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1.
1H‐ and 13C‐NMR spectroscopy and FT‐Raman spectroscopy are used to investigate the properties of a polymer gel dosimeter post‐irradiation. The polymer gel (PAG) is composed of acrylamide, N,N′‐methylene‐bisacrylamide, gelatin, and water. The formation of a polyacrylamide network within the gelatin matrix follows a dose dependence nonlinearly correlated to the disappearance of the double bonds from the dissolved monomers within the absorbed dose range of 0–50 Gy. The signal from the gelatin remains constant with irradiation. We show that the NMR spin–spin relaxation times (T2) of PAGs irradiated to up to 50 Gy measured in a NMR spectrometer and a clinical magnetic resonance imaging scanner can be modeled using the spectroscopic intensity of the growing polymer network. More specifically, we show that the nonlinear T2 dependence against dose can be understood in terms of the fraction of protons in three different proton pools. © 2000 John Wiley & Sons, Inc. J Appl Polym Sci 79: 1572–1581, 2001  相似文献   

2.
The chemical mode of action as a flame retardant of calcium carbonate nanoparticles combined with ammonium polyphosphate in polypropylene was investigated. Reduction in burning rates for 0.5 mm thick samples were observed without appreciable char formation up to 30 wt % loading of additives. Thermogravimetric analysis (TGA) of the mixture of CaCO3 and ammonium polyphosphate (APP) showed that calcium carbonate nanoparticles react with ammonium polyphosphate before the degradation of the phosphate chains. TGA–FTIR studies of the polymer composite samples and powder mixtures of the additives confirmed the evolution of ammonia and carbon dioxide due to interaction between the additives. X‐ray diffraction (XRD) analysis of chars, obtained after burning the films, showed definite diffraction peaks corresponding to that of calcium metaphosphate. The inert gasses produced by the interaction of the additives hindered the advancing flame and, thus, reduces the burning rates, at times even without char formation. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2011  相似文献   

3.
A novel flame‐retardant synergist, chitosan/urea compound based phosphonic acid melamine salt (HUMCS), was synthesized and characterized by Fourier transform infrared spectroscopy and 31P‐NMR. Subsequently, HUMCS was added to a fire‐retardant polypropylene (PP) compound containing an intumescent flame‐retardant (IFR) system to improve its flame‐retardant properties. The PP/IFR/HUMCS composites were characterized by limiting oxygen index (LOI) tests, vertical burning tests (UL‐94 tests), microscale combustion calorimetry tests, and thermogravimetric analysis to study the combustion behavior and thermal stability. The addition of 3 wt % HUMCS increased the LOI from 31.4 to 33.0. The addition of HUMCS at a low additive amount reduced the peak heat‐release rate, total heat release, and heat‐release capacity obviously. Furthermore, scanning electron micrographs of char residues revealed that HUMCS could prevent the IFR–PP composites from forming a dense and compact multicell char, which could effectively protect the substrate material from combusting. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 40845.  相似文献   

4.
Mg(OH)2 (MH) nanoparticles were synthesized by hydration of the light‐burned MgO at low temperature (70°C). Effects of additives, such as magnesium nitrate and magnesium acetate, on the size, morphology and agglomeration of MH particles were investigated. MH nanoparticles have platelet‐like structure and approximately 20–40 nm in thicknesses. The supersaturation degree plays an important role in magnesia hydration and is defined. When magnesium acetate was used as the additive, the hydroxyl ion can be homogeneously introduced into the solution. The size and morphology of MH nanoparticles are more homogeneous. Modified by titanate coupling agent, MH nanoparticles were used as the flame retardant for polypropylene (PP). The combustibility, mechanical properties and thermal behaviors of the PP/MH composites were characterized. The mechanical properties of PP/MH composites are not seriously deteriorated with increasing MH content. When the amount of MH fraction reached 65, the limiting oxygen index (LOI) value and UL 94 testing result of MH65 are 33.8 and V‐0 grading, respectively. The onset temperature (T10%) and the maximum thermal decomposition temperature (Tmax) of MH65 separately increased by approximately 100°C and 77°C than those of neat PP. Copyright © 2012 John Wiley & Sons, Ltd.  相似文献   

