在高压下规整填料中的流动实验研究

Both distillation performance and hydrodynamic study for backmixing by tracer technique were carried out in a high-pressure packed column with 0.15 m inner diameter over a wide range of operating conditions. Isobutane and n-pentane are employed as test mixture in the distillation experiment and air/water is used for the hydrodynamic study. The column is installed with Mellapak 350Y structured packing and the total packing height is 2.0 m. With the increasing operating pressure, the separation efficiency increases slightly while the F-factor corresponding to the maximum efficiency at each pressure is descending. It is noted that, at all operating pressures, with the increase of F-factor, the packing efficiency is slightly higher up to the flooding point. The application of SRP model to high-pressure distillation gives much lower values of HTUOG than those obtained experimentally. An additional term, the height of mixing unit, is introduced to correct the SRP model and improve its accuracy at high pressure. From the tracer experiments, the height of mixing unit for gas phase was found to be larger than that for the liquid phase. From this viewpoint, it is believed that the gas phase backmixing gives more unfavorable influence on the separation efficiency in comparison with liquid phase.     

Interfacial Properties of Ethyl Cellulose/Cellulose Acetate Blends by HPLC

The high performance liquid chromatography method (HPLC) with ethyl cellulose/cellulose acetate (EC/CA) blends and EC as column packing material, and small molecular weight compound as probe molecules was employed to measure the retention volume (VR) and equilibrium distribution coefficient (K) of both inorganic and organic solutes. The interfacial separation properties of EC/CA blends were characterized by the HPLC data. The effects of the blends on the interfacial adsorption properties, hydrophilicity, affinity, polar and non-polar parameters of EC membrane materials were studied subsequently. The research results indicate that the interfacial adsorption properties and hydrophilicity of EC have been improved by solution blending with CA. The alloys are superior to EC in the separation efficiency for non-dissociable polar organic solute. The EC/CA alloy (80:20, w) is suitable for desalting and desaccharifying.     

Analysis of ionogenic surfactants by HPLC with ion-pair extraction detector

A technique for developing a selective and highly sensitive detection method was studied, which responds to particular ionogenic surfactants using a system of connecting the post-column reaction detector with a high performance liquid chromatograph (HPLC). HPLC conditions used for the separation were: column packing and size, TSK-LS410 (5μ) and 6 mm i.d. × 250 mm; mobile phase, a mixture of methanol, water, sodium perchlorate and phosphoric acid. A Technicon AutoAnalyzer II system was used as the post-column reaction detector. Orange II was used to form the hydrophobic ion-pair complexes for cationic and amphoteric surfactants, and Methylene blue for anionic surfactants. By this method, cationic, amphoteric and anionic surfactants were easily identified in the chromatograms. The analytical results of their homolog distributions were in good agreement with those obtained by conventional gas chromatographic (GC) methods.     

加压下规整填料塔内气液两相轴向返混实验研究

An experimental study of the extent of axial backmixing in both gas and liquid phases was conducted in a 150 mm ID column packed with Mellapak 250Y corrugated structured packing. The column was operated at pressures ranging from 0.3 MPa to 2.0MPa with nitrogen and water flowing countercurrently through the packing. The amount of axial backmixing was experimentally evaluated by the pulse response techniques using hydrogen in gas phase and an aqueous solution of NaCl in liquid phase as inert tracers. The response of the tracer was monitored by means of thermal conductivity in the gas phase and electrical conductance in the liquid phase. The experimentally determined residence time distribution (RTD) curves were interpreted in terms of the diffusion-type modei. The results indicated that the axial backmixing in the gas increased notably with gas flowrate and slightly with operating pressure and liquid flowrate. The liquid-phase axial backmixing was an increasing function of both gas and liquid flowrates an     

加压下填料塔中液相轴向反混的研究

Liquid phase axial mixing was measured with the tracer technique in a packed column with inner diameter of 0.15m,in which the structured packing,Mellapak 350Y,was installed.Tap water as the liquid phase flowed down through the column and stagnant gas was at elevated pressure ranging from atmospheric to 2.0MPa.The model parameters of Bo andθwere estimated with the least square method in the time domain.As liquid flow rate was increased,the liquid axial mixing decreased.under our experimental conditions,the effect of pressure on Bo number on single liquid phase was negligible,and eddy diffusion was believed to be the primary cause of axial mixing in liquid phase.     

