The intercalation of ammonium sulfamate into kaolinite and its effect on the fire performance of polypropylene

2017 ◽  
Vol 31 (10) ◽  
pp. 1352-1370 ◽  
Author(s):  
Wufei Tang ◽  
Hongfei Li ◽  
Sheng Zhang ◽  
Jun Sun ◽  
Xiaoyu Gu

Kaolinite has often been intercalated before being introduced into polymers to improve its dispersibility; however, the conventional intercalation usually reduces the flame retardancy of the composite. This work reports our recent efforts on improving both the flame retardant efficiency and dispersibility of kaolinite in polypropylene (PP) by intercalating with ammonium sulfamate (AS). The intercalation had been performed through three steps: dimethyl sulfoxide was firstly introduced into kaolinite layers under supersonic wave, then it was replaced by potassium acetate-aqueous (KAc), and finally the intercalated KAc was replaced by AS to obtain AS-intercalated kaolinite. The structure of intercalated kaolinite was characterized by X-ray diffraction (XRD), Fourier-transform infrared spectroscopy, and thermogravimetric analysis (TGA). The flammability evaluation by limit oxygen index, vertical burning test (UL-94), cone calorimeters test (CONE), and TGA indicated that the fire resistance, thermal stability, and physical properties of PP can be effectively enhanced by the introduction of AS-intercalated kaolinite. The peak heat release rate (pHRR) value of PP composite containing only 1.5 wt% intercalated kaolinite (1169 kW m−2) had been reduced 13.2% compared with that of the sample containing 1.5 wt% raw kaolinite (1346 kW m−2). The morphology analysis from scanning electron microscope images and XRD patterns demonstrated that the compatibility and dispersibility of kaolinite in PP had been significantly improved by intercalation. The flame retardant mechanism of AS-intercalated kaolinite in PP was proposed.

BioResources ◽  
2021 ◽  
Vol 16 (4) ◽  
pp. 7953-7965
Author(s):  
Qijie Chen ◽  
Zhi Rong ◽  
Zhuo Liu ◽  
Na You ◽  
Guangyang Xie

A flame retardant containing phosphorus and nitrogen was synthesized using phytic acid and dicyandiamide, and it was subsequently used to prepare flame-retardant cellulosic paper via an impregnation method. Vertical flame and limiting oxygen index (LOI) were used to evaluate the flame retardancy of the paper. The paper containing modified phytic acid was characterized with Fourier transform infrared spectroscopy (FTIR), thermogravimetry (TG), X-ray diffraction (XRD), and scanning electron microscopy (SEM). When the concentration of modified phytic acid was 20%, the char length of the treated paper decreased from 12.5 cm to 4.1 cm, the LOI value increased from 19.6% to 41.5%, and the tensile index was only 3.66% lower than that of the control paper. The modified phytic acid was judged to have good flame-retardant effects on the paper.


Coatings ◽  
2019 ◽  
Vol 9 (8) ◽  
pp. 479 ◽  
Author(s):  
Yachao Wang ◽  
Jiangping Zhao

An ecological ammonium thiocyanate (NH4SCN)-modified geopolymeric coating was facilely prepared for flame-retarding plywood. The effect of NH4SCN on the flame resistance was preliminarily investigated using cone calorimeter (CC), scanning electron microscope (SEM), X-ray diffraction (XRD), and thermal gravimetry (TG). The results show that 1 wt.% NH4SCN as dopant is of paramount importance to generate a compact and continuous coating. The formation of a smooth, intact, and uniform-swelling siliceous layer during combustion facilitates enhanced fire resistance, evidenced by the increased fire performance index (FPI), reduced fire growth index (FGI), and 39.7% decreased value of peak heat release rate (pHRR), in comparison to those of the sample without NH4SCN. Because of the reducibility of O2-consuming NH4SCN, the compact shielding-layer containing carbonate and sulfate, as well as the release of NH3, the NH4SCN-modified geopolymeric coating exerts an enhancement on the flame-retardant efficiency.