5.
A series of polymeric flame retardants (PFRs) containing phosphorus‐nitrogen‐bromide were synthesized from spirocyclic pentaerythritol bisphosphorate disphosphoryl chloride (SPDPC), 2‐methoxyl‐4,6‐dichloro‐1,3,5‐triazine (MDCT), and tetrabromobisphenol A (TBBPA). The influence of monomer ratio on their thermal stability was investigated by adjusting the proportion of SPDPC/MDCT (mol/mol) from 80/20 to 20/80. The flammability properties of the PFRs blended with ABS were evaluated using LOI and UL‐94 vertical test. The structures of the flame retardants were characterized by means of Fourier transform infrared spectra (FTIR) and proton nuclear magnetic resonance spectroscopy (1H‐NMR). The results show that the initial temperature of decomposition is 274°C and with 35% charring residue at 500°C when the ratio of SPDPC/MDCT is 50/50. V‐0 ratings in the UL‐94 vertical test were achieved at 20–30% loading of PFRs, when LOI values reached at least 26.9%. The flame retardancy is strongly dependent on the ratio of P, N, and Br. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2010  相似文献   

6.
Nanocomposite UV coatings with adjustable properties for use on wood substrates in outdoor conditions were developed. Nanoscale ZnO was shown to be an efficient light absorber. Coatings were characterized in terms of elongation at brake, residual PI and double bond conversion, universal hardness, transparency, hydrophobicity, and yellowing. Coated samples were artificially weathered and studied with regard to their optical and mechanical properties, as well as to changes in brightness, transparency, hydrophobicity, and water permeability. The prepared wood coatings showed an increased weather fastness and improved optical properties. The suitability for use in outdoor conditions was assured by optimizing the elasticity of the coating and decreasing its water permeability.

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7.
A sulfur‐containing flame retardant (SFR) was synthesized from polyphosphoric acid, epoxy chloropropane, and thiourea. Using a water‐soluble isocyanate‐terminated (WIT) cross‐linker, the flame retardant was applied as a flame‐retardant finishing on nylon fabric. WIT is a compound that not only cross‐links SFR and nylon cellulose but also contains no formaldehyde. Comparisons of the main performances of SFR with those of N‐methyloldimethylphosphonopropionamide (known as ‘Pyrovatex CP’) and a bicyclic phosphonite (known as ‘Antiblaze 19T’) indicate that the presence of sulfur in SFR plays a crucial role in decreasing the flammability of the nylon fabric. The limiting oxygen index value and damaged carbon length of the finished nylon fabric were 29.4% and 5.7 cm, respectively, when the concentrations of SFR and WIT were 200 and 40 g/L, respectively, and the baking temperature and time were 150 °C and 3 min, respectively. After 10 laundry cycles, the fabric still retains some flame retardancy. Copyright © 2016 John Wiley & Sons, Ltd.  相似文献   

8.
A novel flame retardant (SPDH) containing phosphorus was synthesized through the reaction of 10‐(2, 5‐dihydroxyphenyl)‐9, 10‐dihydro‐9‐oxa‐10‐phosphaphenanthrene‐10‐oxide (DOPO‐HQ) and synthesized intermediate product 3, 9‐dichloro‐2, 4, 8, 10‐tetraoxa‐3, 9‐diphosphaspiro(5.5)undecane‐3, 9‐dioxide (SPDPC). The structure and properties of SPDPC and SPDH were characterized by Fourier transform infrared spectroscopy (FTIR), nuclear magnetic resonance (NMR) spectroscopy and thermogravimetric analysis (TGA). After blending with poly(ethylene‐co‐vinyl acetate) (EVA), the flame‐retardant properties of EVA/SPDH composites were estimated by cone calorimeter, limited oxygen index (LOI) and UL‐94 tests, whereas the thermal stabilities were investigated using TGA. The morphological microstructure of the char formed by EVA/SPDH composite after combustion in cone calorimeter was investigated by scanning electron microscopy (SEM). The results indicate that the flame retardant and thermal stability were improved by incorporation of SPDH. The rich foamy char layers were observed from the residues after combustion in a cone calorimeter, which exactly benefits the improvement of thermal stability and flame retardant property of materials. Copyright © 2010 John Wiley & Sons, Ltd.  相似文献   

