Liquid-phase esterification of methacrylic acid with methanol catalyzed by cation-exchange resin in a fixed bed reactor:Experimental and kinetic studies

The kinetic behavior of esterification between methacrylic acid and methanol catalyzed by NKC-9 resin was studied in a fixed bed reactor.The reaction was conducted in the temperature range of 323.15 to 368.15 K with the molar ratio of reactants from 0.8 to 1.4 under certain pressure.The measurement data were regression with the pseudo-homogeneous(P-H),Eley-Rideal(E-R),and Langmuir-Hinshelwood(L-H)heterogeneous kinetic models.Independent adsorption experiments were implemented to gain the adsorption equilibrium constants of four components.Among the above three models,the L-H model exhibited the best fitting results.The stability of NKC-9 was evaluated by long-term running with the yield of methyl methacrylate no decrease during 3000 h operation.The structure and physicochemical properties of the new and used catalyst were performed by several characterizations including thermogravimetric analysis(TG),scanning electron microscope(SEM),X-ray diffraction(XRD)and Fourier transform infrared spectroscopy(FT-IR)and so on.

Denatured Thermodynamics of Proteins in Weak Cation-exchange Chromatography

The thermostability of some proteins in weak cation-exchange chromatography was investigated at 20-80 ℃. The results show that there is a fixed thermal denaturation transition temperature for each protein. The appearance of the thermal transition temperature indicates that the conformations of the proteins are destroyed seriously. The thermal behavior of the proteins in weak cation-exchange and hydrophobic interaction chromatographies were compared in a wide temperature range. It was found that the proteins have a higher thermostability in a weak cation-exchange chromatography system. The thermodynamic parameters(Δ H 0, Δ S 0) of those proteins were determined by means of Vant Hoff relationship(ln k -1/ T ). According to standard entropy change(Δ S 0), the conformational change of the proteins was judged in the chromatographic process. The linear relationships between Δ H 0 and Δ S 0 can be used to evaluate 'compensation temperature'( β ) at the protein denaturation and identify the identity of the protein retention mechanism in weak cation-exchange chromatography.

Elution Behaviour of Monocarboxylic Acids on a Cation-exchange Resin Column

The retention mechanism of monocarboxylic acids on a cation-exchange resin column was investigated. It was assumed that both Donnan membrane equilibrium and adsorption equilibrium were involved in the chromatographic process. On the basis of the proposed mechanism, an equation was derived for correlating distribution coefficient, Kd, dissociation constant, Aa, and adsorption equilibrium constant, K, of the analyzed acid. By this approach, retention data for some aliphatic acids under different operating conditions were predicted. Results are reasonably in agreement with experiment.

Impact of Hydrogen Ion Concentration on Amino Acids Composition of Macadamia Protein: Approached Using Cation-Exchange Chromatography

In the present context, the objective of this study was to synthesize and analyze the content of AA of macadamia protein and the impact of hydrogen ion concentration (pH) on AA composition. The determination of AA mainly by cation-exchange chromatography was also investigated. Reproducible and reliable techniques for quantification and identification of AA usually require derivatization. However, techniques such as AA analyzer are composed of cation-exchange chromatography and other components can sideline the derivatization with significant accuracy. The present analysis revealed a higher concentration of essential amino acids especially acidic AA, Glu and Asp and basic AA, Arg than other AA in macadamia protein. The study constitutes first report of use of bubble chart for evaluation of AA and explaination of AAS. The results may elaborate that the degradation of AA of macadamia protein for extraction of pH 11 is caused by the impact of pH. Moreover, the nutritional values of AA present in macadamia protein could change for the better by adjusting pH of extraction.