2019 ◽  
Vol 9 (17) ◽  
pp. 3464 ◽  
Author(s):  
Tentu Nageswara Rao ◽  
Imad Hussain ◽  
Ji Eun Lee ◽  
Akshay Kumar ◽  
Bon Heun Koo

Zirconia (ZrO2)-based flame retardant coatings were synthesized through the process of grinding, mixing, and curing. The flame retardant coatings reinforced with zirconia nanoparticles (ZrO2 NPs) were prepared at four different formulation levels marked by F0 (without adding ZrO2 NPs), F1 (1% w/w ZrO2 NPs), F2 (2% w/w ZrO2 NPs), and F3 (3% w/w ZrO2 NPs) in combination with epoxy resin, ammonium polyphosphate, boric acid, chitosan, and melamine. The prepared formulated coatings were characterized by flammability tests, combustion tests, and thermogravimetric analysis. Finally, char residues were examined with scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDS). The peak heat release rate (PHRR) of the controlled sample filled with functionalized ZrO2 NPs was observed to decrease dramatically with increasing functionalized ZrO2 NPs loadings. There was an increase in the limit of oxygen index (LOI) value with the increase in the weight percentage of ZrO2 NPs. The UL-94V data clearly revealed a V-1 rating for the F0 sample; however, with the addition of ZrO2 NPs, the samples showed enhanced properties with a V-0 rating. Thermal gravimetric analysis (TGA) results revealed that addition of ZrO2 NPs Improved composite coating thermal stability at 800 °C by forming high residual char. The results obtained here reveal that the addition of ZrO2 NPs in the formulated coatings has shown the excellent impact as flame retardant coatings.


2018 ◽  
Vol 20 ◽  
pp. 92-105 ◽  
Author(s):  
Sara Verusca de Oliveira ◽  
E.A. dos Santos Filho ◽  
Edcleide Maria Araújo ◽  
C.M. Correia Pereira ◽  
Fábio Roberto Passador

Polyethylene (PE) nanocomposites were prepared by melt intercalation, in order to evaluate the flame retardant effect of this material. For the development of nanocomposites were used the montmorillonite clay (MMT), organoclay (OMMT) and flame retardant product (FRP) with the percentage of 1, 3, 6 and 9 wt%. Grafted polyethylene with maleic anhydride (PE-g-MA) was used as a compatibilizer of the systems. PE and its systems were evaluated: XRD, TEM, TG and flammability (UL94HB, oxygen index (LOI) and cone calorimetry). The X-ray diffraction showed a partial intercalation and exfoliation as well as formation of microcomposite. The phase morphology of the systems was observed by TEM that it showed that the system with 1% OMMT clay presented a predominance of exfoliation. Already the system with 3% OMMT showed partial exfoliation and this exfoliation reduced as the clay content increased. By TG it was seen that MMT, OMMT and FRP acted improving the thermal behavior of the nanocomposites compared to PE matrix. The results obtained for the oxygen index showed that both PE and its systems presented flame retardancy behavior. By means of the horizontal flammability tests, it was found that the presence of 1% MMT clay reduced 25% the flammability of PE. By cone calorimetry it was found that the system that contains 9% of OMMT clay decreased by about 33% the flammability of PE.


2010 ◽  
Vol 174 ◽  
pp. 362-365 ◽  
Author(s):  
Song Lin Wang ◽  
Xiao Ming Song

The feasibility and technological conditions of the preparation of flame retardant paper based on fiber using co-precipitation synthesis of Mg-Al hydrotalcites as filler in papers were investigated. The crystallizations, granularities of Mg-Al hydrotalcites and characters of flame retardant papers were investigated through transmission election microscope and X-ray diffraction technique etc. The results indicated that Mg-Al hydrotalcites were layered hexagonal nanoparticles, with perfectly crystallized structure and striking performance in furnish retention improvement. The flame retardant papers based on fiber using Mg-Al hydrotalcites as fillers have excellent inflaming retarding performance. The oxygen index of the flame retardant paper produced is above 25 % at the dosage of 15 wt%.


2020 ◽  
Vol 10 (03) ◽  
pp. 2050003
Author(s):  
M. R. Hassan ◽  
M. T. Islam ◽  
M. N. I. Khan

In this research, influence of adding Li2CO3 (at 0%, 2%, 4%, 6%) on electrical and magnetic properties of [Formula: see text][Formula: see text]Fe2O4 (with 60% Ni and 40% Mg) ferrite has been studied. The samples are prepared by solid state reaction method and sintered at 1300∘C for 6[Formula: see text]h. X-ray diffraction (XRD) patterns show the samples belong to single-phase cubic structure without any impurity phase. The magnetic properties (saturation magnetization and coercivity) of the samples have been investigated by VSM and found that the higher concentration of Li2CO3 reduces the hysteresis loss. DC resistivity increases with Li2CO3 contents whereas it decreases initially and then becomes constant at lower value with temperature which indicates that the studied samples are semiconductor. The dielectric dispersion occurs at a low-frequency regime and the loss peaks are formed in a higher frequency regime, which are due to the presence of resonance between applied frequency and hopping frequency of charge carriers. Notably, the loss peaks are shifted to the lower frequency with Li2CO3 additions.


Author(s):  
Peng Liu ◽  
Hongbin Zhang ◽  
Sinong Wang ◽  
Hui Yu ◽  
Bingjie Lu ◽  
...  