9.
Fluorescence intensity ratios (FIRs) of the 640 nm and 602 nm emissions from Sm3+ were recorded at various temperatures T to identify the temperature increases ΔT associated with laser‐induced local heating of Ag nanoparticles. The FIRs increased as intensities of the excitation beam from a 532‐nm continuous‐wave laser increased. Estimated T of the irradiated region increased to as high as 586°C when at laser irradiation of 1.5 W on the surface containing Ag nanoparticles. Local heating due to the surface plasmon resonance of Ag nanoparticles is a main reason for the ΔT that eventually leads to precipitation of PbS quantum dots in glasses.  相似文献   

10.
Eu3+‐doped Mg3‐xEux(BO3)2 (x = 0.000, 0.005, 0.010, 0.020, 0.050, and 0.100) phosphors were synthesized for the first time by solution combustion synthesis method, which is a fast synthesis method for obtaining nano‐sized borate powders. The optimization of the synthesis conditions of phosphor materials was performed by TG/DTA method. These phosphors were characterized by XRD, FTIR, SEM‐EDX, and photoluminescence, PL analysis. The XRD analysis exhibited that all of the prepared ceramic compounds have been crystallized in orthorhombic structure with space group Pnnm. Also, the influence of europium dopant ions on unit cell parameters of host material was analyzed using Jana2006 program and the crystalline size was determined by Debye‐Scherrer's formula. The luminescence properties of all Eu3+‐doped samples were investigated by excitation and emission spectra. The excitation spectra of Mg3‐xEux(BO3)2 phosphors show characteristic peak at 420 nm in addition to other characteristic peaks of Eu3+ under emission at 613 nm. The emission spectra of Eu3+‐doped samples indicated most intensive red emission band dominated at 630 nm belonging to 5D07F2 magnetic dipole transition. Furthermore, the optimum or quenching concentration of Eu3+ ion has been determined as x = 0.010 showed the maximum emission intensity when it was excited at 394 nm.  相似文献   

11.
Molybdates of Li+ and Yb3+ are studied to investigate the luminescence under UV excitation. LiYb(MoO4)2 and Eu3+‐doped LiYb1xEux(MoO4)2 (x=001–1.0) phosphors were synthesized by solid state reaction under mixing of Eu2O3, Yb2O3, Li2CO3 and MoO2 in air atmosphere. Two broad absorption bands centered at 333 and 236 nm are observed in LiYb(MoO4)2 compound. They are attributed to the 1A11T1 and 1T2 transitions due to the O2?→Mo6+ electron transfers in MoO4 tetrahedron. An emission band with a peak at about 440 nm is found, which is attributed to the 3T11A1 transition of MoO4. Appearance of near‐infrared (NIR) Yb3+ emission observed under UV excitation is understood by the MoO4→Yb3+ Foerster‐Type energy transfer due to spectral overlap between the low‐energy tail of the broad 440 nm emission band and the high‐energy tail of the broad Yb3+ absorption band and due to short Yb3+‐MoO4 distance. Yb3+ emission observed in LiYb1?xEux(MoO4)2 by Eu3+ excitation is understood by the Eu3+→Yb3+ energy transfer by cross‐relaxation (CR) process between the 5D07F6 Eu3+ transition and the 2F7/22F5/2 Yb3+ transition. The CR efficiency shows maximum efficiency of 0.24 at x=0.15 of higher acceptor Yb3+ concentration than donor Eu3+ concentration. Three Yb3+ emission bands with peaks at 994, 1002, and 1023 nm are observed, depending on the excitation wavelength. This is explained by less‐shielded 4f electrons of Yb3+ by the 5s25p6 outermost electron shells, which are also responsible for unusual broadband Yb3+ absorption and emission. From appearance of NIR Yb3+ emission under excitation by not only UV light but also red light, these compounds are expected to be suitable for efficient photovoltaic application to Si‐based solar cells.  相似文献   

