ε-聚赖氨酸吸附条件的优化

以吸附率为指标,通过单因素试验比较了5种不同的树脂类型、p H值、溶质浓度和树脂量对ε-聚赖氨酸(ε-PL)的吸附效果,进一步采用响应面设计优化了HZD-3B和D155树脂的吸附条件,分析了两种树脂吸附ε-PL的吸附等温线以及吸附动力学曲线。结果表明,试验的5种树脂中,HZD-3B和D155树脂的吸附效果较好。HZD-3B最佳静态吸附条件为:溶液起始p H 8.5、起始浓度40g/L、树脂用量150g/L、温度25℃、吸附13h,ε-PL的最大吸附率是97.69%;D155最佳静态吸附条件为:溶液起始p H 8、起始浓度40g/L、树脂用量150g/L、温度25℃、吸附14h,ε-PL的最大吸附率是96.84%;等温线数据拟合均较符合Freundlich方程,动力学数据拟合均较符合二级动力学方程。发酵液验证试验结果显示,ε-PL最大吸附量与纯品吸附量基本一致。     

降低生物柴油中自由脂肪酸的吸附剂研究

以甘蔗渣为原材料,通过高温煅烧制备甘蔗渣吸附剂,用于降低生物柴油中的自由脂肪酸含量。采用SEM、热重分析仪对甘蔗渣吸附材料进行表征分析,研究不同煅烧温度对吸附剂吸附性能的影响,以及不同吸附条件对吸附效果的影响。结果表明,在实验条件下,当甘蔗渣吸附材料煅烧温度为600℃、吸附剂用量0.30 g、吸附温度25℃、吸附时间100 min时,可以将生物柴油原料油的酸值降至0.4 mg/g。     

弱酸性氨基二硫代甲酸酯功能化聚氯乙烯树脂对Hg2+的吸附与脱附性能

以聚氯乙烯为原料依次与四乙烯五胺、CS2和ClCH2COONa反应合成了一种含氮、氧、硫的弱酸性氨基二硫代甲酸酯功能化的聚氯乙烯螯合树脂,树脂的结构经红外分析和元素分析表征。探讨了在不同pH值、Hg2+初始浓度、吸附温度和时间等条件下合成树脂对Hg2+的吸附性能。结果表明,螯合树脂对Hg2+有较快的吸附速率,pH=2.0左右时树脂对Hg2+的吸附效果最好,随着温度的升高吸附量逐渐增大,35 ℃时Hg2+起始浓度为0.01766 mol/L时,树脂对Hg2+的吸附量可达3.330 mmol/g。树脂对Hg2+的吸附符合Langmuir和Freundlich等温式。用0.2 mol/L硝酸-10%硫脲对吸附后的树脂进行洗脱,脱附率达99.2%。     

强碱性阴离子交换树脂对水中磺胺二甲基嘧啶的吸附特性

以强碱性阴离子交换树脂作为吸附剂,对模拟废水中的磺胺二甲基嘧啶进行吸附实验。静态吸附实验结果表明,温度为25℃,p H=7,磺胺二甲基嘧啶的初始浓度为10mg/L,吸附平衡时间为40min的条件下,强碱性阴离子交换树脂对磺胺二甲基嘧啶的吸附量为0.244mg/g。经准二级动力学方程拟合出的qe为0.263mg/g与实验所得值0.244mg/g接近,且相关系数R~2=0.9991,能较好地描述强碱性阴离子交换树脂对SM2的吸附行为。通过Langmuir吸附模型拟合的qm为0.274mg/g,与实验值更接近,且R~2=0.9972。吸附动力学和吸附热力学的分析表明,强碱性阴离子交换树脂对磺胺二甲基嘧啶的吸附行为是物理吸附为主的单分子层吸附。而动态吸附实验结果表明,当温度为25℃,p H=7,磺胺二甲基嘧啶的初始浓度为10mg/L时,动态吸附穿透时间为250min,吸附饱和时间为670min,动态吸附过程中强碱性阴离子交换树脂对磺胺二甲基嘧啶的最大吸附量为0.231mg/g。     

