Phase‐transfer‐agent‐aided polymerization and graft copolymerization of acrylamide

The use of phase‐transfer catalysts, with water‐insoluble initiators, for polymerization and graft copolymerization reactions was explored. The polymerization of a water‐soluble vinyl monomer, acrylamide (AAm), and the graft copolymerization of AAm onto a water‐insoluble polymer backbone, isotactic polypropylene (IPP), with a water‐insoluble initiator, benzoyl peroxide (BPO), and a phase‐transfer catalyst, tetrabutyl ammonium bromide (Bu₄N⁺Br^?), were carried out in a water/xylene binary solvent system. The conversion percentage of AAm into polyacrylamide (PAAm) and the percentage of grafting of AAm onto IPP were determined as functions of various reaction parameters, such as the BPO, AAm, and phase‐transfer‐catalyst concentrations, the amounts of water and xylene in the water/xylene mixture, the time, and the temperature. The graft copolymer, IPP‐g‐PAAm, was characterized with IR spectroscopy and thermogravimetric analysis. By a comparison of the results of the phase‐transfer‐catalyzed graft copolymerization of AAm onto IPP and the preirradiation method, it was observed that the optimum reaction conditions were milder for the phase‐transfer‐catalyst‐aided graft copolymerization. Milder reaction conditions, including the temperature, the time of reaction, and a moderate initiator (BPO), in comparison with high‐energy γ‐rays, led to better quality products, and the reaction proceeded smoothly with high productivity. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 91: 2364–2375, 2004     

Syntheses and properties of N‐vinylpyrrolidione‐g‐EPDM and its modified polymer

The graft copolymerizations of N‐vinylpyrrolidione(NVP) onto ethylene–propylene–diene terpolymer (EPDM) were carried out with benzoyl peroxide (BPO) as an initiator in toluene. The synthesized EPDM‐g‐NVP (ENVP) was characterized by infrared (IR) spectroscopy and gel permeation chromatography (GPC). The effects of initiator and monomer concentrations, reaction time, and temperature were investigated in the graft copolymerization. The highest graft efficiency was obtained at 0.04 mol of NVP, 2 g of EPDM, 2 wt % of BPO and 80°C for 72 h. Modified ENVP (MENVP) was obtained by the reaction of ENVP and KOH in MeOH. Properties of EPDM, ENVP, and MENVP were investigated by a thermogravimetric analyzer (TGA), an instron tensile tester, a Fade‐O‐Meter, and a UV spectrophotometer. Tensile strength and light resistance of ENVP were better than those of MENVP. The dyeability of polymers was increased in following order: MENVP > ENVP > EPDM. © 1999 John Wiley & Sons, Inc. J Appl Polym Sci 72: 1177–1184, 1999     

Homogeneous graft copolymerization of acrylonitrile onto high α‐cellulose in a dimethyl acetamide and lithium chloride solvent system

Homogeneous graft copolymerization of acrylonitrile (AN) monomer onto high α‐cellulose was investigated in a lithium chloride/N,N‐dimethyl acetamide (DMAc/LiCl) solvent system. Benzoyl peroxide (BPO) and azobisisobutyronitrile (AIBN) were used as radical initiators. By varying temperature, time, and monomer concentrations in grafting reactions, the optimum conditions for both initiator systems were fixed. The graft yield for the AN–BPO system was higher than that for the AN–AIBN system. The optimum conditions of reactions were at temperatures of 70 and 60°C with initiator concentrations of 0.4% (0.36 mmol) and 2% (1.24 mmol) for the AN–AIBN and AN–BPO systems, respectively, at a monomer concentration of 5% (14.1 mmol) solution. The number of grafts per cellulose chain was in the range from 2.2 to 1.1 for AN–BPO and 0.5 to 2.1 for the AN–AIBN system. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 89: 630–637, 2003     

Syntheses and properties of graft polymers of N‐substituted acrylamides onto EPDM

