Synthesis and properties of fluorinated aromatic poly(amide imide)s based on 4,4′‐bis(4‐amino‐2‐trifluoromethylphenoxy)benzophenone and various bis(trimellitimide)s

A CF₃‐containing diamine, 4,4′‐bis(4‐amino‐2‐trifluoromethylphenoxy)benzophenone ( 2 ), was synthesized from 4,4′‐dihydroxybenzophenone and 2‐chloro‐5‐nitrobenzotrifluoride. Imide‐containing diacids ( 3 and 5B_a – 5B_g ) were prepared by the condensation reaction of aromatic diamines and trimellitic anhydride. Then, two series of novel soluble aromatic poly(amide imide)s (PAIs; 6A_a – 6A_k and 6B_a – 6B_g ) were synthesized from a diamine ( 4A_a – 4A_k or 2 ) with the imide‐containing diacids ( 3 and 5B_a – 5B_g ) via direct polycondensation with triphenyl phosphate and pyridine. The aromatic PAIs had inherent viscosities of 0.74–1.76 dL/g. All of the synthesized polymers showed excellent solubility in amide‐type solvents, such as N‐methyl‐2‐pyrrolidone and N,N‐dimethylacetamide (DMAc), and afforded transparent and tough films by DMAc solvent casting. These polymer films had tensile strengths of 90–113 MPa, elongations at break of 8–15%, and initial moduli of 2.0–2.9 GPa. The glass‐transition temperatures of the aromatic PAIs were in the range 242–279°C. They had 10% weight losses at temperatures above 500°C and showed excellent thermal stabilities. The 6B series exhibited less coloring and showed lower yellowness index values than the corresponding 6A series. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 102:3641–3653, 2006     

丁二酮肟吸光光度法测定陶瓷色釉料中的镍

当有氧化剂存在时，在氨性溶液中，镍与丁二酮肟生成酒红色的络合物。借此可作镍的比色测定。若离子本身有颜色，则影响测定，但可用空白校正。     

Preparation and characterization of high-surface-area titanium dioxide by sol-gel process

One of the important ways to improve photocatalytic efficiency is to prepare catalyst with enhanced surface area. In this work, titanium dioxide (TiO₂) nanoparticles having enhanced surface area were synthesized under the interference of SiO₂. The mixed oxide, SiO₂-TiO₂ (10% mol% Si), was prepared by a sol-gel procedure using titanium tetra-n-butoxide as Ti-precursor. The commercial SiO₂ nanoparticles were added into the TiO₂ sols after hydrolysis. After condensation and calcination heat treatment, the SiO₂-TiO₂ nanoparticles were obtained. To achieve the purpose of obtaining the high-surface-area TiO₂, the SiO₂ was removed subsequently by aqueous NaOH solution. The TiO₂ products were characterized by transmission electron microscopy (TEM), X-ray diffraction (XRD), electron spectroscopy for chemical analysis (ESCA), and by N₂ adsorption-desorption isotherm. A fine mesoporous structure was formed for as-prepared TiO₂ after calcination at 400^∘C and the average pore diameter was about 7 nm. The porous TiO₂ products possess mixing phases of anatase and rutile. Phase transformation from anatase to rutile occurred when the samples were calcined. The phase transition temperature is sensitive to the silicon content. The particle size of ∼43 nm remained constant upon calcinations from 500 to 700^∘C. The specific surface area was increased up to 66% compared to regular TiO₂ samples that were prepared by the similar sol-gel procedure. The porous TiO₂ nanostructures exhibited enhanced photocatalytic performance to decompose methylene blue under UV irradiation.     

Approximate migration coefficient of interfacial transition zone and the effect of aggregate content on the migration coefficient of mortar

In this study, the electrochemical technique is applied to accelerate chloride ion migration in mortar to estimate its transport properties. In order to investigate the effect of aggregate content on the chloride migration coefficient of mortar, specimens with different fine aggregate volume fractions were cast and tested. The chloride migration coefficient of mortar was determined experimentally as a function of the volume fraction of aggregate. The chloride migration coefficient of mortar is used to assess the dilution, tortuosity and interfacial transition zone (ITZ) effects of aggregate in the cement-based composites. A model modified from the Bruggeman theory for the migration coefficient of mortar is used, and the regression analysis is used to determine the approximate chloride migration coefficient of ITZ. Based on the experimental and regression analytical results, the approximate ITZ migration coefficient is 2.83, 1.76 and 1.55 times of the matrix migration coefficient for the ITZ with the thickness of 20, 40 and 50 μm, respectively.     