Liquid–liquid equilibrium extraction of ethanol with mixed solvent for bioethanol concentration

The extraction of ethanol with the solvents of aldehydes mixed with m-xylene was studied for the bioethanol concentration process.Furfural and benzaldehyde were selected as extraction solvents,with which the solubility of water is small,expecting large distribution coefficient of ethanol.The liquid–liquid two-phase region was the largest with m-xylene solvent,followed by benzaldehyde and furfural.The region of two liquid–liquid phase became larger with the mixed solvent of m-xylene and furfural than that with furfural solvent.The NRTL model was applied to the ethanol–water–furfural–m-xylene system,and the model could well express the liquid–liquid equilibrium of the system.For any solvent used in this study,the separation selectivity of ethanol relative to water decreased as the distribution coefficient of ethanol increased.The separation selectivity with m-xylene was the largest among the employed solvents,but the distribution coefficient was the smallest.The solvent mixture of furfural and m-xylene showed relatively high distribution coefficient of ethanol and separation selectivity,even in the higher mass fraction of m-xylene in the solvent phase.The ethanol extraction with a countercurrent multistage extractor by a continuous operation was simulated to evaluate the extraction performance.The ethanol content could be concentrated in the extract phase with relatively small number of extraction stages but low yield of ethanol was obtained.     

高效液相色谱-蒸发光散射检测法分析蛋黄磷脂酰胆碱(英文)

Egg yolk phosphatidylcholine(EYPC) is being widely used in food and pharmaceutical industries nowadays owing to its surface activity,pharmaceutical usefulness,and so on.Common determination methods of phospholipids were based on the American Oil Chemists’ Society(AOCS) Official Method Ja7b-91,in which n-hexane/2-propanol/acetate buffer was used as the mobile phase.In order to achieve desired results,gradient elu-tion or buffer solution was used,which made the detection process more complicated.Moreover,water or buffer solution could affect the silica gel column both on its lifespan and the separation efficiency significantly.In this study,different mobile phase and detector were used to simplify EYPC analyzing process instead of using water within the mobile phase.The optimized HPLC operating conditions are as follows:pure methanol as a mobile phase,flow rate of 1.0 ml·min-1,silica gel column(250 mm×4.6 mm,5 μm,Inertsil GLTM),column temperature 30 ℃ and low temperature evaporative light scattering detector(40 ℃,0.35 MPa) as used.Under this optimal condition,the linear relative coefficient of the standard curve is 0.998 and the recovery was in the range of 96.83%-101.58% with a relative standard deviation of 1.79%(n=6).     

Physicochemical characterization of galactosyldiglycerides and their quantitation in wheat flour lipids by high performance liquid chromatography

A high performance liquid chromatographic (HPLC) method was developed for analyzing digalactosyldiglycerides (DGDG) and monogalactosyldiglyceride (MGDG) in polar lipids fractionated from lipid extracts of wheat or flour. Wheat lipid samples were prepared by solvent extraction, then fractionated on a silica gel packed open column. A Spherisorb ODS (octadecyl silane) column with methanol/water elution system was used for separation of glycolipids in the polar lipid fractions. The detection limit of the refractive index detector with interferometric optics was 0.25μg for both DGDG and MGDG. Separating on nonpolar bonded phase columns permitted us to differentiate, based on fatty acid composition and position, among components within the specific glycolipid classes. Semipreparative HPLC on analytical columns was used to subfractionate the polar lipids. The glycolipids were collected for functional group characterization. Approximately 35% of each DGDG subfraction was accounted for as carbohydrate. The absence of phosphorus precluded phospholipids. Fatty acid analysis by gas chromatography showed the first DGDG to be linoleic acid, whereas the second DGDG peak was composed of linoleic, oleic and palmitic acids. Mass spectrometric analysis of the first DGDG peak showed linoleic acid in both the SN-1 and 2 positions. Mass spectrometric analysis revealed that palmitic or oleic acid in the second peak was preferentially located on the SN-1 position; linoleic acid was on the SN-2 position. Contribution no. 80-207J, Department of Grain Science and Industry, Kansas Agricultural Experiment Station, Kansas State University, Manhattan, KS. Part of a dissertation submitted by T.N. Tweeten in partial fulfillment of the PhD degree. Honored Student Award Presentation at AOCS annual meeting, San Francisco, April 1979.     

