2-溴-3,3,3-三氟丙烯的制备

以3,3,3-三氟丙烯和溴为原料,经加成反应合成了中间产物1,2-二溴-3,3,3-三氟丙烷,随后在氢氧化钠水溶液中进行消除反应制备了目标产物2-溴-3,3,3-三氟丙烯,通过试验得到了较佳的反应条件。     

Evaluation of Porous Structure of Cement Pastes Made with Residual Rice Husk Ash

In several countries, the residual RHA （rice husk ash） has been produced in rice processing industries or in thermoelectric plants that use rice husk to generate heat and/or electrical energy, usually without burning process control. This causes a reduction in the amorphous silica content of residual RHA, which distinguishes them from the RHA produced according to controlled burning process, which is totally amorphous and considered a highly reactive pozzolan. In this paper, the hydration products and the porous structure of binders paste were studied by replacing, in weight of 5%, 10% and 20% of Portland cement OPC （ordinary Portland cement）, by residual RHAs named A and B, which have high and low content of amorphous silica, respectively, using microstructure evaluation techniques as XRD （X-ray diffraction）, TG （thermogravimetric） tests and MIP （mercury intrusion porosimetry）. A reducing the size of the pores of the pastes was observed according to the increase of content replacement of RHA A and RHA B.     

Effects of hydrogen addition on the high temperature deformation behavior of TC21 titanium alloy

The true stress-strain curves of TC21 titanium alloy charged with up to 0.7 wt.% hydrogen were obtained by the isothermal hot compression tests which were carried out on an Instron 5500 machine at 1023 to 1223 K and 0.001 to 0.1 s⁻¹. The dependence of the steady state flow stress on hydrogen content was determined. The results showed that with the increase of hydrogen content flow stress decreased at lower hydrogen content and then increased at higher hydrogen content. Suitable hydrogen addition can significantly decrease the flow stress and improve the hot workability of TC21 titanium alloy. The flow stress behaviors and the dependence of hydrogen content on flow stress were clarified by microstructural observation. The optimum hydrogen content at different deformation temperature was determined.     

Study of hot forging behavior of as-cast Mg–3Al–1Zn–2Ca alloy towards optimization of its hot workability

Mg–3Al–1Zn–2Ca (AZX312) alloy has been forged in the temperature range of 350–500 °C and at speeds in the range of 0.01–10 mm s⁻¹ to produce a rib-web shape with a view to validate the processing map and study the microstructural development. The process was simulated through finite-element method to estimate the local and average strain rate ranges in the forging envelope. The processing map exhibited two domains in the following ranges: (1) 350–450 °C/0.0003–0.05 s⁻¹ and (2) 450–500 °C/0.03–0.7 s⁻¹ and these represent dynamic recrystallization (DRX) and intercrystalline cracking, respectively. The optimal workability condition according to the processing map is 425–450 °C/0.001–0.01 s⁻¹. A wide flow instability regime occurred at higher strain rates diagonally across the map, which caused flow localization that should be avoided in forming this alloy. The experimental load–stroke curves correlated well with the simulated ones and the observed microstructural features in the forged components matched with the ones predicted by the processing map.     

Smoke and toxicity suppression by zinc salts in flame‐retardant polyurethane‐polyisocyanurate foams filled with phosphonate and chlorinated phosphate

Three types of zinc salts, ZnAl₂O₄, ZnFe₂O_4, and Zn₂SiO_4, were prepared by coprecipitation. Potential smoke and toxicity suppression by zinc salts in flame‐retardant polyurethane‐polyisocyanurate foams (FPUR‐PIR) with dimethylmethylphosphonate (DMMP) and tris (2‐chloropropyl) phosphate (TCPP) were investigated. The crystal structure and dispersity of zinc salts in FPUR‐PIR were characterized by X‐ray diffraction (XRD) and scanning electron microscopy (SEM). Smoke density, flame retardancy, and thermal degradation were studied using smoke density rating (SDR), limiting oxygen index (LOI), the cone calorimeter test, and thermogravimetry coupled with FTIR spectrophotometry (TGA‐FTIR). The results indicated that pure zinc salts were obtained and evenly dispersed on the cell wall of FPUR‐PIR. SDR and the specific extinction area (SEA) were significantly decreased, the time to second heat release rate peak (pk‐HRR) of FRUP‐PIR was delayed after incorporation of the zinc salts; zinc salts partially inhibited phosphorus oxide release into the gas phase, enhanced the condensed phase effect of phosphorus, reduced, and prolonged the release of isocyanate compound and hydrogen cyanide from FRUP‐PIR; due to an increase in the amount of char residues, which indicated the suppression of smoke and toxicity volatiles. ZnFe₂O₄ resulted in better char formation at the initial degradation stage of FPUR‐PIR, and ZnAl₂O₄ retained more phosphorus in the solid phase at higher temperature. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 41846.     