Optimal reaction conditions for the minimization of energy consumption and by‐product formation in a poly(ethylene terephthalate) process

We determined the optimal reaction conditions to minimize the energy cost and the quantities of by‐products for a poly(ethylene terephthalate) process by using the iterative dynamic programming (IDP) algorithm. Here, we employed a sequence of three reactor models: the semibatch transesterification reactor model, the semibatch prepolymerization reactor model, and the rotating‐disc‐type polycondensation reactor model. We selectively chose or developed the reactor models by incorporating experimentally verified kinetic models reported in the literature. We established the model for the entire reactor system by connecting the three reactor models in series and by resolving some joint problems arising when different types of reactor models were interconnected. On the basis of the simulation results of the reactor system, we scrutinized the cause and effect between the reaction conditions and the final quality of the polymer product. Here, we set up the optimization strategy by using IDP on the basis of the integrated reactor model, and the process variables with significant influence on the properties of polymer were selected as control variables with the help of a simulation study. With this method, we could refine the reaction conditions at the end of each iteration step by contracting the spectra of control regions, and the iteration process finally stopped when the profile of the optimal trajectory converged. We also took the constraints on the control variables into account to guarantee polymer quality and to suppress side reactions. Constituting six different strategies by setting weighting vectors differently, we examined the differences in optimal trajectories, the trend of optimality, and the quality of the final polymer product. For each of the strategies, we conducted the optimization to examine whether the number‐average degree of polymerization approached the desired value. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 86: 993–1008, 2002     

Optimal process conditions of shrinkage and warpage of thin‐wall parts

Optimal process conditions of thin‐wall injection molding of a cellular phone cover were investigated with the consideration of interaction effects between process parameters. L₂₇ experimental tests based on Taguchi's method were performed, and then Cyclone Scanner, PolyCAD and PolyWorks were used to measure the shrinkage and warpage of the thin‐wall injected parts to determine the optimal process conditions. Based on the results of the analysis of variables and the F‐test, interaction effects for each observed factor were determined. The results indicated that the packing pressure was the most important process parameter affecting the shrinkage and warpage of the thin‐wall part. The optimal process conditions were different for the shrinkage and the warpage. This was because during the injection process, the mechanisms affecting shrinkage or warpage were different. Compared with the results obtained with simplified thin‐wall parts in the literature, it was found that the geometry of a real commercial part did affect the optimal process conditions and the order of influence of process parameters. The optimal process conditions determined by Taguchi's method for reducing the shrinkage and warpage were verified experimentally in this work. Polym. Eng. Sci. 44:917–928, 2004. © 2004 Society of Plastics Engineers.     

Effect of Co2+, Ni2+, Cu2+, or Zn2+ on properties of polyaniline nanoparticles

Uniform polyaniline (PANI) nanoparticles with typical sizes of about 50 nm were electropolymerized on indium tin oxide surfaces in the presence of Co²⁺, Ni²⁺, Cu²⁺, or Zn²⁺. According to shaping theory, we first suggest the reason forming PANI spherical particles. Their conductivity, UV‐vis spectra, FTIR spectra, X‐ray diffraction, and thermogravimetric analysis were investigated. The conductivities and crystallinity of PANI doped with these ions are higher than those of PANI doped with HCl (PANI/HCl). Both UV‐vis absorption spectra and FTIR spectra indicate the interactions between Co²⁺, Ni²⁺, Cu²⁺, or Zn²⁺ and PANI chains. TG analysis also shows that the thermal stability of PANI doped by Co²⁺, Ni²⁺, Cu²⁺, or Zn²⁺ is lower than that of PANI/HCl. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2007     

Three-dimensional modelling of Non-Newtonian fluid flow in a coat-hanger die

The three-dimensional model of isothermal flow of power-law fluid in a coat-hanger die has been developed using finite element method. The shape of coat-hanger die used in the present model was determined according to the previous analytical design equation which is based on one-dimensional flow model in the manifold and the slot. Because uniform flow rate across the die outlet is most important to achieve uniform thickness of extruded polymer sheet or film, flow rate distribution is mainly examined to determine the valid process condition for the design equation as the design parameters are changed. The effects of fluid property in terms of power-law index and process parameters not considered in one-dimensional design equation such as die inlet size and the presence of land were analyzed. Results show that the manifold angle is the most influencing design parameter on flow rate distribution. When the material of different power-law index from design value is processed, the change of power-law index affects the uniformity of flow rate appreciably.