12.
Two novel triazine ring‐containing macromolecules, designated as charring‐foaming agent 1 (CFA1) and charring‐foaming agent 2 (CFA2), were synthesized by a series of polycondensation reactions. Their chemical structures were analyzed by Fourier transform infrared spectroscopy (FTIR), nuclear magnetic resonance spectroscopy (13C solid‐state NMR), and elemental analysis, and their thermal degradation properties were assessed by thermogravimetric analysis (TGA). TGA data revealed that CFA1 and CFA2 show high thermal stability and have a high propensity for char formation, their initial decomposition temperatures being 300.2°C and 287.1°C, and their char residues at 800°C amounting to 32.2 wt % and 21.1 wt %, respectively. CFA1 presents higher thermal stability and more char residue than CFA2. Based on experimental results of the flame retardancy (limiting oxygen indices values and UL‐94 V‐0 rating) and the TG data of new intumescent flame retardant polypropylene (IFR‐PP) containing CFA1 and CFA2, CFA1 exhibits more outstanding intumescent flame retardance than CFA2. IFRs containing CFA1 and CFA2 enhanced Notched Izod Impact strength of IFR‐PP, and slightly lower tensile strength of IFR‐PP. IFR2 shows more advantageous effect on mechanical properties of IFR‐PP than IFR1. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010  相似文献   

13.
Miaojun Xu  Xu Li  Bin Li 《火与材料》2016,40(6):848-860
A novel cross‐linked organophosphorus–nitrogen polymetric flame retardant additive poly(urea tetramethylene phosphonium sulfate) defined as PUTMPS was synthesized by the condensation polymerization between urea and tetrahydroxymethyl phosphonium sulfate. Its chemical structure was well characterized by Fourier transform infrared (FTIR) spectroscopy, 13C and 31P solid‐state nuclear magnetic resonance. The synthesized PUTMPS and curing agent m‐phenylenediamine were blended into epoxy resins to prepare flame retardant epoxy resin thermosets. The effects of PUTMPS on fire retardancy and thermal degradation behavior of EP/PUTMPS thermosets were investigated by limiting oxygen index (LOI), vertical burning test (UL‐94), cone calorimeter measurement, and thermalgravimetric analysis (TGA) tests. The surface morphologies and chemical compositions of char residues for cured epoxy resins were investigated by scanning electron microscopy and X‐ray photoelectron spectroscopy (XPS), respectively. Water resistant properties of epoxy resin thermosets were evaluated by putting the samples into distilled water at 70°C for 168 h. The results demonstrated that the EP/12 wt% PUTMPS thermosets successfully passed UL‐94 V‐0 flammability rating and the LOI value reached 31.3%. The TGA results indicated that the incorporation of PUTMPS promoted epoxy resin matrix decomposed and char forming ahead of time, which led to a higher char yield and thermal stability for epoxy resin thermosets at high temperature. The morphological structures and analysis of XPS for the char residues of the epoxy resin thermosets shown that PUTMPS benefited to the formation of a sufficient, more compact, and homogeneous char layer with rich flame retardant elements on the materials surface during burning, which prevented the heat transmission and diffusion, limited the production of combustible gases, inhibited the emission of smoke, and then led to the reduction of the heat release rate and smoke produce rate. After water resistance tests, EP/12 wt% PUTMPS thermosets still remained excellent flame retardancy. Copyright © 2015 John Wiley & Sons, Ltd.  相似文献   

