无定型聚芳醚酮的氯甲基化改性

采用硫酸作溶剂及催化剂,1,4-二氯甲氧基丁烷（BCMB）为氯甲基化试剂,在均相反应体系中对酚酞聚芳醚酮（PEK-C）进行氯甲基化改性。 采用无致癌性的BCMB作为氯甲基化试剂实现了环境友好,并且成本低,效率高。 试验结果表明,反应机理由苯环亲电取代与亲核取代2种反应构成。 为避免交联反应的发生,反应要在较低温度下进行（10~30 ℃）。 在此温度范围内可制得氯甲基化程度达3.4且完全线型的氯甲基化酚酞聚芳醚酮。 通过反应温度及时间可对树脂氯甲基化程度（χCH2Cl-）实施有效的调控。 CMPEK-C的结构由IR和1H NMR进行了表征,测定了CMPEK-C的Tg与χCH2Cl-之间的依赖关系及CMPEK-C的耐热及溶解性能。     

Preparative purification of five bioactive components from Agrimonia pilosa Ledeb by high-speed counter-current chromatography

High-speed counter-current chromatography (HSCCC) coupled with ultraviolet (UV) detection or evaporative light-scattering detection was successfully applied for preparative separation of five bioactive compounds from Agrimonia pilosa Ledeb. In preliminary process, D101 macroporous resin was used to separate the crude extract of the plant and four fractions (20, 40, 50, and 60% aqueous ethanol elutions) were produced. Then, these fractions were directly subjected to HSCCC purification. Five chemicals including taxifolin-3-glucoside (6.4 mg), quercetin-3-rhamnoside (13.0 mg), tiliroside (14.7 mg), agrimonolide (21.4 mg), and tormentic acid (29.8 mg) with the purities of 94.24, 95.37, 97.42, 95.29, and 96.34% were separated from each 200 mg prepared fraction. The purities were analyzed by high-performance liquid chromatography, and the chemical structures of the products were identified by UV detection, mass spectrometry, nuclear magnetic resonance, and the standards. This paper used a simple method to separate five bioactive compounds from A. pilosa Ledeb, and it could provide a new idea for the purification of bioactive compounds from other medicinal plants.     

BER催化还原一些含氮功能基化合物的研究

用强碱性阴离子交换树脂制备了硼氢阴离子交换树脂还原剂(BER),使其在氯化铜等金属化合物的催化下还原一些芳香硝基、氰基、氮氮双键等含氮功能基化合物.还研究了BER的制备条件:如温度、溶剂、不同金属化合物对还原反应的影响,并初步探讨其反应机理.     

高分子路易斯酸催化剂—阳离子交换树脂四氯化锡复合物

大孔强酸性聚苯乙烯系阳离子交换树脂与SnCl_4在CS_2中反应可生成一种稳定的高分子路易斯酸催化剂.其制备简单、易分离.这种催化剂不怕水,对酯化、缩醛、缩酮、醚化及付氏烷基化反应具有较好的催化作用,且催化性能稳定,至少可重复使用10次.     

用新型AP树脂分离铑—铱和同时富集测定铑`铱`铂`钯

铑-铱分离-向被认为是最困难的课题之一,即使文献曾报道Rh-Ir的分离,但实际Rh并未与萃取剂或吸附剂反应,而是与非贵金属离子一同留在溶液中。我们曾用光谱半定量方法研究了AP树脂对Rh、Ir的吸附行为,结果是Rh不被吸附而Ir能被吸附。本文通过改变Rh的离子状态,使之能被AP树脂吸附完全,而与留在溶液中的非贵金属分离,然后在柱上用不同淋洗液再使Rh-Ir分离。     

