A Novel Process Using Ion Exchange Resins for the Coproduction of Ethyl and Butyl Acetates

Before proposing an innovative process for the coproduction of ethyl and butyl acetates, the individual syntheses of ethyl acetate and butyl acetate by two different routes were first studied. These syntheses involved the reaction of ethanol or n-butanol with acetic acid or acetic anhydride in the presence of ion exchange resins: Amberlyst 15, Amberlyst 16, Amberlyst 36 and Dowex 50WX8. Kinetic and thermodynamic studies were performed with all resins. The lowest activation energy (Ea) value was obtained with Dowex 50WX8, which was identified as the best-performing resin, able to be reused at least in four runs without regeneration. The presence of water-azeotropes during the synthesis of ethyl acetate makes its purification difficult. A new strategy was adopted here, involving the use of ethanol and acetic anhydride as the starting material. In order to minimize acetic acid as co-product of this reaction, a novel two-step process for the coproduction of ethyl and butyl acetates was developed. The first step involves the production of ethyl acetate and its purification. Butyl acetate was produced in the second step: n-butanol was added to the mixture of acetic acid and the resin remaining after the first-step distillation. This process yields ethyl acetate and butyl acetate at high purity and shows an environmental benefit over the independent syntheses by green metrics calculation and life cycle assessment.

Taste masking of ciprofloxacin by ion-exchange resin and sustain release at gastric-intestinal through interpenetrating polymer network

The aim of the study was to taste mask ciprofloxacin(CP)by using ion-exchange resins(IERs)followed by sustain release of CP by forming interpenetrating polymer network(IPN).IERs based on the copolymerization of acrylic acid with different cross linking agents were synthesised.Drug-resin complexes(DRCs)with three different ratios of drug to IERs(1:1,1:2,1:4)were prepared&evaluated for taste masking by following in vivo and in vitro methods.Human volunteers graded ADC 1:4,acrylic acid-divinyl benzene(ADC-3)resin as tasteless.Characterization studies such as FTIR,SEM,DSC,P-XRD differentiated ADC 1:4,from physical mixture(PM 1:4)and confirmed the formation of complex.In vitro drug release of ADC 1:4 showed complete release of CP within 60 min at simulated gastric fluid(SGF)i.e.pH 1.2.IPN beads were prepared with ADC 1:4 by using sodium alginate(AL)and sodium alginate-chitosan(AL-CS)for sustain release of CP at SGF pH and followed by simulated intestinal fluid(SIF i.e.pH 7.4).FTIR spectra confirmed the formation of IPN beads.The release of CP was sustain at SGF pH(<20%)whereas in SIF media it was more(>75%).The kinetic model of IPN beads showed the release of CP was non-Fickian diffusion type.

Determination of Sc by Ion-exchanger Colorimetry

Ion exchanger colorimetry for scandium in the form of ternary color system “Sc(Ⅲ) CPA pc Ac” was developed. The influences of types and grain sizes of resin, adsorption modes and the acidity on the determination were studied systematically, and the optimum operating conditions and the allowable amounts of foreign ions were determined. In comparison with the ordinary solution colorimetry, both of the sensitivity and the selectivity of this ion exchanger colorimetry are improved obviously. The preliminary uses of this method to the determination of Sc(Ⅲ) in two synthetic samples were satisfied.

Adsorption of Copper from an Ammonia-Thiosulfate Media Using DOWEX 550A Ion Exchange Resin

The study of copper adsorption onto ion exchange resins of anionic type is part of the gold recovery from ammonia-thiosulfate solutions, where copper is the main impurity of the system because it acts as a catalyst of gold dissolution reaction. A study is made of the adsorption and desorption of copper in the form of the complex in an ammonia-thiosulfate media on an ion exchange resin, DOWEX 550A, classified as a strong base, which in its inner structure has a quaternary amine functional group. In the studied pH range copper adsorption increased with increasing pH, while the presence of thiosulfate decreased it, the same as the ammonia content, due to the greater presence of cuprotetramine, . Elution of the copper complexes from the resin was more efficient with sulfite than with perchlorate.