14.
10‐Ethyl‐9‐oxa‐10‐phosphaphenanthrene‐10‐oxide ( 1 ) can be nitrated using acetic anhydride and fuming nitric acid. The nitro group is reduced using palladium on charcoal and hydrogen. These reaction conditions are used for the synthesis of an analogous DOPO‐based diaminic hardener ( 7 ). An evaluation of the curing behavior, mechanical properties and flammability of a neat resin made of DGEBA and 7 (DGEBA + 7 ) and of a carbon fiber‐reinforced resin made of DGEBA, 4,4′‐diaminodiphenylsulfon (DDS) and 7 (DGEBA + DDS + 7 ) shows the potential of this hardener to lead to flame‐retardant systems while keeping relevant properties on a high level; especially when compared to a similar system (DGEBA + DDS + 1 ).

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15.
BACKGROUND: Most enzymes, including protease, play a key role in biotechnology, but their use is quite limited due to poor recovery, limited reusability and instability. Immobilized enzymes offer advantages over free enzymes. This paper reports a simple method for the preparation of immobilized papain, an endolytic cysteine protease (EC: 3.4.22.2), on carboxyl‐activated silica nanoparticles. RESULTS: The carboxyl‐activated carriers produced reactive carboxyl groups which then react with the free amino groups of enzyme to give peptide bonds (? CO? NH? ). The results showed that the thermal and pH stabilities of the immobilized papain were higher than those of free enzyme. And the apparent Km value of the immobilized papain was 1.26 times higher than that of free enzyme. Moreover, the immobilized papain retained more than 45% of the original activity after ten reuses continuously. CONCLUSION: The results indicated that papain was successfully immobilized on the surface of the activated carriers. The immobilized papain had not only higher activity recovery, but also better stability, reusability and environmental adaptability. Copyright © 2012 Society of Chemical Industry  相似文献   

16.
A phosphorus‐containing amine, bis(4‐aminophenoxy)phenyl phosphine oxide (BAPP), suitable for curing epoxy resins with improved fire performance was synthesized and characterized with Fourier transform infrared spectroscopy and nuclear magnetic resonance. The reactivity of the amino group was evaluated by differential scanning calorimetry of the epoxy–amine mixture and by proton nuclear magnetic resonance of the amino unit. With BAPP as a curing agent, a range of high‐functionality, aerospace epoxy resins were cured, and the dynamic kinetic parameters calculated from Kissinger's and Ozawa's models were compared with those from the more widely used amines. The thermal degradation properties of the phosphorus‐containing epoxy resins were studied by thermogravimetric analysis, the degradation activation energy was calculated, and a multistep thermal degradation process was observed. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 92: 2093–2100, 2004  相似文献   

17.
Two novel copolymers of polyfluorenes/poly(p‐phenylenevinylene)s copolymers with ptert‐butyl‐phenylenemethylene groups in the C‐9 position of alternating fluorene unit, poly[1,4‐(2,5‐dibutyloxyl)‐phenyleneviny lene‐alt‐9‐(ptert‐butyl‐phenylenemethylene)fluorene] and poly[1,4‐(2,5‐dioctyloxyl)‐phenylenevinylene‐alt‐9‐(ptert‐butyl‐phenylenemethylene)fluorine], have been synthesized via the Heck polycondensation reaction. The synthesized polymers were characterized by FTIR, NMR, DSC, TGA, UV–vis, and PL spectra. The polymers showed high glass transition temperatures and good thermal stability. A polymer light‐emitting diode with the configuration ITO/PEDOT:PSS/P2/Ca/Al has been fabricated. The device emitted a yellow light with a peak wavelength of 578 nm similar to the PL spectra of the copolymer film. A maximal luminance of 534 cd/m2 was obtained at a driving voltage of 24.5 V. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 102: 3955–3962, 2006  相似文献   