Mass transfer characteristics in a rotating packed bed with split packing

The rotating packed bed (RPB) with split packing is a novel gas–liquid contactor, which intensifies the mass transfer processes controlled by gas-side resistance. To assess its efficacy, the mass transfer characteristics with adjacent rings in counter-rotation and co-rotation modes in a split packing RPB were studied experimentally. The physical absorption system NH3–H2O was used for characterizing the gas volumetric mass transfer coeffi-cient (kyae) and the effective interfacial area (ae) was determined by chemical absorption in the CO2–NaOH sys-tem. The variation in kyae and ae with the operating conditions is also investigated. The experimental results indicated that kyae and ae for counter-rotation of the adjacent packing rings in the split packing RPB were higher than those for co-rotation, and both counter-rotation and co-rotation of the split packing RPB were superior over conventional RPBs under the similar operating conditions.     

Numerical simulation and experimental study of the characteristics of packing feature size on liquid flow in a rotating packed bed

Rotating packed bed has high efficiency of gas–liquid mass transfer. So it is significant to investigate fluid motion in rotating packed bed. Numerical simulations of the effects of packing feature size on liquid flow characteristics in a rotating packed bed are reported in this paper. The particle image velocimetry is compared with the numerical simulations to validate the turbulent model. Results show that the liquid exists in the packing zone in the form of droplet and liquid line, and the cavity is droplet. When the radial thickness of the packing is less than 0.101 m, liquid line and droplets appear in the cavity. When rotational speed and radial thickness of the packing increase, the average diameter of the droplets becomes smaller, and the droplet size distribution becomes uniform. As the initial velocity of the liquid increases, the average droplet diameter increases and the uniformity of particle size distribution become worse. The droplet velocity increases with the radial thickness of the packing increasing, and gradually decreases when it reaches the cavity region. The effect of packing thickness is most substantial through linear fitting. The predicted and simulated values are within ±15%. The cumulative volume distribution curves of the experimental and simulated droplets are consistent with the R-R distribution.     

功能化Zr-MOF强化混合基质膜CO2分离

混合基质膜（MMMs）在气体分离领域具有良好的应用前景,金属有机框架（MOFs）由于具有高孔隙率和有机连接基团,常被用作填料制备MMMs。但由于MOFs与聚合物的界面相容性问题,MMMs的气体分离性能提升受到限制。本文合成了功能化的Zr-MOF（UiO-66-AC）,并利用其与聚醚共聚酰胺（Pebax）共同制备了混合基质膜。填料中引入的羰基和羧基等基团提供了MOFs与聚合物基质之间较强的界面相互作用。与纯Pebax膜相比,UiO-66-AC/Pebax MMMs的气体渗透性能得到了显著提高。当填料质量分数为6%时,膜的CO₂渗透系数为102.4 Barrer,CO₂/N₂和CO₂/CH₄选择性分别为90.6和26.0,CO₂/N₂分离性能突破了Robeson上限(2008),表明该混合基质膜在CO₂的分离应用上具有潜力。     

UiO-66的制备、功能化及膜分离研究进展

UiO-66是一种具有优异物理化学稳定性的金属有机骨架（MOFs）材料,近年来引起了研究者们的强烈关注。本文详细介绍了UiO-66的结构,重点探讨了溶剂热法过程中的一系列影响因素,包括使用不同的金属前体,改变合成温度、溶剂、各组分配比以及模板剂等,制备各种性能的UiO-66。针对溶剂热法合成效率较低的问题,介绍了微波合成法、微流控、连续流和无溶剂法等其它UiO-66的制备方法。为了扩大UiO-66的应用范围,对其有机配体进行功能化改性或与其他材料复合改性,具体介绍了改性后UiO-66在气体吸附、水处理、催化、电化学和化学传感等方面的应用。最后综述了利用UiO-66具有多孔特性构建分离膜方面的研究进展,具体阐述了纯UiO-66膜和UiO-66复合膜在气体分离和水处理方面的应用。     

Integrating of metal-organic framework UiO-66-NH2 and cellulose nanofibers mat for high-performance adsorption of dye rose bengal

