年产200吨4，4’-二氟二苯甲酮（DFBP）的工业化设计及可行性研究

本文在大量实验数据基础上，对4，4’-二氟二苯甲酮(DFBP)进行了年产200吨规模的工业化设计，从技术关键、工艺流程、设备选材、三废治理及成本核算等方面对DFBP工业化设计的可行性进行了评价，该设计有如下特点：工艺简单、合理，操作稳定、安全，三废治理有效，原材料及设备投资少，见效快，适合工业化大生产。     

用于脱除C5及MTBE中甲醇的渗透汽化膜研究

Several pervaporation membranes, cellulose acetate (CA), polyvinylbutyral (PVB), poly(MMA-co-AA), MMA-AA-BA, CA/PVB blend and CA/poly(MMA-co-AA) blend, were prepared, and their pervaporation properties were evaluated by separation of methanol/C5 or methanol/MTBE (methyl tert-butyl ether). The results shows that the CA composite membrane has a high separation performance (flux Jmenthanol =350g.m-2.h-1 and separation factor a > 400) for methanol/C5 mixtures, and the pervaporation characteristics of MMA-AA-BA copolymer membranes changes with the ratio of copolymer. For CA/poly(MMA-co-AA) blend membrane, the pervaporation performance is improved in comparison with CA or poly(MMA-co-AA) membrane. From the experiment of CA/PVB blend membranes for methanol/MTBE mixture, it is found that the compatibility of blends may affect the separation features of blend membrane.     

Mechanical properties of a cryogenically mechanically alloyed polycarbonate–poly(aryl ether ether ketone) system

The processing–property relationship of a model cryogenically mechanically alloyed polymer–polymer system [polycarbonate (PC) and poly(aryl ether ether ketone) (PEEK)] was investigated. PC and PEEK powders were cryogenically mechanically alloyed for 10 h, and the resulting two‐phase powder particles were processed into testable coupons with a miniature ram‐injection molder. The bulk mechanical properties of the coupons made from the mechanically alloyed powders and nonmechanically alloyed powders were investigated as a function of mechanical alloying and injection‐molding parameters. The injection‐molded coupons were mechanically tested in the three‐point‐bending mode. The results demonstrated that no measurable improvement was achieved in the energy to break, strain at failure, or failure strength in the coupons made from the mechanically alloyed materials in comparison with those of the coupons made from the nonmechanically alloyed powders. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 88: 1196–1202, 2003     

Sulfonated polyether ether ketone composite proton exchange membranes incorporated with a novel hierarchical-structure hybrid nanofiller consisting solid superacid zirconium phosphate and CNTs

How to simultaneously improved the proton conductivity and mechanical strength is a key problem facing currently used proton exchange membranes (PEMs). Herein, a solid inorganic superacid-zirconium phosphate (ZrP) with a two-dimensional layer structure was combined with one-dimensional carbon nanotubes (CNTs) to prepare hybrid nanofiller ZrP-CNTs by an in situ chemical deposition method. The new hybrid nanofiller was then applied to modify sulfonated polyether ether ketone (SPEEK), a widely used PEM matrix, to obtain a series of composite membranes. The structure and properties of the membranes were fully characterized by SEM, XRD, FTIR, TG, tensile properties, and proton conductivity. The results showed that the proton conductivities of the membranes were significantly improved due to the addition of super solid acid-ZrP that has abundant proton sources or proton sites. Moreover, the composite membranes exhibited better mechanical properties and thermal stability than those of pure SPEEK membrane, owing to the great interface interaction and good compatibility between ZrP-CNTs and SPEEK. The composite membrane (2 wt% ZrP-CNTs) demonstrated the optimal comprehensive performance. Its proton conductivity was 36.63 mS cm⁻¹ and its tensile strength was 37.56 MPa, which was 70% and 10%, respectively, higher than those of the pure SPEEK membrane under the same condition.     

Controllable Synthesis of Submicrometer Core–Shell Modifier and Its Effect on Toughening Polypheylene Ether/Polystyrene Blends

Core–shell polybutadiene-graft-polystyrene (PB-g-PS) graft copolymers with different ratios of PB to PS are synthesized by emulsion polymerization. Further, the PB-g-PS copolymers are blended with polypheylene ether (PPE) and PS to prepare PPE/PS/PB-g-PS blends. The effects of PB-g-PS copolymer structure and matrix composition on the morphological, mechanical properties, and deformation mechanism of the blends are studied. The results show that the synthesized submicrometer-sized PB-g-PS copolymer has an excellent toughening efficiency, both the copolymer and PS are introduced into PPE resin to produce a ternary blend which is combined with high toughness and processing properties. The optimum toughening effect on PPE/PS matrix is observed at the core–shell weight ratio of 70/30 in PB-g-PS copolymer, and the impact strength of the blends increased from 101 to 550 J m⁻¹. In addition, the dispersion pattern of rubber particles in the matrix gradually changes from uniform dispersion to aggregation as the core–shell ratio of PB-g-PS copolymers increases. On the other hand, with the increase of PPE content, the dispersion of rubber particles in PPE/PS matrix is improved, and the deformation mechanism is changed from cracking to a combination of crazing and shear yielding, which can lead to absorb more energy to achieve better toughness.     