Reaction kinetics for the heterogeneously resin-catalyzed and homogeneously self-catalyzed esterification of thioglycolic acid with 2-ethyl-1-hexanol

Producing 2-ethyl-1-hexyl thioglycolate(ETE)via esterification reaction with thioglycolic acid(TGA)aqueous solution as raw material by reactive-separation coupling technology is a promising process intensification method.To choose suitable reactive-separation coupling strategy,the kinetic studies of the esterification of TGA with 2-ethyl-1-hexanol(EHL)were carried out in a batch system.The commercial ion exchange resin was employed as an eco-friendly catalyst.The effects of temperature,catalyst concentration and molar ratio were determined.It was interesting to observe that the equilibrium conversion of TGA increased with the increase of catalyst mass fraction due to the adsorption of product water onto resin surface.The activity-based pseudo-homogeneous(PH),Eley-Rideal(ER)and Langmuir-Hinshelwood-Ho ugen-Watson(LHHW)models were used to fit the kinetics data of the resin-catalyzed reaction.The models of ER and LHHW performed better than the PH model.The kinetics of the TGA-self-catalyzed reaction was also determined.An activity-based homogeneous kinetics model could well describe this self-catalyzed reaction.These results would be meaningful to the selection and design of an appropriate reactionseparation strategy for the production of ETE,to realize the process intensification.

Research Progress on the Separation of Alkaloids from Chinese Medicines by Column Chromatography

Alkaloids have a variety of bioactivities and great development value in the fields of pharmaceuticals, cosmetics and health food. Column chromatography is a common method for preparing alkaloids. In this paper, the research status of the separation and purification of alkaloids from Chinese medicines by column chromatography is reviewed, and the factors that influence the refining of alkaloids via a macroporous adsorption resin, ion exchange resin and silica gel are summarized. The thermodynamic and kinetic modeling methods for the static adsorption of adsorbents are also reviewed in this paper. It is suggested that the modeling method of the column chromatography process be deeply studied to establish a more stringent quality control method for sampling liquid and to strengthen the online detection of the chromatography process to improve the refining effect of alkaloids.

STUDY ON THE SEPARATION OF PENTOSE AND HEXOSE FROM GLUCOSE YEAST WATER

D-ribose is a unique, 5-carbon sugar that occurs naturally in all living cells. D-ribose has been used as a staring material for preparation of some certain medicines or just as a new nutraceutical that helps the body naturally restore its energy level. The fermentative processes are the best for their relatively simple series of production steps and relatively cheap starting materials. However, because of the many impurities in glucose yeast water and its dark color, pretreatment and purification must be done to the fluid before D-ribose can be separated. In this paper, separation and purification of D-ribose was carried out using cation exchange resins, of which Ca2+ exchange resin had the best effect. The optimal condition for adsorption is a flow velocity of 0.5BV/h at adsorption temperature of 25℃. The optimal condition for desorption is a flow velocity of 0.5 BV/h at desorption temperature of 80℃.

Development and Research of Non⁃Stirring Conveying Device for Waste Resin in Nuclear Power Plant

Blockage in the storage and transportation of waste resin is a difficult problem in the radioactive waste treatment process of nuclear power plants.In this study,in order to solve the problems of unstable resin transport concentration and easy blockage of conveying equipment and pipelines in nuclear power plants in China,a set of non⁃stirring conveying devices is developed,and theoretical calculations,simulation analysis and experimental verification are carried out.By transporting resin using the no stirring conveying device developed in this paper,it is not only to eliminate the risk of blockage and ensure the safety of transportation,but also to adjust the concentration of conveying resin to change the transport efficiency according to the operating conditions.The effective bearing rate of waste resin storage tank can be improved,so that the comprehensive performance of waste resin storage and transportation in nuclear power plants can be greatly improved.

Solidification of Spent Ion Exchange Resin Using ASC Cement

Ion exchange resins (IERs) have been widely used in nuclear facilities. However, the spent radioactive IERs result in major quantities of low and intermediate level radioactive wastes. This article describes a laboratory experimental study on solidification processing of IERs using a new type of cement named ASC cement. The strength of the cementation matrix is in the range of 1820 MPa (28 d); the loading of the spent IER in the cement-resin matrix is over 45% and leaching rates of 137Cs, 90Sr and 60Co are 7.92×10 -5, 5.7×10 -6, and 1.19×10 -8 cm/d. The results show that ASC cement can be a preferable cementation material for immobilization of radioactive spent IER.

