间歇式水热合成制备丝光沸石膜及其异丙醇脱水应用

采用市售廉价大孔α-Al₂O₃管作为基质材料，通过热浸渍法在管外表面涂敷晶种，随后在无模板剂体系下，利用新型的间歇式水热合成法制备丝光沸石膜。对比了传统加热和间歇式加热对丝光沸石膜形貌、结构及渗透蒸发异丙醇脱水分离性能的差异。考察了合成液中Na₂O/SiO₂、SiO₂/Al₂O₃和NaF/SiO₂物质的量之比在间歇式水热合成下对丝光沸石膜的影响。研究结果表明，当合成液中Na₂O/SiO₂、SiO₂/Al₂O₃和NaF/SiO₂物质的量之比分别为0.24、16.7和0.25时，制备的丝光沸石膜渗透蒸发异丙醇脱水分离性能最佳，在75℃下，对异丙醇/水(9∶1，w/w)的渗透通量达5.60 kg·m^-2·h^-1，水对异丙醇的分离因数大于10 000。     

猪卵核移植的研究

以湖北白猪为受体，杜洛克为供体进行了猪卵核移植的研究．结果表明，半胱氨酸对卵具有保护作用；卵龄对核移植效率有显著影响，以４２～４８ｈ为宜；激活后卵母细胞做受体可提高移核胚的发育率；供体核发育期对移核胚的发育有显著影响．核移植后的重组胚移入受体后，经体内发育得到了５只核移植仔猪．     

Pervaporation as a Separation Technique for Direct Determination of Volatile Selenium Species by Atomic Fluorescence Spectrometry

Abstract

This paper reports for the first time a suitable way to determine methylated selenium compounds using the new approach of pervaporation coupled to atomic fluorescence spectrcmetry (PV-AFS).

The method developed allows direct extraction, separation, preconcentration and determination of dimethylselenium (DMSe) and dimethyldiselenium (DMDSe) from slurry samples. Under the optimum conditions, the detection limits (LODs) were found to be 0.66 ng and 0.39 ng for DMSe and DMDSe, respectively, the precision being about 6–9 % for 10 ng mL as selenium concentration. The linearity ranges were from the LOD to 0.7 μg mL^?1 for DMSe and from the LOD to 0.4 μg mL^?1 for DMDSe (as Se). The pervaporation efficiencies were 55 ± 1 % and 85 ± 5 % for DMSe and DMDSe, respectively. The proposed method was successfully applied to determine methylated selenium species in sewage sludge, garlic and oyster samples. The concentrations found were from 0.07 to 1.42 μg g^?1.

As no certified reference materials are available for these analytes, validation was carried out by recovery studies in these matrices, and the results showed that the proposed method performed satisfactorily.     

两步变温晶种法制备丝光沸石膜及其渗透汽化乙酸脱水性能

在水热晶种法基础上采用两步变温晶化以高水硅比(n_H2O/n_SiO2)稀溶液配方为合成液,研制用于渗透汽化(PV)乙酸脱水的丝光沸石膜(MOR膜),考察了变温晶化各段时间、水硅比与氟离子对 MOR膜的形貌与分离性能的影响规律。结果表明：高温段晶化时间、水硅比与氟离子对MOR膜的形貌、结晶度和膜层厚度产生显著影响,并影响MOR膜渗透气化分离性能;在高温段(150 ℃)和低温段(120 ℃)的晶化时间分别为 18和 6 h,在水硅比为 60且含氟离子体系中所制备的 MOR膜的性能最佳,其对质量分数50%的乙酸水溶液的渗透通量和分离系数分别为1.45 kg·m^-2·h^-1和1 008。     

NaA分子筛膜的制备及其渗透蒸发性能

采用喷涂法在多孔α-Al2O3载体上制备了NaA分子筛膜(M),其结构和形貌经SEM和XRD表征。对M的渗透蒸发性能进行了研究,结果表明:喷涂时间和晶种浓度是影响M渗透蒸发性能的关键因素。在喷涂时间为30 s,晶种浓度为1 wt%的最佳条件下制备的M,在348 K时对90 wt%乙醇的渗透通量为2.64kg·m-2·h-1,分离因子>10 000。     

Synthesis of Polyimides Containing Fluorine and Their Pervaporation Performances to Aromatic/Aliphatic Hydrocarbon Mixtures

Two kinds of polyimides containing fluorine were synthesized based on dianhydride of 2,2‐bis(3,4‐dicarboxyphenyl)hexafluoropropane dianhydride (6FDA) and diamines including 2,2‐bis[4‐(4‐aminophenoxy)phenyl] hexafluoropropane (BDAF) and 2,2‐bis[4‐(4‐aminophenoxy)phenyl]propane (BAPP) using solution condensation and following chemical imidization. The structures of 6FDA‐BDAF and 6FDA‐BAPP were characterized by FT‐IR, NMR, and XRD. Their glass transition temperatures characterized by DSC were in the range of 235–251°C, and the initial decomposition temperatures determined by TGA were over 540°C. The membranes of polyimide thus obtained were employed in pervaporation separation of aromatic/aliphatic mixtures. 6FDA‐BDAF membranes obtained better separation performances than 6FDA‐BAPP and had a flux of 0.66 kg · µm/m² · h and separation factor of 6.49 for toluene/n‐heptane (20/80 wt.%) at 80°C. The effects of the fluorine group on polyimides properties and separation performances were investigated.     

微波辅助加热法制备NaA沸石膜及其性能研究的综合化学化工实验*

结合自身实验教学和科研实验经验,设计了一个包括NaA晶种管的制备,微波辅助加热法制备NaA沸石膜,膜渗透汽化性能测试及膜材料微结构表征等过程的综合化学化工实验。本实验涵盖绿色合成、性能测试、表征及膜分离单元操作,知识要点多、学科覆盖面广,有助于提高学生的实践操作能力、创新意识和综合运用知识的能力,适合作为学生综合性实验。     

多孔α-Al_2O_3载体上Silicalite-1膜的表面改性与选择性透醇分析

分别使用十二烷基三甲氧基硅烷(DMS)和硬脂酸(STA)对α-Al2O3载体上二次生长合成的silicalite-1膜进行修饰,提高其表面疏水性。红外光谱和接触角测试结果表明,改性剂以化学键的形式结合于分子筛膜表面,膜表面由亲水变为疏水。表面改性的最佳预处理温度为150℃,改性剂的最佳质量分数为10%。进一步研究了膜表面润湿特性和热稳定性,其中DMS改性后的分子筛膜在空气中经250℃高温处理后仍保持疏水性不变。在乙醇/水分离应用中,高温脱除模板剂后缺陷的孔径分布在1~5nm,表面改性后乙醇分离因子较改性前提高5倍,最高可达21.6。     

A Graphene Oxide Membrane with Highly Selective Molecular Separation of Aqueous Organic Solution

A graphene oxide (GO) membrane is supported on a ceramic hollow fiber prepared by a vacuum suction method. This GO membrane exhibited excellent water permeation for dimethyl carbonate/water mixtures through a pervaporation process. At 25 °C and 2.6 wt % feed water content, the permeate water content reached 95.2 wt % with a high permeation flux (1702 g m^?2 h^?1).