微波改性膨润土-石墨烯颗粒制备及对水中铬(Ⅵ)的吸附性能研究

用十六烷基三甲基溴化铵(CTMAB)和十八烷基三甲基氯化铵(OTAC)分别制得粉末状有机膨润土,并利用聚乙烯醇(PVA)为粘结剂,淀粉为造孔剂,在微波条件下,将2种粉末状有机膨润土与石墨烯复合,经高温焙烧制备改性膨润土-石墨烯颗粒CTMAB-MBGG、OTAC-MBGG。结果表明,OTAC-MBGG的吸附效果略优于CTMAB-MBGG,其最佳制备方案为:淀粉含量为0.7g,焙烧温度为550℃,焙烧时间为1h。模拟废水p H值为6,吸附温度为50℃,50r/min的恒温振荡器内,投加量1g/100m L,吸附时间为30min时,OTAC-MBGG对Cr(Ⅵ)的去除率可达96.54%。EDX和XRD结果表明,石墨烯与有机改性膨润土复合成功,颗粒吸附剂的层间距明显增大。     

改性沸石处理含铅废水的试验研究

采用沸石为吸附材料,研究其对废水中Pb2+的吸附作用和机理。研究了吸附剂用量、搅拌时间、pH值以及废水浓度等因素对吸附效果影响的探讨。试验结果表明,利用KCl改性后的沸石0.4g,在pH值为8~9的条件下,处理100mL Pb2+质量浓度为10.11mg/L的废水25min,废水中的Pb2+去除率最高可达99.60%,剩余浓度为0.05mg/L,远低于国家污水综合排放标准(GB8978-1996)的一级标准。     

污泥/钛铁矿复合吸附剂的制备及其吸附Cr(Ⅵ)研究

以城市污水处理厂剩余污泥为原料,添加微量钛铁矿,采用氯化锌活化法制备复合吸附剂,并考察了其对含Cr(Ⅵ)废水的处理效果。研究表明:钛铁矿添加量1.5%、氯化锌浓度3 mol/L、固液比1∶2、活化温度550℃和活化时间40 min时,复合吸附剂碘吸附值可达523.24mg/g,比表面积为285.003 m2/g,相对于不添加钛铁矿的纯污泥吸附剂分别提高了27.95%和43.08%;吸附Cr(Ⅵ)废水研究表明,当pH为1.5、吸附剂用量为4 g/L、吸附时间为120 min时,吸附率可达99.17%,吸附量为12.4 mg/g。     

石墨烯@有机膨润土颗粒对刚果红的吸附性能研究

制备了石墨烯@有机膨润土颗粒,利用FT-IR、SEM、N_2吸附-脱附与模型拟合分析,研究了该颗粒吸附剂对刚果红的吸附性能与机理。结果表明,石墨烯中的羧基与季铵盐离子形成了酰胺键,官能团-OH、N-H、Si-O-Si、Al-O-Si等参与吸附反应;颗粒吸附剂的平均孔径为5.53nm,以介孔为主,BET比表面积为60.3506m~2/g;室温下,投加量为20g/L,p H值为5,110r/min的转速下振荡180min时,石墨烯@有机改性膨润土颗粒对100mg/L刚果红模拟废水的去除率达97.09%;吸附过程符合准二级动力学方程,吸附行为更符合Freundlich吸附等温模型,表明其吸附为多层非均相吸附。     

MgZnAl-EDTA柱撑水滑石的制备及其对Pb(Ⅱ)的吸附

以共沉淀法合成的Mg2ZnAl-CO3水滑石为前体,采用离子交换插层组装方法制备了Mg2ZnAl-EDTA柱撑水滑石,并用XRD和IR进行表征。以水滑石前体和柱撑水滑石为吸附剂,用于废水中Pb2+的吸附。柱撑水滑石的吸附容量明显大于水滑石前体,柱撑水滑石的最佳吸附条件为:温度45℃,pH 5.5,吸附时间150min,Pb2+初始浓度100 mg·L-1。在最佳吸附条件下,柱撑水滑石对废水中Pb2+的饱和吸附量为183.51 mg/g。     