UiO-66-NH₂ is an efficient material for removing pollutants from wastewater due to its high specific surface area, high porosity and water stability. However, recycling them from wastewater is difficult. In this study, the cellulose nanofibers mat deacetylated from cellulose acetate nanofibers were used to combine with UiO-66-NH₂ by the method of in-situ growth to remove the toxic dye, rose bengal. Compared to previous work, the prepared composite could not only provide ease of separation of UiO-66-NH₂ from the water after adsorption but also demonstrate better adsorption capacity (683 mg∙g^‒1 (T = 25 °C, pH = 3)) than that of the simple UiO-66-NH₂ (309.6 mg∙g^‒1 (T = 25 °C, pH = 3)). Through the analysis of adsorption kinetics and isotherms, the adsorption for rose bengal is mainly suitable for the pseudo-second-order kinetic model and Freundlich model. Furthermore, the relevant research revealed that the main adsorption mechanism of the composite was electrostatic interaction, hydrogen bonding and π–π interaction. Overall, the approach depicts an efficient model for integrating metal-organic frameworks on cellulose nanofibers to improve metal-organic framework recovery performance with potentially broad applications.     

Construction of defect-containing UiO-66/MoSe2 heterojunctions with superior photocatalytic performance for wastewater treatment and mechanism insight

Metal–organic frameworks are recognized as promising multifunctional materials, especially metal–organic framework-based photocatalysts, which are considered to be ideal photocatalytic materials. Herein, a new type of UiO-66/MoSe₂ composite was prepared using the solvothermal method. The optimum composite was selected by adjusting the mass ratio of UiO-66 and MoSe₂. X-ray diffraction analysis showed that the mass ratio influenced the crystal plane exposure rate of the composite, which may have affected its photocatalytic performance. The composite is composed of ultra-thin flower-like MoSe₂ that wrapped around cubic UiO-66, a structure that increases the abundance of active sites for reactions and is more conducive to the separation of carriers. The photocatalytic properties of the composite were evaluated by measuring the degradation rate of Rhodamine B and the catalyst’s ability to reduce Cr(VI)-containing wastewater under visible light irradiation. Rhodamine B was decolorized completely in 120 min, and most of the Cr(VI) was reduced within 150 min. The photochemical mechanism of the complex was studied in detail. The existence of Mo⁶⁺ and oxygen vacancies, in addition to the Z-type heterojunction promote the separation of electrons and holes, which enhances the photocatalytic effect.     

BiOBr/UiO-66-（COOH）2复合材料制备及光催化性能研究

为提高传统光催化材料BiOBr和UiO-66-（COOH）₂的性能和对可见光的吸收强度,以及它们的光催化活性和光催化效率,通过简单的溶剂热法制备了一种新型复合光催化剂BiOBr/UiO-66-（COOH）₂。运用X射线衍射光谱（XRD）、扫描电镜（SEM）、透射电镜（TEM）、红外光谱（FT-IR）、光致发光（PL）光谱、N₂吸附-脱附、紫外-可见漫反射光谱（UV-Vis DRS）和电化学等手段对其进行表征,并对其光催化降解甲基橙的效率进行了研究。结果表明,相对于单一的BiOBr材料,与UiO-66-（COOH）₂复合之后的BiOBr/UiO-66-（COOH）₂催化剂保留了原有材料的结构,相应的比表面积增大,对可见光的吸收强度增强。将BiOBr/UiO-66-（COOH）₂用于光催化降解甲基橙,在氙灯照射120 min后,甲基橙的降解率达到70%,分别约为纯UiO-66-（COOH）₂和BiOBr的3.68倍和1.43倍,光催化活性显著提高,光催化降解过程符合一级反应动力学规律。     

DRYING OF AIR IN SILICA GEL PACKED COLUMNS

Silica gels that were made humidity indicating by impregnation of CoCl₂ were used for air drying in isothermal packed column. The effects of type of silica gel, packing height, particle size and air flow rate on breakthrough curves were studied. The breakthrough curves predicted by Rasmuson and Neretniek's analytical solution were in good agreement with experimental data.     

