柱层析法分离木糖醇和山梨醇的研究

本文研究了层析、D031、001×7聚苯乙烯—二乙烯基苯磺酸型阳离子交换树脂和它们的H~+、NH_4~+、Co~(2+)、Ba~(2+)、Ak~(3+)、Fe~(3+)或Cr~(+3)等离子基型对木糖醇和山梨糖醇的柱层析分离效果。结果表明,层析H~+、Fe~(3+)型和D031H~+型树脂能有效地分离木糖醇和山梨醇。最适宜温度均为55℃,最适宜洗脱液流量:层析H~+及Fe~(3+)型树脂分别为4.8ml/min和2.8ml/min,D031H~+型为3.0ml/min。以10~(-3)mol/dm~3的十二烷基硫酸钠的3％正丙醇溶液为洗脱液能明显提高分离能力。     

离子交换法纳米Cu2O的制备及光催化性能的研究

采用强酸性阳离子交换树脂（R—H）,以CuSO4·5H2O为原料,制备出R2-Cu型阳离子交换树脂,R2-Cu型阳离子交换树脂与酒石酸钾钠进行离子交换得到Cu（OH）2,再用葡萄糖还原制得Cu2O纳米粒子,用IR、XRD、BET、TEM等手段对样品进行了表征,并以催化罗丹明B为模拟染料,日光（4月晴天,T=15～25℃）为光源,在自制的无色透明的玻璃反应器进行光催化降解反应,考察了Cu2O纳米粒子的催化性能．     

树脂吸附法深度处理焦化废水

将树脂吸附剂应用于焦化废水的深度处理,考察了温度、投加量、初始pH、时间和流速对CODcr和色度去除效果的影响.静态吸附实验确定了最佳吸附树脂为NDA-99型树脂,最佳投加量为3.00g/L,无需调节pH,最佳温度为303K,吸附等温线满足Freundlich方程.通过动态实验确定了最适宜工艺条件为:流速20BV/h,单柱废水处理量为200BV/批;处理后废水中CODcr浓度从199mg/L降到100mg/L以下,色度从98倍降到50倍以下.使用8％的NaOH溶液脱附再生,最佳脱附流速为5BV/h.     

有机胺对阳离子交换树脂性能的影响

采用浸泡方法分别研究了氨、乙醇胺、吗啉对阳离子交换树脂性能的影响。利用光学显微镜观察浸泡前后阳离子交换树脂的形貌。55℃下,分别在pH值为9.3的氨、乙醇胺及吗啉的溶液中浸泡不同时间后离子交换树脂的总交换容量、含水率、湿视密度、湿真密度变化均不明显。以3种不同浓度(0.9mol/L、1.4mol/L、1.9mol/L)的氨、乙醇胺及吗啉的溶液分别浸泡离子交换树脂,浸泡后总交换容量、含水率、湿视密度、湿真密度的变化也不大。在恒定pH值与不同浓度碱化溶液中浸泡后,黑琥珀色半透明离子交换树脂的颜色均变浅。实验结果表明有机胺对凝胶型阳离子交换树脂的性能和形貌影响不大。     

H3PO4改性PS-EDTA树脂对水相中Cu2+、Zn2+和Cd2+的吸附性能研究

大孔氯甲基化聚苯乙烯小球先后与乙二胺、2-氯乙酸反应得EDTA型螯合树脂(PS-EDTA),再用磷酸在室温处理得PS-EDTA/P树脂。PS-EDTA/P树脂被用于水相中Cu2+、Zn2+和Cd2+的吸附净化处理,探讨了溶液的pH值、初始金属离子浓度、时间、温度等因素对吸附性能的影响,并研究了其对重金属离子的吸附动力学和热力学。结果表明,PS-EDTA/P树脂对Cu2+和Zn2+的吸附符合Langmuir等温式、对Cd2+的吸附符合Freundlich等温式,准二级吸附动力学方程能够很好地描述3种金属离子在树脂上的吸附动力学行为。同时,PS-EDTA/P树脂对重金属吸附的热力学参数表明,PS-EDTA/P树脂对Cu2+、Zn2+和Cd2+的吸附是一个自发的、吸热的过程。已吸附Cu2+、Zn2+和Cd2+的树脂可以用0.1mol/L HCl解吸,解吸后的树脂对Cu2+、Zn2+和Cd2+仍具有较高的吸附量。     

木薯羧甲基淀粉对铜离子的吸附性能

采用搅拌球磨机对木薯淀粉进行机械活化,以活化60 min的木薯淀粉为原料,干法合成羧甲基淀粉吸附剂。考察羧甲基淀粉的取代度、溶液的pH值、Cu2+的初始浓度、吸附时间、羧甲基淀粉的投加量等因素对羧甲基淀粉吸附Cu2+性能的影响。结果表明,该羧甲基淀粉对Cu2+有很好的吸附作用;用取代度为0.841的羧甲基淀粉处理含Cu2+的废水,在pH=7.0、羧甲基淀粉的投加量50.00 mg/L、吸附时间15 min时,羧甲基淀粉对废水中Cu2+的吸附率高达98.80%,处理后的水质达到国家污水综合排放标准(GB8978-1996)中一级标准要求。     

三相流化床电极反应器深度处理制浆废水

应用三相流化床电极反应器(新型电化学反应器)处理制浆废水.研究了曝气量、槽电压、溶液pH值及FeSO4浓度等因素对电解效果的影响.结果表明,该反应器深度处理制浆废水的最佳工艺条件为:槽电压20 V,曝气量为0.3 m3.h-1,FeSO4浓度为1000 mg.L-1,pH值≈2.5,反应时间为90 m in时COD去除率为70.1%.     