螯合树脂微柱分离富集火焰原子吸收法测定地质样品中的痕量银

利用新合成的螯合树脂聚[4 乙烯苄基 (2 羟乙基硫醚)]制备微型吸附柱,采用螯合树脂微柱分离富集 火焰原子吸收法测定了地质样品中的痕量银。研究了螯合树脂微柱的吸附性能及影响吸附的因素,在稀王水介质中进行吸附,采用酸性硫脲为洗脱剂,以峰面积方式检测,测定Ag 的线性范围0.010～1.0μg mL,灵敏度提高40倍,吸附率在80%,相对标准偏差<4.2%,树脂柱可重复利用100次以上。     

Scale-Up Preparation of Crocins I and II from Gardenia jasminoides by a Two-Step Chromatographic Approach and Their Inhibitory Activity Against ATP Citrate Lyase

Crocins are highly valuable natural compounds for treating human disorders, and they are also high-end spices and colorants in the food industry. Due to the limitation of obtaining this type of highly polar compound, the commercial prices of crocins I and II are expensive. In this study, macroporous resin column chromatography combined with high-speed counter-current chromatography (HSCCC) was used to purify crocins I and II from natural sources. With only two chromatographic steps, both compounds were simultaneously isolated from the dry fruit of Gardenia jasminoides, which is a cheap herbal medicine distributed in a number of countries. In an effort to shorten the isolation time and reduce solvent usage, forward and reverse rotations were successively utilized in the HSCCC isolation procedure. Crocins I and II were simultaneously obtained from a herbal resource with high recoveries of 0.5% and 0.1%, respectively, and high purities of 98.7% and 99.1%, respectively, by HPLC analysis. The optimized preparation method was proven to be highly efficient, convenient, and cost-effective. Crocins I and II exhibited inhibitory activity against ATP citrate lyase, and their IC₅₀ values were determined to be 36.3 ± 6.24 and 29.7 ± 7.41 μM, respectively.     

三价锰离子引发烯类单体在聚乙烯醇上接枝聚合的研究

<正> 无论是淀粉;纤维素,还是聚乙烯醇(PVA)的接枝反应,Ce(Ⅳ)被认为是一个十分有效的引发剂,已有较详尽的研究。与Ce(Ⅳ)相类似,Mn(Ⅲ)也可以和一些高聚物组成氧化还原引发体系,由此产生自由基,引发烯类单体在高分子主干上进行接枝聚合。Ranby等人,以焦磷酸络合的三价锰离子引发烯类单体在纤维素和淀粉的接枝反应中,获得了高效的接枝产物。有用这种引发体系在淀粉上接枝丙烯腈获得吸水276     

时间分辨激光光散射测量系统

自选设计，装配了一套时间分辨的激光光散射测量系统，该系统摄像机，录像机，计算机和自编的软件实现了一体化的数据采集，显示和分析过程，本文给出了该系统的应用实例，球晶的光散射和环氧树脂的固化反应诱导的相分离过程。     

Preparation and application of a novel orotic acid chelating resin for removal of Cu(Ⅱ) in aqueous solutions

A novel chelating resin OABA,capable of removing Cu(Ⅱ) from aqueous solution,was synthesized via the reaction of macroporous chloromethylated PS-DVB copolymer beads with orotic acid.The elemental analysis(EA),Fourier transform infrared spectroscopy(FT-IR),and scanning electron microscopy microscope-energy dispersive X-ray spectroscopy(SEM-EDS) were used in the characterization of the synthesized chelating resin.Multiple,static batch adsorption experiments were conducted at different initial concentrations and temperatures.OABA showed good adsorption capacity for Cu(Ⅱ) and the equilibrium data could be well matched with the Freundlich isotherm model.Coexisting sodium chloride and calcium chloride in solutions favored the Cu(Ⅱ) adsorption.Moreover,the desorption process of Cu(Ⅱ) was tested and over 90%regeneration efficiency for the spent OABA was achieved at ammonia concentrations ranging from 1.0%to 2.0%.The results suggested that OABA would be a potential alternative adsorbent for Cu(Ⅱ),even with other heavy metal ion treatments of wastewater.