Enhanced boron removal from metallurgical grade silicon by the slag refining method with the addition of tin

An effective boron removal method was developed through a process of combining Si–Sn alloy with slag treatment. Boron content in refined silicon and boron removal fraction by slag containing 5 wt% CaO, 25 wt% SiO₂ and 70 wt% Na₂SiO₃ and was investigated under varied Si–Sn alloy composition, slag/Si–Sn alloy mass ratio and refining time. Boron was effectively removed by adding tin to metallurgical grade silicon. In particular, the boron content in metallurgical grade silicon decreased from 12.92 ppmw to 0.79 ppmw by adding 50 at% tin under a mass ratio of 2:1 (slag:alloy) at 1723 K. The amount of boron removed increased with increasing amount of tin added, mass ratio and refining time.     

Preparation,characterization, and dynamic adsorption–desorption studies on polypyrrole encapsulated TiO2 nanoparticles

Binary doped polypyrrole (PPy) encapsulated Titania (TiO₂) nanoparticles were prepared by oxidative polymerization using FeCl₃ as oxidant in presence of camphorsulfonic acid (CSA) as surfactant. Both FeCl₃ (oxidant) and camphorsulfonic acid (surfactant) also act as dopant and hence thus prepared polypyrrole/Titania (TiO₂@PPy) is termed as binary doped nanocomposite i.e. FeCl₃ dopes polypyrrole by oxidation mechanism while camphorsulfonic acid dopes polypyrrole by protonic doping mechanism. The TiO₂@PPy coreshell nanocomposites were characterized by Fourier transform infrared spectroscopy (FTIR), X‐ray diffraction (XRD), thermogravimetry, differential scanning calorimetry (DSC), field emission‐scanning electron microscopy (FE‐SEM), and inductance‐capacitance‐resistance (LCR) measurements. The results indicated that the structural and electrical properties of the TiO₂@PPy coreshell nanocomposites were significantly influenced by the extent of TiO₂ nanoparticles loading of polypyrrole. The direct current (DC) electrical conductivity of the as‐prepared TiO₂@PPy coreshell nanocomposites was higher than that of PPy. As‐prepared TiO₂@PPy coreshell nanocomposites were also studied for their dielectric losses for alternating current (AC) which is useful characteristic for their application in the fabrication of charge storing devices. TiO₂@PPy coreshell nanocomposites showed synergistic effect of combining components in improving their alcohol sensing properties. This improvement may be attributed to the adsorption on and desorption from alcohols TiO₂@PPy interface of the nanocomposites and alcohol vapors causing decrease in depletion region. The TiO₂@PPy coreshell nanocomposites were observed to show better reproducibility of electrical conductivity and fast self‐recovery during the alcohol vapor sensing process. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 43411.     

Synthesis of aminated glycidyl methacrylate grafted rice husk and investigation of its anion‐adsorption properties

In this study, we focused on the synthesis, characterization, and adsorption capacity testing of aminated glycidyl methacrylate grafted rice husk (RH‐g‐GMA–Am). Our goal was to obtain a high‐performance surface for the adsorption of various anions. Glycidyl methacrylate grafted rice husk (RH‐g‐GMA) was prepared by the graft copolymerization of glycidyl methacrylate with rice husk; the product was further subjected to an amination reaction. The surface properties, sorption characteristic functional groups, isotherm and kinetic studies, pore diffusion models, and effects of the temperature and pH on the material properties were studied under batch conditions. The IR spectroscopy results show additional surface functional groups for RH‐g‐GMA–Am. The adsorptions of and on RH‐g‐GMA–Am were found to follow pseudo‐second‐order kinetics; this indicated a possible dominant role played by chemisorption. The rate‐limiting step for mass transfer was found to be boundary layer diffusion. Furthermore, the sorption isotherms for and fit the Langmuir model. The amination of RH‐g‐GMA drastically increased the removal efficiency from 3 to 82% and from 6 to 93% for and , respectively. Moreover, RH‐g‐GMA–Am exhibited a better removal efficiency in the pH range of 4–6.5. Regeneration studies revealed that the surface of RH‐g‐GMA–Am could be regenerated repetitively by simple acid washing with an insignificant decrease in the active surface for consecutive adsorptions. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 43002.