The graft polymerizations of N‐isopropylacrylamide (NIPAM) or N‐phenylacrylamide (NPAM) onto ethylene‐propylene‐diene terpolymer (EPDM) were carried out with benzoyl peroxide (BPO) as an initiator in toluene or THF. The structures of synthesized graft polymers, EPDM‐g‐N‐isopropylacrylamide (ENIPAM) and EPDM‐g‐N‐phenylacrylamide (ENPAM), were identified by infrared (IR) spectroscopy. The effects of monomer concentration, reaction time, and initiator concentration were investigated on the graft polymerization. The highest graft efficiency of NIPAM was obtained at 0.75 mol/L of NIPAM, 4 g of EPDM, 3 wt % of BPO, and 70°C for 48 h and that of NPAM did not much change up to 0.75 mol/L of NPAM, 4 g of EPDM, 3 wt % of BPO, and 70°C for 72 h. The thermal decomposition temperatures, wettabilities, and tensile strengths of ENIPAM and ENPAM all decreased with an increasing concentration of NIPAM and NPAM moiety in the corresponding polymers, respectively. The morphologies of ENIPAM and ENPAM after irradiation showed many gel particles as compared with those of ENIPAM and ENPAM before irradiation. The UV light and ⁶⁰Co γ‐ray resistances of ENIPAM and ENPAM were worse than those of EPDM due to carbonyl group in NIPAM and NPAM. © 1999 John Wiley & Sons, Inc. J Appl Polym Sci 74: 3259–3267, 1999     

Influence of the initiator system on the spatial inhomogeneity in acrylamide‐based hydrogels

The effect of the initiator system used in the gel preparation on the spatial inhomogeneity in poly(acrylamide) (PAAm) and poly(N,N‐dimethylacrylamide) (PDMA) hydrogels was investigated by static light scattering and elasticity measurements. The hydrogels were prepared by free‐radical crosslinking copolymerization of the monomers acrylamide (AAm) or N,N‐dimethylacrylamide (DMA) with N,N′‐methylenebisacrylamide as a crosslinker. Two different redox‐initiator systems, ammonium persulfate (APS)–N,N,N′,N′‐tetramethylethylenediamine (TEMED) and APS–sodium metabisulfite (SPS), were used to initiate the gelation reactions. Compared to the APS–TEMED redox pair, no significant scattered light intensity rise was observed during the crosslinking polymerization reactions initiated by the APS–SPS system. It was found that both PAAm and PDMA gels are much more homogeneous when the APS–SPS redox pair was used as the initiator. The results are explained by the formation of shorter primary chains as well as the delay of the gel point in APS–SPS initiated gel formation reactions. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 103: 3228–3237, 2007     

Isothermal emulsion polymerization of n‐butyl methacrylate with KPS and redox initiators: Kinetic study at different surfactant/initiator concentrations and reaction temperature

Thermal initiators, although widely used in emulsion polymerization, are limited to high reaction temperatures due to their high activation energy. Redox initiators have low activation energies indicating that emulsion polymerization could be conducted at lower temperatures to save energy. In the present study, a redox initiator system comprised of hydrogen peroxide (H₂O₂) and ascorbic acid (AA) in conjunction with a Fe²⁺ ion catalyst is compared with a potassium persulfate (KPS) thermal initiator in an emulsion polymerization system consisting of n‐butyl methacrylate (BMA), sodium lauryl sulfate (SLS) and water. The dependence of particle number on surfactant and initiator concentrations shows that redox‐ and KPS‐initiated systems both follow the Smith‐Ewart theory. However, the high radical flux generated from the redox initiator results in the formation of much smaller latex particles and higher reaction rate with lower molecular weights. Latex particle size and molecular weight could also be influenced by reaction temperature. By using redox initiator, small monodisperse particles (diameter < 50 nm) can be achieved without using a large amount of surfactant. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 43037.     

双官能团引发剂引发甲基丙烯酸甲酯的聚合速率

研究了双官能团引发剂2,5-双(2-乙基己酰过氧化)-2,5-二甲基己烷（TX-141）引发甲基丙烯酸甲酯（MMA）的自由基聚合动力学,考察了引发剂浓度、聚合温度对聚合动力学的影响.结果表明：该体系的聚合活化能为91 kJ&#8226;mol^-1左右,计算得到TX-141引发剂的分解活化能为140 kJ&#8226;mol^-1左右,与实验值接近;TX-141引发剂的反应级数约为0.72,说明MMA聚合终止基元反应中单基和双基终止并存.同时与相似半衰期的过氧化二苯甲酰（BPO）比较,发现当TX-141引发剂浓度为BPO的1/2时,两者在各个聚合温度下的聚合动力学曲线几乎相同;但相对分子质量有明显增加,随聚合转化率增加,TX-141与BPO引发的聚合物数均分子量之比从1.2变化到1.33;由TX-141引发的聚合物低转化率时DSC曲线出现放热峰,而高转化率以及BPO引发的聚合物则没有.说明双官能团引发剂TX-141引发聚合时,在低转化率下TX-141引发剂的2个过氧键没有全部断裂,随聚合进行,断裂程度加深.     