18.
This paper describes the synthesis of phosphorus‐containing polyester‐urethanes and their applications in nanoclay composites and coatings. Polyester was prepared by the reaction of bis(bisphenol‐A) monophenyl phosphonate, maleic anhydride and phthalic anhydride. The polyester was reacted with various diols such as ethylene glycol, diethylene glycol and propylene glycol to obtain polyester polyols. Synthesized polyester polyols were characterized by chemical analysis and instrumental analysis and was used further to react with different isocyanates to develop polyester‐urethanes. The synthesized polyester‐urethanes were blended with organo‐modified montmorillonite nanoclay (1 wt%, 3 wt% and 5 wt%) and were cast in a mold and coated on mild steel panels. The thermal stability of neat polyester‐urethane and the nanoclay composites was determined by thermogravimetric analysis. The flame retardant properties of cast films and their composites were determined by the limiting oxygen index and UL‐94 test methods. The physical and mechanical properties of coatings such as pot life, drying properties, scratch hardness, pencil hardness, impact resistance, adhesion and flexibility were investigated. The chemical resistance properties of the coatings were also determined in different reagents. The data reveal that the polyester‐urethane nanoclay composites with 3 wt% clay hold promise for use in effective flame retardant coatings. © 2013 Society of Chemical Industry  相似文献   

19.
In this study, thermoplastic poly(ester ether) elastomer (TPEE) nanocomposites with phosphorus–nitrogen (P–N) flame retardants and montmorillonite (MMT) were prepared by melt blending. The fire resistance of the nanocomposites was analyzed by limiting oxygen index (LOI) and vertical burning (UL 94) tests. The results show that the addition of the P–N flame retardants increased the LOI of the material from 17.3 to 27%. However, TPEE containing P–N flame retardants only obtained a UL 94 V‐2 ranking; this resulted in a flame dripping phenomenon. On the other hand, TPEE containing the P–N flame retardant and organically modified montmorillonite (o‐MMT) achieved better thermal stability and good flame retardancy; this was ascribed to its partially intercalated structure. The synergistic effect and synergism were investigated by Fourier transform infrared spectroscopy and thermogravimetry. The introduction of o‐MMT decreased the inhibition action of the P–N flame retardant and increased the amount of residues. The catalytic decomposition effect of MMT and the barrier effect of the layer silicates are discussed in this article. The residues after heating in the muffle furnace were analyzed by scanning electron microscopy, energy‐dispersive X‐ray spectroscopy and laser Raman spectroscopy. It was shown that the intercalated layer silicate structure facilitated the crosslinking interaction and promoted the formation of additional carbonaceous char residues in the formation of the compact, dense, folded‐structure surface char. The combination of the P–N flame retardant and o‐MMT in TPEE resulted in a better thermal stability and fire resistance because of the synergistic effect of the mixture. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 41094.  相似文献   

20.
A novel nitrogen‐containing cyclic phosphate (NDP) was synthesized and well characterized by 1H, 13C, 31P NMR, mass spectra and elemental analysis. NDP was used as an additive intumescent flame retardant (AIFR) to impart flame retardancy and dripping resistance for diglycidyl ether of bisphenol‐A epoxy resin (DGEBA) curied by 4,4′‐diaminodiphenylsulfone (DDS) with different phosphorus content. The flammability, thermal stability, and mechanical properties of NDP modified DGEBA/DDS thermosets were investigated by UL‐94 vertical burning test, differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), and Izod impact strength and flexural property tests. The results showed that NDP modified DGEBA/DDS thermosets exhibited excellent flame retardancy, moderate changes in glass transition temperature and thermal stability. When the phosphorus content reached only 1.5 wt %, the NDP modified DGEBA/DDS thermoset could result in satisfied flame retardancy (UL‐94, V‐0). The TGA curves under nitrogen and air atmosphere suggested that NDP had good ability of char formation, and there existed a distinct synergistic effect between phosphorus and nitrogen. The flame retardant mechanism was further realized by studying the structure and morphology of char residues using FT‐IR and scanning electron microscopy (SEM). It indicated that NDP as phosphorus‐nitrogen containing flame retardant worked by both of the condensed phase action and the vapor phase action. Additionally, the addition of NDP decreased slightly the flexural strength of the flame retarded DGEBA epoxy resins, and increased the Izod impact strength of these thermosets. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 41859.  相似文献   

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