场下反应速度大大加快,反应是突变的,无恒速阶段。     

Diamond synthesis from a system of chromium-carbide and Ni70Mn25Co5 alloy

In order to ascertain the mechanism of interaction between carbide and metallic catalyst and formation of diamond under high pressure and high temperature, and find a new method to synthesize diamond with special properties, it is necessary to investigate the reaction behavior of different carbides and metallic solvent_catalysts under high pressure and high temperature. A system of Cr-3C-2 powder and Ni 70Mn 25Co 5 alloy in weight ratio of 1∶6 was treated under 6 0 GPa and 1 500℃ for 20, 30 or 60 min respectively. X_ray diffraction of the samples indicated the Cr 3C 2 decomposed partially after high pressure and temperature treatment, and Cr 7C 3, Cr and diamond formed respectively. There was not any trace of graphite in the samples. The result suggested that the separated carbon atoms could form diamond directly without conversion process of graphite into diamond. The observation of SEI, WDX and EDX also showed that diamond crystals were synthesized in the system, which have perfect surfaces and shapes, with the average grain size of about 40 μm. The properties of the crystals are being investigated.