Transport Properties of Novel Hybrid Cation-Exchange Membranes on the Base of MF-4SC and Halloysite Nanotubes

The diffusion permeability through new hybrid materials based on a Nafion-type membrane (MF- 4SC) and nanotubes of halloysite is investigated using the Nernst-Planck approach. A method of quantitative evaluation of physicochemical parameters (averaged and individual diffusion coefficients and averaged distribution coefficients of ion pairs in the membrane) of system “electrolyte solution—ion-exchange membrane—water”, which was proposed earlier, is further developed. The parameters of hybrid membranes on the base of MF-4SC and nanotubes of halloysite (5% wt and 8% wt) are obtained from experimental data on diffusion permeability of NaCl solutions using theoretical calculations. New model of three-layer membrane system can be used for refining calculated results with taking into account both diffusive layers. It is shown that adding of halloysite nanotubes into the membrane volume noticeably affects exchange capacity as well as structural and transport characteristics of original perfluorinated membranes. Hybrid membranes on the base of MF-4SC and halloysite nanotubes can be used in fuel cells and catalysis.

云南某煤系硫铁矿煤硫综合回收工艺研究

为了有效利用云南某地煤系硫铁矿,采取选煤与选硫铁矿的综合回收方案。在矿石化学多元素分析以及硫形态分析的基础上,进行了螺旋溜槽—摇床重选试验、浮选试验。试验最终采用浮选闭路试验流程,先浮选煤,单独浮选出中矿(该产品并入尾矿),再浮选硫铁矿,最后得到了产率5.38%,碳品位40.32%,含硫7.05%,碳回收率33.76%的煤精矿;产率24.00%,硫品位47.59%,含碳9.64%,硫回收率72.74%的硫精矿,实现了煤和硫铁矿综合回收的目的。

氢同位素纯化分离用钯基膜的研究

本文介绍了氢同位素纯化、分离用钯合金膜的制备技术、种类及其应用情况。根据实际应用情况并分析其优缺点，钯基复合膜其综合性能优异成为今后钯基膜的发展方向，同时还要研发机械强度和耐热性更高的膜支撑体及低成本钯基膜的制备方法，探索高使用寿命、高透过率的新型复合膜。

阳离子交换分离—最小二乘法分光光度同时测定矿石中铌钽

用酒石酸、盐酸混合液作洗脱剂,阳离子交换树脂将矿石中的铌和钽与其它金属元素分离,洗下的铌、钽在盐酸—酒石酸介质中用5-Br-PADAP显色,用最小二乘法处理混合液的分光光度数据,建立浓度与吸光度间的最小二乘法数学模型。文中还对铌钽矿石进行分析,同时与二波长联合分光光度法比较,结果良好。

双水相提取新疆圆柏果实中的总黄酮及抑制亚硝化反应的研究

本文采用超声集成丙醇-硫酸铵双水相体系提取新疆圆柏果实中总黄酮,并用分光光度法测定其含量。探讨了丙醇-硫酸铵双水相(醇-水)体系的形成及提取条件对总黄酮得率的影响,得到的最优条件为:醇-水比0.8∶1,硫酸铵的量8g,料液比1∶50;超声时间40min。结果表明,该方法可有效地从新疆圆柏实中提取总黄酮,在最优条件下提取率为11.33mg/g。在此条件下,圆柏果实总黄酮提取液对亚硝化反应的抑制能力接近抗坏血酸。

A convenient preparation of ethoxymethoxymethane and its effect on the solubility of methanol/gasoline blends

Ethoxymethxoymethane （EMM） was conveniently prepared by acetalization of aqueous formaldehyde with methanol andethanol in a batch reactive distillation mode using a cation-exchange resin catalyst for the first time. EMM was found tO be asignificant cosolvent of methano1/gasoline blends, ？ 2009 Ai You Hao. Published by Elsevier B.V. on behalf of Chinese Chemical Society. All fights reserved.