聚(丙烯酸-co-丙烯酰胺)/蒙脱土/腐殖酸钠复合物对Pb2+的吸附性能

用制备的聚(丙烯酸-co-丙烯酰胺)/蒙脱土/腐殖酸钠复合吸附剂,研究了溶液pH值、吸附时间和Pb2+溶液初始浓度等因素对重金属Pb2+的吸附性能,探讨了复合吸附剂对Pb2+的吸附机理。结果表明,在pH值为6.0、吸附时间2 h、Pb2+溶液初始浓度0.01 mol/L和吸附剂用量0.10 g的条件下,复合吸附剂对Pb2+的吸附量达到364.05 mg/g,平衡所需的时间为15 min。与蒙脱土相比,复合吸附剂具有更高的吸附容量和更快的吸附速率。     

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。     

三乙烯四胺改性榴莲壳吸附水溶液中的Cd~(2+)、Pb~(2+)

采用三乙烯四胺改性榴莲壳,制备新型的改性榴莲壳吸附剂,研究其对Cd2+、Pb2+的吸附性能。结果表明,吸附Cd2+、Pb2+的适宜条件为:pH 6.0,吸附时间120 min。改性后榴莲壳吸附剂对Cd2+、Pb2+的吸附容量有了很大程度的提高,Cd2+、Pb2+最大吸附量分别达到39.30、53.76 mg/g。吸附过程可以很好地用准二级动力学方程描述,吸附等温线用Langmuir方程的拟合效果优于Freundlich方程。     

改性香蕉皮对Pb2+的吸附研究

分别探讨了香蕉皮改性以及改性香蕉皮吸附Pb2+的主要影响因素。改性试验结果表明,香蕉皮的最佳改性剂为体积比为5:1的乙醇与乙酸混合溶液。通过正交试验得到最佳吸附条件为:Pb2+初始浓度20mg/L,pH=5,吸附剂用量为0.7g,吸附时间为70min,其中pH值和Pb2+初始浓度是影响Pb2+去除率的两个主要因素。在此条件下,当搅拌速率为150r/min时,100mL模拟废水中Pb2+去除率达到97.8%,吸附后残留的Pb2+浓度仅为0.46mg/L,达到《污水综合排放标准》(GB8978-1996)中的一级标准。等温吸附实验表明,改性香蕉皮对Pb2+的吸附用亨利等温方程拟合较好。     

原子吸收光谱法测定改性梨渣吸附Pb(Ⅱ)的研究

通过原子吸收光谱法研究了在不同pH、吸附剂量、Pb2+浓度和吸附时间条件下磷酸酯化改性梨渣吸附Pb2+的行为。结果表明:溶液初始pH 4.2时,Pb2+的吸附达到最大值;酯化梨渣≥10 g/L能除去Pb2+为30 mg/L溶液中的91%的Pb2+。酯化梨渣对Pb2+的吸附符合Langmuir等温模型,其最大吸附能力为43.99 mg/g。Pb2+达到吸附平衡的时间为40 min,准一级反应动力学方程可描述酯化梨渣对Pb2+的吸附过程。     

利用手持技术改进测定乙醇分子结构实验

利用压强传感器代替排水集气法,改进测定乙醇分子结构实验的仪器装置,并探索最佳反应条件。另外,设计两个空白实验,结合压强变化曲线对实验误差进行相关讨论。     

光谱仪测试范围的扩展

由于石化行业的生产需要，其材质的使用具有多样性和广泛性，经常会出现顾客委托的测试样品的一个或几个元素跨越光谱仪现有测试程序测量范围的情况。本法通过对光谱仪测试原理的认识，根据光谱仪的测试能力及标样的采集，实现了一个或几个元素测量范围的扩展，并对其测量的影响因素进行了研究。     

Influence of viscosity of medium on processes of oxygen quenching of excited states of mesoporphyrin

The oxygen quenching rate constants for singlet and triplet excited states of the dimethyl ester of mesoporphyrin IX increase with decreasing viscosity of the medium and reach a maximum at a viscosity of approximately 0.4 mPa·sec, after which the rate constants begin to decrease. The drop in rate constant with increasing fluidity of the medium may be related to a nonequilibrium character of the elementary act in the interaction of the reactants in the solvent cage. In viscous media such as isopropyl alcohol, isobutyl alcohol, and isoamyl alcohol, the reaction radius is greater than the sum of the radii of the reacting particles. The long-range character of these processes is due to the relatively weak dependence of the quenching probability on distance.Translated from Teoreticheskaya i Éksperimental'naya Khimiya, Vol. 25, No. 2, pp. 161–167, March–April, 1989.     

