Fire Self-Extinguishing Cotton Fabric: Development of Piperazine Derivatives Containing Phosphorous-Sulfur-Nitrogen and Their Flame Retardant and Thermal Behaviors  

作　　者：Thach-Mien Nguyen SeChin Chang Brian Condon Jade Smith 

机构地区：[1]United States Department of Agriculture, Agricultural Research Service, Southern Regional Research Center, New Orleans, USA

出　　处：《Materials Sciences and Applications》2014年第11期789-802,共14页材料科学与应用期刊（英文）

摘　　要：Recent studies have shown interest in flame retardants containing phosphorus, nitrogen and sulfur a combination small molecule with a promising new approach in preparing an important class of flame retardant materials. Tetraethyl piperazine-1,4-diyldiphosphonate (TEPP) and O,O,O’,O’- tetramethyl piperazine-1,4-diyldiphosphonothioate (TMPT), based on Piperazine derivatives, were prepared successfully and their structures were proved by means of 1H, 13C and 31P NMR. Cotton twill fabric was treated with both compounds to provide different add-on levels. Thermogravimetric Analysis (TGA), microscale combustion calorimeter (MCC), vertical and 45° flame test and limiting oxygen index (LOI) were performed on the treated cotton fabrics and showed promising results. When the treated twill fabrics (5 wt% - 7 wt% add-ons) were tested using the vertical flammability test (ASTMD6413-11), we observed that the ignited fabrics self extinguished and left behind a streak of char. Limiting oxygen index (LOI, ASTM 2863-09) was utilized to determine the effectiveness of the flame retardant on the treated fabrics. LOI values increased from 18 vol% oxygen in nitrogen for untreated twill fabric to a maximum of 30 vol% for the highest add-on of twill. Furthermore, Scanning Electron Microscope (SEM), Attenuated Total Reflection-Infrared (ATR-IR), and Thermogravimetric Analysis-Fourier Transform Infrared (TGA-FTIR) spectroscopy were employed to characterize the chemical structure on the treated fabrics, as well as, the surface morphology of char areas of treated and untreated fabrics. Additionally, analysis of the release gas products by TGA-FTIR shows some distinctive detail in the degradation of the treated fabrics during the burning process.Recent studies have shown interest in flame retardants containing phosphorus, nitrogen and sulfur a combination small molecule with a promising new approach in preparing an important class of flame retardant materials. Tetraethyl piperazine-1,4-diyldiphosphonate (TEPP) and O,O,O’,O’- tetramethyl piperazine-1,4-diyldiphosphonothioate (TMPT), based on Piperazine derivatives, were prepared successfully and their structures were proved by means of 1H, 13C and 31P NMR. Cotton twill fabric was treated with both compounds to provide different add-on levels. Thermogravimetric Analysis (TGA), microscale combustion calorimeter (MCC), vertical and 45° flame test and limiting oxygen index (LOI) were performed on the treated cotton fabrics and showed promising results. When the treated twill fabrics (5 wt% - 7 wt% add-ons) were tested using the vertical flammability test (ASTMD6413-11), we observed that the ignited fabrics self extinguished and left behind a streak of char. Limiting oxygen index (LOI, ASTM 2863-09) was utilized to determine the effectiveness of the flame retardant on the treated fabrics. LOI values increased from 18 vol% oxygen in nitrogen for untreated twill fabric to a maximum of 30 vol% for the highest add-on of twill. Furthermore, Scanning Electron Microscope (SEM), Attenuated Total Reflection-Infrared (ATR-IR), and Thermogravimetric Analysis-Fourier Transform Infrared (TGA-FTIR) spectroscopy were employed to characterize the chemical structure on the treated fabrics, as well as, the surface morphology of char areas of treated and untreated fabrics. Additionally, analysis of the release gas products by TGA-FTIR shows some distinctive detail in the degradation of the treated fabrics during the burning process.

关 键 词：Flame Retardant Cotton Twill Fabric Phosphorus-Nitrogen-Sulfur THERMOGRAVIMETRIC Analysis-Fourier Transform Infrared (TGA-FTIR) MICROSCALE Combustion CALORIMETER (MCC) 

分 类 号：O6[理学—化学]