Acetate-assistant efficient cation-exchange of halide perovskite nanocrystals to boost the photocatalytic CO_(2) reduction

The judicious implantation of active metal cations into the surface of semiconductor nanocrystal(NC)through cation-exchange is one of the facile and viable strategies to enhance the activity of catalysts for photocatalytic CO_(2)reduction,by shortening the transfer pathway of photogenerated carriers and increasing the active sites simultaneously.However,cation-exchange is hard to achieve for halide perovskite NCs owing to the stable octahedron of[PbX6]4−with strong interaction between halogen and lead.Herein,we report a facile method to overcome this obstacle by replacing partial Br−with acetate(Ac−)to generate CsPbBr_(3) NC(coded as CsPbBr_(3−x)Ac_(x)).A small amount of Ac−instead of Br−does not change the crystal structure of halide perovskite.Owing to the weaker interaction between acetate and lead in comparison with bromide,the corresponding octahedron structure containing acetate in CsPbBr_(3−x)Ac_(x) can be easily opened to realize efficient cation-exchange with Ni^(2+) ions.The resulting high loading amount of Ni^(2+) as active site endows CsPbBr_(3−x)Ac_(x) with an improved performance for photocatalytic CO_(2)reduction under visible light irradiation,exhibiting a significantly increased CO yield of 44.09μmol·g^(−1)·h^(−1),which is over 8 and 3 times higher than those of traditional pristine CsPbBr_(3) and nickel doped CsPbBr_(3) NC,respectively.This work provides a critical solution for the efficient metal doping of low-cost halide perovskite NCs to enhance their photocatalytic activity,promoting their practical applications in the field of photocatalysis.

亲水作用色谱柱与阳离子交换树脂柱结合分离无机离子(英文)

A combination of hydrophilic interaction chromatographic(HILIC) column and a weakly acidic cation-exchange resin(WCX) column was used for simultaneous separation of inorganic anions and cations by ion chromatography(IC).Firstly,the capability of HILIC column for the separation of analyte ions was evaluated under acidic eluent conditions.The columns used were SeQuant ZIC-HILIC(ZIC-HILIC) with a sulfobetaine-zwitterion stationary phase(ZIC-HILIC) and Acclaim HILIC-10 with a diol stationary phase(HILIC-10).When using tartaric acid as the eluent,the HILIC columns indicated strong retentions for anions,based on ion-pair interaction.Especially,HILIC-10 could strongly retain anions compared with ZIC-HILIC.The selectivity for analyte anions of HILIC-10 with 5 mmol/L tartaric acid eluent was in the order of I-> NO-3 > Br-> Cl-> H2PO-4.However,since HILIC-10 could not separate analyte cations,a WCX column(TSKgel Super IC-A/C) was connected after the HILIC column in series.The combination column system of HILIC and WCX columns could successfully separate ten ions(Na+,NH+4,K+,Mg2+,Ca2+,H2PO-4,Cl-,Br-,NO-3 and I-) with elution of 4 mmol/L tartaric acid plus 8 mmol/L 18-crown-6.The relative standard deviations(RSDs) of analyte ions by the system were in the ranges of 0.02%-0.05% in retention times and 0.18%-5.3% in peak areas through three-time successive injections.The limits of detection at signal-to-noise ratio of 3 were 0.24-0.30 μmol/L for the cations and 0.31-1.2 μmol/L for the anions.This system was applied for the simultaneous determination of the cations and the anions in a vegetable juice sample with satisfactory results.

Optimized photoluminescence of red phosphor K_(2)LiAlF_(6):Mn^(4+)synthesized by a cation-exchange method

Red phosphor K_2LiAlF_6:Mn^(4+) has been synthesized by a cation-exchange method in HF solution. To optimize their optical properties, phosphors were synthesized using different reaction conditions. The K_2LiAlF_6:0.5%Mn^(4+) synthesized at 20℃ for4 h shows the highest luminescence intensity. The temperature-dependent emission intensity of the phosphor was investigated,and it was found to exhibit good thermal stability, making it a promising red phosphor candidate for warm WLEDs.