Adsorption of naphthalene onto a high-surface-area carbon from waste ion exchange resin

A high-surface-area carbon （KC-1） was prepared from waste polystyrene-based ion exchange resin by KOH activation and used for naphthalene adsorption. The carbon exhibited a good hydrophobic nature with developed porous structure, favoring the adsorption of organic compounds. The Brunauer-Emmett-Teller surface area and total pore volume of KC- 1 were 3442.2 and 1.68 cm3/g, respectively, which can be compared with those of KOH-activated carbons prepared from other precursors. Batch experiments were carded out to investigate the adsorption of naphthalene onto KC-1. The equilibrium data were analyzed by the Langmuir, Freundlich, and Polanyi- Manes isotherms and agreed with the Polanyi-Manes Model. The adsorption of naphthalene depended greatly on the porosity of the carbon, and the dispersive interactions between naphthalene and carbon could be relatively weak. The pH variation in aqueous solution had little effect on the adsorption process. The equilibrium time for 0.04 g/L of carbon dose was around 5 hr. Different models were used to evaluate the kinetic data and the pseudo second-order model was suitable to describe the kinetic process of naphthalene adsorption onto KC-1. Regeneration of spent carbon could be carded out effectively by alcohol treatment. The results indicated that KC-1 was a promising adsorbent for the removal of polycyclic aromatic hydrocarbons from aqueous solutions.

Manufacture of Boron-free Magnesia with High Purity from Residual Brine

A novel method for removing boron with ion exchange resin from residual brines to manufacture boron-free magnesia is described. The concentration of boron in the target magnesia manufactured thereby from Qinghai salt lakes is lower than 5 mg/g, and the typical D50 size of product is 10.625 mm.

The Synthesis of Cyclic Amino Acids

Several cyclic amino acids (1-4) were synthesized from glycine. Isocyanate ester was prepared as the key intermediate and reacted with dibromoalkanes to afford the target compounds.

Condensation of phenol and acetone on a modified macroreticular ion exchange resin catalyst

Macroreticular ion exchange resin catalysts were prepared by suspension polymerization, and then modified by alkylmercaptoamines. The modified catalysts were characterized by N2 adsorption/desorption measure- ments, scanning electron microscopy and differential scanning calorimetry. Key factors such as the mercaptan content, the degree of crosslinking and the structures of the promoters were investigated for the synthesis of Bisphenol A （BPA）. At optimal conditions, the macroreticular ion exchange resin catalysts modified by alkylmercaptoamines showed high catalytic activity and selectivity for BPA synthesis.

Zn Cl_2-modified ion exchange resin as an efficient catalyst for the bisphenol-A production

A Zn Cl2-modified ion exchange resin as the catalyst for bisphenol-A synthesis was prepared by the ion exchange method. Scanning electron microscope（SEM）, Fourier transform infrared spectrophotometer（FT-IR）, thermo gravimetric analyzer（TGA） and pyridine adsorbed IR were employed to characterize the catalyst. As a result, the modified catalyst showed high acidity and good thermal stability. Zn2＋coordinated with a sulfonic acid group to form a stable active site, which effectively decreased the deactivation caused by the degradation of sulfonic acid. Thus the prepared catalyst exhibited excellent catalytic activity, selectivity and stability compared to the unmodified counterpart.

Capability of cation exchange technology to remove proven N-nitrosodimethylamine precursors

N-nitrosodimethylamine（NDMA） precursors consist of a positively charged dimethylamine group and a non-polar moiety, which inspired us to develop a targeted cation exchange technology to remove NDMA precursors. In this study, we tested the removal of two representative NDMA precursors, dimethylamine（DMA） and ranitidine（RNTD）, by strong acidic cation exchange resin. The results showed that pH greatly affected the exchange efficiency, with high removal（DMA 〉 78% and RNTD 〉 94%） observed at pH 〈 pk_a-1 when the molar ratio of exchange capacity to precursor was 4. The exchange order was obtained as follows： Ca^（2＋）〉 Mg^（2＋）〉 RNTD~＋〉 K~＋〉 DMA~＋〉 NH_4~＋〉 Na~＋. The partition coefficient of DMA~＋to Na~＋was 1.41 ± 0.26, while that of RNTD~＋to Na~＋was 12.1 ± 1.9. The pseudo second-order equation fitted the cation exchange kinetics well. Bivalent inorganic cations such as Ca^（2＋）were found to have a notable effect on NA precursor removal in softening column test. Besides DMA and RNTD, cation exchange process also worked well for removing other 7 model NDMA precursors. Overall, NDMA precursor removal can be an added benefit of making use of cation exchange water softening processes.