超声法加入柠檬酸制备分子筛及其性能研究

以化学试剂为原料,在传统水热合成法的基础上,采用超声波法外加助剂(柠檬酸),通过改变柠檬酸的用量、晶化时间和晶化温度设计三水平三因素正交试验合成4A分子筛,采用XRD、SEM、FI-IR及钙离子交换性等方法进行分析表征,并探讨了制备4A分子筛的最优条件。结果表明,4A分子筛制备的最优条件为:晶化温度70℃,柠檬酸/Al_2O_3=0.75(摩尔比),晶化时间4h。4A分子筛对钙离子交换的Langmuir吸附等温方程为q=0.00012x/(1+0.024x)。钙交换能力达到310.71mg CaCO_3/g,钙离子交换的最佳吸附时间为1h,最佳吸附温度为35℃。     

交联聚丙烯酸固载化氧化β-环糊精的合成及其对尿素的吸附性能

大孔交联聚丙烯酸树脂(D151和D152)用氯化亚砜转化为酰氯后,通过成酯反应固载β-环糊精,再进一步用高碘酸钠氧化,合成出具有环状多醛结构的交联聚丙烯酸固载化氧化β-环糊精。系统研究了反应条件对β-环糊精固载化反应的影响,发现摩尔投料比(—COC1/β-CD)为1.5—1/1、温度80℃、时间24 h为最佳固载反应条件。探讨交联聚丙烯酸固载化氧化β-环糊精对尿素的吸附性能,阐明了吸附时间、溶液中尿素浓度、及介质pH值等对吸附量的影响。在尿素浓度130 mg/dL、吸附时间4h、介质pH 7、温度25℃时,交联聚丙烯酸固载化氧化β-环糊精对尿素呈现出最大吸附量82.13 mg/g。     

N-硫代酰基硫乙酸功能化三乙撑四胺交联PVC树脂的制备及对Hg~(2+)的吸附

以聚氯乙烯为原料依次与四乙烯五胺、CS_2和ClCH_2COONa反应合成了一种新的含N、O、S的N-硫代酰基硫乙酸功能化三乙撑四胺交联聚氯乙烯螯合树脂,树脂结构经红外分析和元素分析表征. 探讨了在不同pH值、Hg~(2+)初始浓度、吸附温度和时间等条件下合成树脂对Hg~(2+)的吸附性能. 结果表明,螯合树脂对Hg~(2+)有较快的吸附速率,pH值约为2.0时,树脂对Hg~(2+)的吸附效果最好,随温度升高吸附量逐渐增大. 温度在35 ℃、Hg~(2+)起始浓度为17.66 mmol/L时,树脂对Hg~(2+)的吸附量可达3.330 mmol/g. 树脂对Hg~(2+)的吸附符合Langmuir和Freundlich等温式. 用0.2 mol/L HNO3-10%硫脲对吸附后的树脂进行洗脱,脱附率达99.20%.     

Fe3O4/菹草磁性材料的制备及对刚果红吸附研究

本研究以菹草为原料,采用化学共沉淀方法制备Fe3 O4/菹草磁性纳米材料并应用于刚果红染料的吸附实验中.探究了pH、吸附时间、吸附剂用量、温度四个因素对吸附效果的影响.研究结果表明:该材料吸附刚果红的最佳条件为初始浓度为20 mg·L-1时,pH值为5,吸附剂投加量0.2 g,吸附时间4 h及温度为30℃;在最佳吸附条...     

胺基化壳聚糖树脂吸附分离茶多酚的研究

对珠状壳聚糖树脂进行胺基化改性,制备了胺基化珠状壳聚糖树脂,并用FTIR对胺基化珠状壳聚糖树脂进行了结构表征。利用该树脂对绿茶中茶多酚进行吸附分离,探讨了其吸附条件,考察了其吸附性能。结果表明,胺基化壳聚糖树脂对茶多酚的吸附既符合Langmuir等温式,也符合Freundlich等温式;本实验最佳吸附条件为:温度25℃,茶汤溶液pH值5,吸附时间2h;最大吸附量达到486.0mg/g。     

吸附树脂分离纯化桑叶中1-脱氧野尻霉素的研究

通过亚临界水法提取桑叶中的1-脱氧野尻霉素(1-deoxynojirimycin)(DNJ)。比较AB-8树脂与732树脂以及这两种树脂联用对桑叶提取液中DNJ的纯化效果。结果表明,在洗脱剂为60%乙醇溶液、样品液pH值为7、吸附时间6h、解吸时间2h、动态吸附与解吸速度均为2BV/h的条件下,AB-8树脂的平衡吸附率为37.2%,解吸率为84.8%,所得DNJ含量为2.37mg/g,较原提取液提高2.9倍。在洗脱剂为0.5mol/L氨水溶液、样品液pH值为4、吸附时间8h、解吸时间4h、动态吸附与解吸速度均为2BV/h的条件下,732型阳离子树脂的平衡吸附率为31.3%,解吸率为78.1%,所得DNJ含量为3.134mg/g,较原提取液提高3.8倍。联合使用两种树脂,所得DNJ含量为9.48mg/g,较原提取液提高11.5倍。     

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.     