水合物法天然气脱酸的影响因素

为了促进水合物法分离CO2在天然气脱酸工艺中的应用,以CH4+CO2混合气为例,采用CO2分离率、CH4损失率及分离因子作为水合物法脱酸的评价指标,利用自主设计的水合物法气体分离实验装置考察了初始压力、操作温度、四氢呋喃(THF)及实验用水量对水合物法分离CH4+CO2混合气的影响。结果表明,随初始压力增大和操作温度降低,平衡时气相CO2浓度降低,CO2分离率和CH4损失率同时增大,分离因子小幅减小;随THF浓度增大,平衡时气相CO2浓度增加,在THF摩尔分数为1.0%时,体系具有较大的CO2分离率和分离因子,较低的CH4损失率;随实验用水量增加,平衡时气相CO2浓度降低,CO2分离率增大,CH4损失率减小,分离因子增大。综合分析,可通过提高初始压力、降低操作温度、增加实验用水量,并添加摩尔分数1.0%THF来促进水合物生成,提高分离效率。

机械剥离-EDTA滴定法测定钴铬铝钇钽涂层中三氧化二铝

加入了三氧化二铝的CoCrAlYTa涂层具有更优良的物理和化学性能,同时三氧化二铝作为硬质相存在于涂层中,其含量太高又会严重影响涂层与基体的结合强度,因此建立一种准确测定CoCrAlYTa涂层中三氧化二铝含量的方法十分必要。用车床切削等剥离方式将涂层样品从工件上剥落,研磨成粒度约50μm后,用40mL硝酸（1＋1）加5mL盐酸在低温加热条件下溶解,使样品中的金属铝与三氧化二铝分离。分离后的酸不溶残渣在铂金坩埚中灰化灼烧后,用碳酸钠-硼砂混合熔剂于950~1 000℃熔融分解,或者将酸不溶残渣在镍坩埚中灰化灼烧后,用氢氧化钠加过氧化钠于750℃熔融分解。以稀盐酸浸出熔融物,采用强碱分离钴、铬等干扰元素后,以氟盐取代络合滴定法测定三氧化二铝的含量。实验表明,酸溶分离金属铝的效果好,三氧化二铝的溶出率小于2.5%;用两种熔融分解方式处理酸不溶残渣,测出的三氧化二铝含量一致;样品中的共存元素不干扰三氧化二铝的测定。实验方法应用于CoCrAlYTa涂层样品分析,三氧化二铝测定结果的相对标准偏差（RSD）不大于3.1%,加标回收率为95%~108%,满足喷涂工艺要求。

Hole-growth phenomenon during pyrolysis of a cation-exchange resin particle

A novel central hole-expansion phenomenon is identified, in which the cation-exchange resin is pyrolyzed in a mixed atmosphere of nitrogen and oxygen at 400–500 ℃. In this reaction, the reaction path is predictable and always starts from the center of the resin particle to form a central hole, then continues and expands around the hole, finally forming a uniformly distributed hole group;the particle surface remains intact. Analysis shows that this formation mode is due to the different reaction paths of sulfonic groups between the surface and interior of the particle, caused by the temperature difference. On the surface, transformation reactions happen at high temperatures(410–500 ℃) to form stable organic sulfur structures, while decomposition occurs inside the particle at a relatively low temperature(<410 ℃) and promotes complete pyrolysis of the copolymer matrix to form holes.

Donnan Electric Potential Dependence of Intraparticle Diffusion of Malachite Green in Single Cation Exchange Resin Particles: A Laser Trapping-Microspectroscopy Study

A laser trapping-microspectroscopy technique combined with excitation energy transfer from a fluorescent cationic dye (Rhodamine B, RB+) to a non-fluorescent cationic dye (Malachite Green, MG+) was employed to study pH effects on the diffusion coefficients of MG+ (D(MG+)) in single cation-exchange resin microparticles with the diameters of 16 μm. When RB+-pre-adsorbed resin particles were soaked in an aqueous MG+ solution, the RB+ fluorescence was quenched gradually with the soaking time. The time course of the quenching efficiency of RB+ by MG+ was then used to evaluate the D(MG+) value in the particle. The D(MG+) value increased from 1.1 × 10-11 to 4.3 × 10-11 cm2.s–1 on going the solu- tion pH value from 9 to 4. The results were explained reasonably by a Donnan electric potential model.