Dichroism of absorption and polarization of phosphorescence of molecules of the closed form of nitrobenzospirothiopyran

The spectral-polarization characteristics of absorption and phosphorescence of molecules of the initial form of nitro-substituted indolinospirobenzothiopyran were studied in oriented polyethylene films and in solutions with different polarity. An oscillator model of the electron transitions responsible for the formation of absorption and luminescence spectra was suggested. It was established that the principal differences in the spectral and photophysical properties of the compound studied and its oxygen-containing analog are associated with the fact that the electronegativity of the S atom is lower than that of the O atom. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 6, pp. 1143–1146, June, 1997.     

Determination of heats of detonation and influence of components of composite explosives on heats of detonation of high explosives

The heats of detonation of 20 simple high explosives and explosive mixtures were determined by means of an adiabatic detonation calorimeter designed by the authors. The results indicated that the performance of the instrument was reliable and the experimental data were very accurate. For explosive mixtures, there was a linear accumulative relationship between the heats of detonation of the explosive mixture and its components. Accordingly, the heats of detonation of explosive mixtures could be calculated directly from the heats of detonation of simple explosives and the characteristic heats of other components. The experiments showed that the gold or brass shell of the cylindrical charge could be substituted by a thick-walled porcelain shell, which had the advantage of cheapness.

     

物质分配系数的测定实验改进

实验教学目的是从解决实际问题出发,以实验技术训练和实验设计思想培养为目标。介绍了将单一的物质分配系数测定实验改进为综合实验,提高了实验效果及实验资源利用率。     

Neutral diterpenoids of oleoresins of five species of conifers of Transcarpathia

The compositions of the neutral diterpenoids of the oleoresins of five species of conifers growing in the Transcarpathia have been studied. It has been found that the oleoresins ofAbies alba M.,Larix decidua M., andPicea excelsa L. contain more than 50% of neutral diterpenoids. The group and qualitative compositions of the oxygen-containing diterpenoids have been determined. In the oleoresins ofAbies alba,Picea excelsa, andPicea abies tertiary alcohols — cis-abienol and isocembrol — predominate, while inLarix decidua the main component is the hydroxy ester larixyl acetate. Primary alcohols related to the resin acids have been found in all the oleoresins investigated. Features of the distribution of diterpenoids according to the species of conifers have been revealed. The results obtained are necessary for the chemotaxonomy of conifers of the family Pinceae.Novosibirsk Institute of Organic Chemistry, Siberian Branch, Academy of Sciences of the USSR. Translated from Khimiya Prirodynkh Soedinenii, No. 6, pp. 812–816, November–December, 1988.     

Calculation of enthalpies of hydrogenation of hydrocarbons

Sets of hydrogen molecule equivalents have been developed which permit the calculation of hydrogenation of different types of carbon-carbon bonds from ab initio total energies (3-21G and 6-31G* basis sets, and, to a more limited extent, for MP2/6-31G* data) of reactants and products. The calculated enthalpies of hydrogenation are in good agreement with experiment for unstrained molecules, with average errors on the order of 2 kcal/mol. The 6-31G* equivalents allow the enthalpies for strained molecules to be calculated accurately, but the 3-21G equivalents do not. The equivalents for both basis sets have been tested by calculating the enthalpies of hydrogenation of carbon-carbon bonds in nitrogen- and oxygen-containing organic molecules, free radicals, and classical carbocations. The results are in good agreement with experiment in most cases.     

非那雄胺合成工艺改进

非那雄胺能抑制5α-还原酶的活性,明显降低二氢睾酮水平,是一种治疗良性前列腺增生的有效药品。该合成工艺以甾烯酮酸为原料,将其与氯化亚砜反应,无须分离即与叔丁胺反应得17β-酰胺化合物,再氧化开环,环合,氢化,脱氢合成了非那雄胺。经元素分析、IR、1HNMR、13CNMR、MS分析表征了其结构。该法无须使用昂贵的2,2-二吡啶二硫化物和剧毒药品苯亚硒酸酐,且以乙酸铵代替氨气,降低了对设备的要求和腐蚀,更适用于工业生产。