1-烷基吲哚-3-乙酸的合成

以吲哚-3-乙腈为原料,经过与卤代烷在碱存在下的N-烷基化和碱水解2步反应分别合成了1-甲基吲哚-3-乙酸(2a)和1-[3-(四氢-2H-吡喃-2-氧基)丙基]-1H-吲哚-3-乙酸(2b),总收率分别为87%和68%,其结构经1H NMR和Ms确证。     

具有双螺吡喃结构的光致变色化合物的合成研究

以2,3,3-三甲基-4H-吲哚为起始原料,通过羟乙基化、闭环和缩合反应,三步合成了一种具有双螺吡喃结构的化合物,并且对反应机理进行了研究。通过条件实验对合成工艺进行了优化,合成的总收率达到48．3％。     

Heißgasfiltration im Synthesegas aus Biomasse

During thermochemical conversion of biological material in a fluidized bed reactor the nutrients are remaining as dust in the product gas. Hot gas filtration represents a possibility to recover these minerals. The characteristics of this gas add up new technical tasks. The following article gives an account of long lasting experience of operation and optimization in a pilot plant.     

光气法合成邻羟基苯甲腈研究

邻羟基苯甲腈是一种重要的化工中间体,广泛应用于医药、农药、染料、高分子合成等工业生产中。研究了水杨酰胺和光气在甲苯溶液中合成邻羟基苯甲腈的反应,得出最佳反应条件为n(水杨酰胺)∶n(光气)=1∶1.2、反应温度90～100℃、反应时间5 h。经溶剂甲苯回收后,将邻羟基苯甲腈重结晶提纯,产品质量分数为95.1%,收率达92.3%。     

合成条件对Mg—AI—CO23一LDHs的物相及组成的影响＊

以Mg（NOa）2·6H20为镁源,以Al（N03）3·9H20为铝源,采用共沉淀法制备了阴离子型层状材料Mg-A1-COjLDHs,并用X射线衍射（XRD）、傅里叶变换红外光谱（Fr—IR）、扫描电镜（SEM）和透射电镜（TEM）对产物进行了表征。探讨了加料方式、插层阴离子的用量以及沉淀反应温度对所形成产物物相等的影响。XRD分析结果显示不同加料方式所制备的产物均具有典型的层状结构特征,其中pH恒定法所合成的产物结晶度更高;红外光谱显示产物中存在插层阴离子C023-;EDX元素分析结果表明产物组成中含有Mg和Al,且n（镁）：”（铝）=2．6。上述表征结果说明：加料方式、插层阴离子的用量以及沉淀反应温度对产物的物相没有影响,但对产物的结晶度有一定的影响。当初始原料的配比为n（Mg）：n（A1）：n（OH）：n（C（）23-）-6：2：20：2时,在45℃下完成沉淀反应,再将沉淀于65℃下晶化18h可以得到具有典型层状结构的Mg-A1一C0;一LDHs。     

溶剂共沸脱水法合成BP04粉体

以硼酸和质量分数为85％磷酸为反应原料,环己烷做带水剂,在不同的反应时间下,利用溶剂共沸脱水法制备磷酸硼粉体。产物的XRD、FT-IR分析表明,在磷酸硼中含有少量未反应的硼酸。产物分别在120、140℃下进行热处理,每2h取样进行FT-IR、XRD测试。测试结果表明,共沸2h制得磷酸硼在120℃下热处理6h,或140℃下热处理4h,可得到纯的磷酸硼粉体。共沸5h制得磷酸硼120℃下热处理4h,或140℃下热处理2h,可得到纯的磷酸硼粉体。     

Effect of residual excess carbon on the densification of ultra-fine HfC powder

The residual carbon content of ultra-fine hafnium carbide (HfC) powder was controlled by the optimization of the synthesis process, and the effect of residual carbon on the densification of HfC powder was analyzed. The amount of residual carbon in the HfC powder could be reduced by the de-agglomeration of HfO₂ powder before the carbo-thermal reduction (CTR) process. The average particle size of HfO₂ powder decreased from 230 to 130 nm after the de-agglomeration treatment. Ultra-fine (d₅₀: 110 nm) and highly pure (metal basis purity: >99.9 % except for Zr) HfC powder was obtained after the CTR at 1600 °C for 1 h using the C/Hf mixing ratio of 3.3. In contrast, the C/Hf ratio increased to 3.6 without the de-agglomeration treatment, indicating that a large amount of excess carbon was required for the complete reduction of the agglomerated HfO₂ particles. HfC ceramics with high relative density (>98 %) were obtained after spark plasma sintering at 2000 °C under 80 MPa pressure when using the HfC powder with low excess carbon content. In contrast, the densification did not complete at a higher temperature (2300 °C) and pressure (100 MPa) when the HfC powder contained a large amount of residual carbon. The results clearly indicated that residual carbon suppressed the densification of HfC powder in case the carbide powder had low oxygen content, and the residual carbon content could be controlled by the optimization of the synthesis process. The average grain size and Vickers hardness of the sintered specimen were 6.7(±0.7) μm and 19.6 GPa, respectively.     

C_5石油树脂合成及改性研究新进展

阐述了C5石油树脂的结构、性能及聚合机理;综述了氯铝酸离子溶液等新型催化剂、合成技术、加氢改性工艺和新型精制催化剂的研究进展,以及C5石油树脂用作柴油降凝剂和路标漆的最新应用研究。指出了加氢精制技术生产高软化点、无色的石油树脂是今后C5石油树脂的发展方向。     

The intramolecular capture of thermally generated merocyanine dyes derived from naphthopyrans: Photochromism of 5-(diarylhydroxymethyl)-2H-naphtho[1,2-b]pyrans

A series of 2H-naphtho[1,2-b]pyrans bearing a diarylmethanol unit at C-5 have been synthesised by the addition of an excess of an aryllithium reagent to alkyl 2H-naphtho[1,2-b]pyran-5-carboxylate precursors. These naphthopyrans show photochromism when exposed to ultraviolet irradiation and also generate intense colours at low pH through triarylmethine cation generation. However, photochromism of the triarylmethine cation derived from the naphthopyran unit could not be detected. An irreversible cascade process initiated by the thermally-induced ring-opening of the diarylmethanol substituted 2H-naphtho[1,2-b]pyrans in the presence of an acid catalyst afforded novel benzopentalenonaphthalenone dyes.     

Synthesis, characterization, and optical properties of new metal complexes with the multi-sulfur 1,2-dithiolene ligand

Metal complexes containing a new multi-sulfur atom containing 1,2-dithiolene ligand, [4′,5′:5,6] [1,4] dithiino[2,3-b] quinoxaline-1′,3′-dithiolate, have been synthesized and characterized by electrochemical measurements, IR, UV-NIR and ESR spectroscopies. X-ray structure analysis reveals that the anions of the Ni-complex derived from the new ligand form a zig-zag chain along the b axis, and the anions of Au complex of the ligand stack along the a axis while the cations occupy the holes. The Ni-complex exhibits remarkable absorption at 1082 nm (? = 15?000 dm³ mol⁻¹ cm⁻¹) and good solubility that render this complex as a promising near-IR dye for Q-switching neodymium lasers. The third-order non-linear optical properties of the complexes are measured by the Z-scan technique with a 6.5 ns pulsed laser at 532 nm. The Au complexes exhibit non-linear optical absorptive abilities, while the non-linear absorption of the nickel complex is negligible. All of the complexes show effective self-defocusing performance. The third-order non-linear optical susceptibilities for the Au complexes have been determined to be of the order of 10⁻¹³ esu.