粉煤灰/壳聚糖复合材料制备及处理含重金属工业废水的研究

研究了粉煤灰/壳聚糖制复合颗粒吸附材料的工艺条件、再生方法,并用其处理含重金属工业废水。实验结果表明,壳聚糖与粉煤灰质量比为0.08:1,乙酸浓度为4%,液固质量比为0.6:1,制成的颗粒材料吸附效果好。在未调节该废水pH值的条件下,复合颗粒吸附材料用量为0.025g/mL,吸附时间为60min,温度为25℃,Cu2+、Pb2+、Zn2+的去除率分别为99.25%、75.16%、79.33%,处理后的废水中Cu2+、Zn2+的残留浓度远低于国家污水综合排放标准(GB8978-1996)一级标准,Pb2+的残留浓度低于该标准最高允许排放值。吸附遵循Langmuir吸附等温式:CCu/Q=1.3249CCu+0.1458。对Cu2+、Pb2+、Zn2+的吸附选择性顺序为:Cu2+Zn2+Pb2+。用1mol/LNaCl溶液对吸附饱和复合颗粒吸附材料进行再生,用其处理该废水效果仍然较好。     

盐改性沸石处理低浓度含Cu~(2+)模拟废水的研究

沸石是一种经济、高效和环境友好的材料,具有吸附、离子交换与催化性能,可作为一种水处理材料用于控制环境污染。本论文探讨了利用盐改性沸石处理低浓度含Cu2+模拟废水的主要影响因素,包括处理时间、改性沸石用量、p H值、废水浓度和处理温度。实验结果表明,用2mol/L Na Cl改性的沸石1.2g处理100.0m L Cu2+质量浓度为10.44mg/L的模拟废水50min,最高去除率达到96.84%,Cu2+剩余浓度为0.33mg/L,处理效果达到《污水综合排放标准》(GB8978-1996)一级标准。     

球形纤维素基磁性阳离子的化学转化制备及机理研究

通过正交设计实验确定了用化学转化法制备球形纤维素基磁性阳离子交换树脂的最佳条件,即:将树脂在室温下浸渍于摩尔比为1∶2的Fe3 与Fe2 混合铁盐溶液中90min,然后,加入2mol/L的NaOH溶液,在搅拌下转化20min,Fe3 、Fe2 将转化为FeFe2O4并将均匀的分布在树脂的表面及大孔结构中,从而获取磁性树脂.并初步探讨了阳离子交换树脂磁化的机理.     

二氧化碳和丙烯直接合成甲基丙烯酸的NiPMo/TiO2催化剂的研究

用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%.     

Synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives

Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields.     

Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction

In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.     

CoFe2O4自形成磁性液体场致结构化对磁化的影响

The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula.     

Highly regioselective Buchwald–Hartwig amination at C-2 of 2,4-dichloropyridine enabling a novel approach to 2,4-bisanilinopyridine (BAPyd) libraries

The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.     

KMnO4-mediated oxidative CN bond cleavage of tertiary amines: Synthesis of amides and sulfonamides

KMnO₄-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields.     

Chemistry of heterocyclic compounds at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences, over 50 years (Review)

The review contains a concise historical account and information on the most significant researches undertaken by the staff at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry of Heterocyclic Compounds. Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008.     

A general and convenient synthesis of 4-(tosylmethyl)semicarbazones and their use in amidoalkylation of hydrogen,heteroatom, and carbon nucleophiles

A general synthesis of previously unknown semicarbazone-based α-amidoalkylating reagents, 4-(tosylmethyl)semicarbazones, has been developed. The synthesis involved three-component condensation of semicarbazones of aliphatic or aromatic aldehydes with the same or other aldehydes and p-toluenesulfinic acid. The scope and limitations of this reaction were investigated. The compounds obtained were demonstrated to be an efficient α-(4-semicarbazono)alkylating agents. They were reacted with H- (sodium borohydride), O- (sodium methylate), S- (sodium phenylthiolate), N- (pyrrolidine, sodium succinimide), P- (trialkyl phosphites), and C-nucleophiles (sodium diethyl malonate) to give the corresponding products of the tosyl group substitution, 4-substituted semicarbazones, including analogues of nitrofurazone. Among the prepared compounds tested in vitro for antibacterial and antifungal activity, three nitrofuryl-containing semicarbazones exhibited high biological activities with minimum inhibitory concentration (MIC) values of 8–32 μg/mL.     

Sulfur-directed metal-free and regiospecific methyl C(sp3)–H imidation of thioanisoles

Regiospecific and direct imidation of the methyl C(sp³)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products.     

Synthesis of novel chiral bidentate hydroxyalkyl-N-heterocyclic carbene ligands and their application in palladium-catalyzed Mizoroki–Heck couplings and asymmetric addition of diethylzinc to benzaldehyde

A small library of new chiral bidentate hydroxyalkyl-imidazolium salts 1 is conveniently synthesized on multi-gram scale from inexpensive and commercially available chiral pool amino acids. The corresponding carbenes, generated by deprotonation of imidazolium salts 1, in combination with palladium(II) chloride were tested in the Mizoroki–Heck coupling reaction. The most significant results in terms of yields and reactivities were achieved with low catalyst loading. The catalytic activities of these imidazolium salts were also investigated in the asymmetric addition of diethylzinc to benzaldehyde. The use of MgO nanoparticles as an additive in conjunction with these ligands played a crucial role in increasing the efficiency of these reactions.