AbstractThe crystallinity indices (CrI) of Chinese handmade papers were investigated using the X-ray diffraction (XRD) method. Four Chinese handmade papers, Yingchun, Zhuma, Yuanshu and Longxucao papers were used as model substrates of mulberry bark, ramie, bamboo and Eulaliopsis binata papers, respectively. Two forms of the paper samples, paper sheets and their comminuted powders, were used in this study. The results showed that their XRD patterns belong to the cellulose-I type and Iβ dominates the cellulose microstructure of these paper samples. Moreover, it was found that the microstructures and CrIs of cellulose of these papers were changed by the grinding treatment. This work suggested that the sheet form of the handmade papers is suitable to determine CrI by XRD, despite the contribution of non-cellulosic components in the papers. The order of CrIs for these paper sheet samples was Yingchun, Zhuma, Longxucao and Yuanshu papers. Besides CrIs, differences in cross-sectional areas of the crystalline zone of cellulose can be used for comparing different types of handmade papers. It was also found that the CrIs and crystallite size of paper cellulose varied between the sheet samples and the powder samples, illustrating that the pulverisation has a negative influence on the microstructure of the handmade papers.


2014 ◽  
Vol 1061-1062 ◽  
pp. 83-86
Author(s):  
Hong Wu ◽  
De Yi Zheng

In this paper, the effects of different sintering temperature on the microstructure and piezoelectric properties of Pb(Nb2/3Zn1/3)0.03(Zr52Ti48)0.97O3(PNZZT) ceramic samples were investigated. The Pb(Nb2/3Zn1/3)0.03(Zr52Ti48)0.97O3 ceramics materials was prepared by a conventional mixed oxide method. In the period of the experiment, the relationship between crystallographic phase and microstructure were analyzed by X-ray diffraction(XRD) and scanning electron microscopy(SEM) respectively. The XRD patterns shows that all of the ceramic samples are with a tetragonal perovskite structure. Along with sintering temperature increased and the x is 0.03, the grain size gradually become big. Through this experiment, it has been found that when the x is 0.03 and sintered at 1130°C for 2 h, the grains grow well, the grain-boundary intersection of the sample combined well and the porosity of the ceramics decreased, an excellent comprehensive electrical properties of the Pb(Nb2/3Zn1/3)0.03(Zr52Ti48)0.97O3 samples can be obtained. Its best electrical properties are as follows: dielectric constant (ε) is 1105, dielectric loss(tg) is 0.017, electromechanical coupling coefficient (Kp) is 0.287, piezoelectric constant(d33) is 150PC/N


2009 ◽  
Vol 79-82 ◽  
pp. 71-74
Author(s):  
Qi Wang ◽  
Lin Qiao ◽  
Peng Song

In this paper, the resistance to H2S attack of pastes made from slag-fly ash blended cement used in oil well (SFAOW) was studied, in which fly ash (FA) was used at replacement dosages of 30% to 60% by weight of slag. Samples of SCOW and SFAOW pastes were demoulded and cured by immersion in fresh water with 2 Mp H2S insulfflation under 130oC for 15 days. After this curing period, compression strength and permeability of the samples were investigated. The reaction mechanisms of H2S with the paste were carried out through a microstructure study, which included the use of x-ray diffraction (XRD) patterns and scanning electron microscope (SEM). Based on the obtained data in this study, incorporation of FA into SCOW results in the comparable effects in the resistance to H2S attack. When the replacement dosage of slag is about 40%, the paste exhibits the best performance on resistance to H2S attack with compression strength 36.58Mp.


2013 ◽  
Vol 12 (01) ◽  
pp. 1350006
Author(s):  
AHMED E. HANNORA ◽  
FARIED F. HANNA ◽  
LOTFY K. MAREI

Mechanical alloying (MA) method has been used to produce nanocrystallite Mn -15at.% Al alloy. X-ray diffraction (XRD) patterns for the as-milled elemental α- Mn and aluminum powder samples show a mixture of α + β- MnAl phases after 20 h of milling and changes to a dominant β- MnAl phase structure after 50 h. An average crystallite size of 40 nm was determined from Hall–Williamson method analysis after 5 h of milling. Moreover, the thermal analysis results using differential thermal analysis (DTA), suggested a possible phase transformation after 20 h of milling. Isothermal treatments are carried in the temperature range of 450°C to 1000°C. Room-temperature vibrating sample magnetometer (VSM) measurements of the hysteretic response revealed that the saturation magnetization Bs and coercivity Hc for 10 h ball milled sample are ~ 2.1 emu/g and ~ 92 Oe, respectively.


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