Semicontinuous separation of dimethyl ether (DME) produced from biomass

A ternary semicontinuous system for the separation of bio‐dimethyl ether from methanol and water is presented. The performance of eight potential control configurations, including the application of temperature inferential control, is evaluated. Dynamic simulations of the semicontinuous system and associated control scheme demonstrate that the temperature inferential control configuration is effective in achieving the separation objectives while remaining within operational limits. The semicontinuous system using the inferential temperature control scheme is simulated and shown to be economically preferable to the traditional continuous process for a range of production rates. © 2013 Canadian Society for Chemical Engineering     

2,4-二氨基苯基胆甾醚的合成

以溴苯为原料,经硝化后,在四丁基溴化铵相转移催化剂作用下与胆固醇成醚、硝基还原反应得到2,4-二氨基苯基胆甾醚,并对成醚反应的条件进行了优化。较佳合成反应条件是:以甲苯为溶剂,n(2,4-二硝基溴苯)∶n(胆固醇)=1.55∶1,反应温度25℃,w(NaOH)=50%,反应时间3.5 h,产率为72%。所得中间体和目标化合物经过红外光谱和核磁波谱的表征。     

Effect of polyarylene ether nitriles on processing and mechanical behaviors of phthalonitrile‐epoxy copolymers and glass fiber laminated composites

A series of copolymers and glass fiber composites were successfully prepared from 2,2‐bis [4‐(3,4‐dicyanophenoxy) phenyl] propane (BAPh), epoxy resins E‐44 (EP), and polyarylene ether nitriles (PEN) with 4,4′‐diaminodiphenyl sulfone as curing additive. The gelation time was shortened from 25 min to 4 min when PEN content was 0 wt % and 15 wt %, respectively. PEN could accelerate the crosslinking reaction between the phthalonitrile and epoxy. The initial decomposition temperatures (T_i) of BAPh/EP copolymers and glass fiber composites were all more than 350°C in nitrogen. The T_g of 15 wt % PEN glass fiber composites increased by 21.2°C compared with that of in comparison with BAPh/EP glass fiber composite. The flexural strength of the copolymers and glass fiber composites reached 119.8 MPa and 698.5 MPa which increased by 16.6 MPa and 127.3 MPa in comparison with BAPh/EP composite, respectively. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Horizontal reactive distillation for multicomponent chiral resolution

A novel horizontal reactive distillation apparatus and a new overall process scheme are proposed for continuous multicomponent chiral resolution via reversible enantioselective acylation of a chiral (racemic) substrate by a chiral (racemic) acyl donor. The process enables simultaneous production of up to four enantiomers with enhanced chiral purity. Kinetic studies, miniplant experiments, and process simulation results are described for a model lipase‐catalyzed reaction: (R)‐enantioselective transesterification of (R,S)‐1‐n‐butoxy‐2‐propanol with (R,S)‐1‐methoxy‐2‐acetoxypropane to produce (R)‐1‐n‐butoxy‐2‐acetoxypropane, (R)‐1‐methoxy‐2‐propanol, and the two unreacted (S)‐enantiomers of the (R,S)‐reagents. A horizontal, compartmentalized reactive distillation vessel is specified instead of a conventional reactive distillation column to provide longer liquid‐phase residence time needed for adequate conversion. Low vapor‐traffic pressure drop allows operation under vacuum at reduced temperatures for good enzyme stability and enantioselectivity. The general technology has potential as a means to producing a wide range of chiral synthons used in asymmetric syntheses of chiral pharmaceuticals and other biologically active products. © 2013 American Institute of Chemical Engineers AIChE J, 59: 2603–2620, 2013     

Effect of PES on the morphology and properties of proton conducting blends with sulfonated poly(ether ether ketone)

Development of alternate materials to Nafion, based on ionically conducting polymers and their blends is important for the wider applications of proton exchange membrane fuel cells. In this work, blends of sulfonated poly(ether ether ketone) (SPEEK) with poly(ether sulfone) (PES) are investigated. SPEEK with various ion exchange capacity (IEC) was prepared and blended with PES, which is nonionic and hydrophobic in nature. A comparative study of the water uptake, proton conductivity, and thermo‐mechanical characteristics of SPEEK and the blend membranes as a function of the IEC is presented. Addition of PES decreases the water uptake and conductivity of SPEEK. Chemical and thermal stability and mechanical properties of the membrane improve with the addition of PES. The effect of water content on the thermo‐mechanical properties of membranes was also studied. The morphology of blend membranes was studied using SEM to understand the microstructure and miscibility of the components. On the basis of the results, a plausible microstructure of the blends is presented, and is shown to be useful in understanding the variation of different properties with blending. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013