高稳定铪金属-有机骨架材料的合成及二氧化碳捕获性能

采用高温高浓度的溶剂热方法,合成了具有高结晶度的一种金属-有机骨架（metal-organic framework,MOF）材料UiO-66（Hf）,并发现该材料在沸水、酸碱等苛刻条件下具有非常好的化学稳定性。为了提高其对气体的吸附分离性能,进一步采用具有不同官能团的有机配体--氨基对苯二甲酸（H₂BDC-NH₂）、硝基对苯二甲酸（H₂BDC-NO₂）、溴对苯二甲酸（H₂BDC-Br）,设计合成了孔道表面具有不同化学性质的三种新型铪MOF材料,且这些材料与UiO-66（Hf）具有相同的拓扑结构。同时,气体吸附实验结果表明,极性基团的引入,尤其是氨基的引入,能极大提高材料对CO₂/N₂以及CO₂/CH₄体系的分离性能。这为以后应用于化工体系分离的新型多孔材料合成提供了理论指导。     

Influence of exchanged cations (Na, Cs, Sr and Ba) on xylene permeation through ZSM-5/SS tubular membranes

Na-ZSM-5 membranes were synthesized by secondary growth on the outer surface of stainless steel porous tubes. The membranes were ion-exchanged with Cs⁺, Ba²⁺ and Sr²⁺ to investigate their effect upon the separation of p-xylene from m-xylene and o-xylene. The permeation through the membranes was measured between 150 and 400 °C using each xylene isomer separately and a ternary mixture. All the membranes were selective to p-xylene in the temperature range studied. N₂ and xylene permeation measurements together with SEM observations were used to determine whether or not cracks and/or pinholes developed after exposure to the xylene isomers at high temperature (400 °C). Neither pore blockage nor extra-zeolitic pores developed after the ion exchange procedure and subsequent calcination. Furthermore, duplicate synthesized membranes of each cation form had similar separation factors and permeances. The duplicate values differ much less than the measurement error. The p-xylene permeation flux decreased in the order: Na-ZSM-5 > Ba-ZSM-5 > Sr-ZSM-5  Cs-ZSM-5 while the permeation flux of the m- and o-xylene decreased in the order Na-ZSM-5 > Sr-ZSM-5 > Ba-ZSM-5 > Cs-ZSM-5. The membrane that exhibited the best performance was Ba-ZSM-5, with a maximum p/o separation factor of 8.4 and a p-xylene permeance of 0.54 × 10⁻⁷ mol s⁻¹ m⁻² Pa⁻¹ at 400 °C.     

An integrated system of biological and catalytic oxidation for the removal of o-xylene from exhaust

Biofiltration is an efficient technology for treatment of gaseous waste. Its disadvantages, however, include large volume of bioreactor and slow adaptation to fluctuating concentrations in waste gas. Catalytic oxidation offers a high destructive efficiency at relatively low operating temperature and small unit. A bench scale system integrated with a biofilter and a catalytic oxidation unit for the treatment of gases containing o-xylene was investigated in this study. The catalytic oxidation unit was packed with Cu/Al₂O₃ catalyst. The results showed that 90% of o-xylene could be removed in the biofilter at the load below 38.2 g m⁻³ h⁻¹. High o-xylene concentration in inlet gas resulted in an overload of the biofilter. Using the Cu/Al₂O₃ catalytic oxidation unit, the concentration of o-xylene could be reduced evidently. The combination of the chemical and microbial processes not only led to a high and stable efficiency of o-xylene conversion, but also improved capacity resisting the shock loads. The Cu/Al₂O₃ was studied for o-xylene oxidation in temperature range of 90–320 °C. The o-xylene conversion was improved correspondingly with the increasing of oxidation temperature. The reaction mechanism of o-xylene oxidation on Cu/Al₂O₃ was also investigated using diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS).     

Liquid chromatographic separation of xylene isomers on α-cyclodextrin bonded phases

Mesoporous glass beads and silica were modified with α-cyclodextrin (CD) for the separation of xylene isomers by means of direct bonding, linking spacer group, and cross-linking agent. The separation efficiency of the (α-CD modified silica particles was tested by using simple column chromatography. A strong inclusion complex formation of p-xylene was observed from the column packed with α-CD bonded phases. Spacer group and crosslinking agent decreased the formation of the inclusion complex of p-xylene and increased selectivity between m-xylene and o-xylene. The inclusion complex formation of p-xylene was strongly diminished when the mobile phase was switched from methyl alcohol to toluene. The column packed with the cross-linked a-CD bonded silica showed the best performance in the separation of xylene isomers.