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。     

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.

     

Synthesis of phenolic components of Grains of Paradise

Two vanilloids, (5E)-8-(4-hydroxy-3-methoxyphenyl)oct-5-en-4-one (1) and 4-[3-hydroxydecyl]-2-methoxyphenol (2), isolated from the dried seeds of Grains of Paradise (Aframomum melegueta), were synthesized; the latter compound was made as the S-enantiomer and the material derived from the seeds was found to be a 1:1.7 mixture of the R and S isomers. The synthetic route used should allow the preparation of analogs having extended alkyl chains and consequently different lipophilicity, and 3, a homolog of 2, was also prepared.     

Summary of development of the theory of stability of colloids and thin films

In this review, the research of the author in the field of colloidal systems is summarized. The factors influencing colloidal stability are systematized and analyzed. Examples are presented to illustrate the practical utilization of the theory of stability of colloids and thin films.This review was prepared on the basis of the works of the author, which were awarded the State Premium for 1991 in the field of science and technology, chemistry section.Institute of Physical Chemistry, Russian Academy of Sciences, 117915 Moscow. Translated from Izvestiya Akademii Nauk, Seriya Khimicheskaya, No. 8, pp. 1708–1717, August, 1992.     

Study of hydration of two cements of different strengths

Main hydration products of two cement pastes, i.e. CSH-gel, portlandite (P) (and specific surface S) were studied by static heating, and by SEM, TEM and XRD, as a function of cement strength (C-33 and C-43) hydration time (th) and subsequent hydration in water vapour.Total change in mass on hydration and air drying, M_o, increased with strength of cement paste and with hydration time. Content of water escaping at 110 to 220°C, defined as water bound with low energy, mainly interlayer and hydrate water, was independent on cement strength but its content increased with (th). Content of chemically bound (zeolitic) water in CSH-gel, escaping at 220-400°C, was slightly dependent on strength and increased with (th). It was possibly derived from the dehydroxylation of CSH-gel and AFm phase. Portlandite water, escaping at 400-500°C, was independent on cement strength and was higher on longer hydration. Large P crystals were formed in the weaker cement paste C-33. Smaller crystals were formed in C-43 but they increased with (th). Carbonate formated on contact with air (calcite, vaterite and aragonite), decomposed in cement at 600-700^oC. It was high in pastes C-33(1 month) and C-43(1 month), i.e. 5.7 and 3.3%, respectively; it was less than 1% after 6 hydration months (low sensitivity to carbonation) in agreement with the XRD study showing carbonates in the air dry paste (1month), and its absence on prolonged hydration (6 months) and on acetone treatment. Water vapour treatment of (6 months) pastes or wetting-drying increased this sensitivity.Nanosized P-crystals, detected by TEM, could contribute to the cement strength; carbonate was observed on the rims of gel clusters.This revised version was published online in November 2005 with corrections to the Cover Date.     

氯氧化镁生成热的研究

用氧化镁氯化镁水溶液制备了8水合氯氧化镁[nMg(OH)2·MgCl2·8H2O], 并测定了其在盐酸中的溶解热, 实验结果表明, 氯氧化镁溶解热与n值呈线性关系, 根据溶解热求出5Mg(OH)2·MgCl2·8H2O和3Mg(OH)2·MgCl2·8H2O的生成热分别为-7727.1和5888.1kJ·mol^1^-。     

Thermodynamics of the formation of oxosulfides of rare-earth elements

The enthalpies of solution of several oxosulfides of rare-earth elements and the high-temperature enthalpies of oxosulfides and oxosulfates of lanthanum and yttrium were measured using solution calorimetry and high-temperature microcalorimetry techniques. Standard enthalpies of formation and some thermodynamic properties of oxosulfides and oxosulfates were calculated. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 2 pp. 294–297, February, 1997.     

探究“铁的锈蚀条件”实验创新设计

设计了铁的锈蚀实验,说明了铁钉的处理方法,增加了温度、酸、碱的影响条件,实现了铁跟蒸馏水及空气中氧气快速反应而生锈,使实验在5 min左右就能够得到准确的结果。