Development of Hormone-Active Fiber in the Form of Artificial Insulin Depot

This study examines the phenomena of the hormone-active fibers obtaining process, in the form of artificial insulin depot. As a fibrous carrier of insulin cation-exchange polyacrylonitrile (PAN) fibers and biodegradable polysaccharide alginate fibers were used. The process of obtaining fibrous artificial insulin depot was based on the chemisorption of insulin from insulin aqueous solutions by these fibers. The parameters of insulin chemisorption reaction were determined and their influence on quantities of bonded insulin in the artificial depot was studied. The impact of fiber polymer nature on the intensity of insulin chemisorption was studied and determined. Also, the location and deposition of insulin in and onto the fiber, fiber topography were studied. The maximum amounts of bounded insulin for the cation-exchange PAN fibers were 395.0 mg porcine insulin chromatographic / g of fiber, and for the alginate fibers were about 300? mg of porcine insulin chromatographic / g of fiber.

离子排斥色谱用于厌氧消化处理的水中脂肪族羧酸的分析(英文)

The analysis of seven aliphatic carboxylic acids(formic,acetic,propionic,iso-butyric,n-butyric,iso-valeric and n-valeric acid) in anaerobic digestion process waters for biogas production was examined by ion-exclusion chromatography with dilute acidic eluents(benzoic acid,perfluorobutyric acid(PFBA) and sulfuric acid) and non-suppressed conductivity/ultraviolet(UV) detection.The columns used were a styrene/divinylbenzene-based strongly acidic cation-exchange resin column(TSKgel SCX) and a polymethacrylate-based weakly acidic cation-exchange resin column(TSKgel Super IC-A/C).Good separation was performed on the TSKgel SCX in shorter retention times.For the TSKgel Super IC-A/C,peak shape of the acids was sharp and symmetrical in spite of longer retention times.In addition,the mutual separation of the acids was good except for iso-and n-butyric acids.The better separation and good detection was achieved by using the two columns(TSKgel SCX and TSKgel Super IC-A/C connected in series),lower concentrations of PFBA and sulfuric acid as eluents,non-suppressed conductivity detection and UV detection at 210 nm.This analysis was applied to anaerobic digestion process waters.The chromatograms with conductivity detection were relatively simpler compared with those of UV detection.The use of two columns with different selectivities for the aliphatic carboxylic acids and the two detection modes was effective for the determination and identification of the analytes in anaerobic digestion process waters containing complex matrices.

One-Step Procedure for Direct Purification of Pediocin-Like Bacteriocins and Cationic Antimicrobial Peptides from Complex Culture Medium on an Analytical, Semipreparative, and Preparative Scale. A New Type of Liquid Chromatography—Colloidal High-Performance Liquid Chromatography (CHPLC)

A simple time- and labor-saving one-step procedure suitable for analytical-, semipreparative-, and preparative-scale preparation of bacteriocins and other cationic antibacterial peptides (for example as lysozyme) has been developed. Suspensions of bacterial cells, other colloidal- and fast-particle materials, and dissolved anionic molecules passed through the column;however, cationic bacteriocins were separated by chromatography. The purity of the target substance at more than 97% was achieved by the judgment of spectral, chromatographic, and antimicrobial activity. A many-fold concentration increase was achieved for bacteriocins, lysozyme, and bacitracin (a commercial antibiotic) in comparison with the starting solutions (see the text below). In the experiments, homemade cation-exchange columns have been used. The columns have been prepared by the grafting of glass fibers with a diameter of 0.2 μm. In this paper, applications of a new type of liquid chromatography—colloidal high-performance liquid chromatography (CHPLC)—were demonstrated.