Kinetics of the curing reaction of unsaturated polyester resins catalyzed with new initiators and a promoter

In this article, the curing of unsaturated polyester resins catalyzed with a promoter [cobalt(II) octoate] and free‐radical initiators is presented. The new initiators were formed by the oxidation process of ethyl methyl ketone or cyclohexanone with hydrogen peroxide and the mixture of solvents containing hydroxyl groups. As a reference, a typical curing system containing ethyl methyl ketone hydroperoxide (Luperox) and the promoter was used. The differential scanning calorimetry runs were performed at different heating rates. The experimental data were fitted with the empirical kinetic model. First, the kinetic parameters (activation energy, frequency factor, and reaction order) were obtained with a single reactive process and with the nth‐order reaction f(α), the nth‐order reaction f(α) with autocatalysis, and the first‐order reaction f(α) with autocatalysis. Second, two or three different reactive processes with the nth‐order reaction f(α) for each step were used. The obtained values of the activation energies for the curing of the unsaturated polyester resins with the free radical initiator–cobalt(II) salt catalytic system were in the range 40–60 kJ/mol for the polymerization initiated by the redox decomposition of the initiators and 80–90 kJ/mol for the polymerization initiated by the thermal decomposition of the initiators at high temperatures. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 102: 1870–1876, 2006     

Kinetic study of the polymerization of ethyl acrylate in an aqueous nitric acid medium

A kinetic study of the aqueous polymerization of ethyl acrylate (EA) was carried out at 30°C in a dilute nitric acid medium with ammonium ceric nitrate (ACN)–n‐propanol (nPA) and ACN–ethanol as redox initiator systems. The ceric‐ion consumption was first‐order with respect to the ceric‐ion concentration with both initiator systems. The formation of complexes between Ce(IV) and reducing agents was observed. The orders with respect to the Ce(IV), reducing agents, and monomer were evaluated for aqueous polymerizations of EA initiated by Ce(IV)–nPA and Ce(IV)–ethanol redox initiator systems. The overall activation energy for the aqueous polymerization of EA was evaluated in the temperature region of 27–40°C with both initiator systems. A kinetic mechanism for the aqueous polymerization of EA initiated by redox initiator systems is presented. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 99: 218–224, 2006     

Modification of polypropylene through intercrosslinking graft copolymerization of poly(vinyl alcohol): Synthesis and characterization

Modification of polypropylene (PP) has been successfully carried out through intercrosslinking of poly(vinyl alcohol) (PVA), by chemical graft copolymerization method using benzoyl peroxide (BPO) as radical initiator. Prior to grafting, PP was irradiated by gamma rays at a constant dose rate of 3.40 kGy/h to introduce hydroperoxide groups. Optimum conditions pertaining to maximum percentage of grafting were evaluated as a function of different reaction parameters. Maximum percentage ofgrafting of PVA (75%) was obtained at [BPO] = 5.51 × 10^?2 mol/L in 120 min at 70°C using 15 mL of water. Characterization of pristine PP and PP‐g‐PVA was carried out by FTIR, thermogravimetric analysis, and scanning electron micrography. Swelling studies were carried out in pure, binary, ternary, and quaternary solvent systems comprising of water, ethanol (EtOH), dimethylsulfoxide (DMSO) and N, N‐dimethylformamide (DMF) in different ratios. Maximum swelling values of PP‐g‐PVA (both composite and true graft) was observed in pure DMSO followed by DMF, EtOH, and water and it was also higher than that observed in mixed solvent system. Water retention studies of pristine PP and PP‐g‐PVA (both composite and true graft) were investigated at different time periods, temperature, and pH. Maximum % water retention of PP‐g‐PVA (composite) (108%) was observed in 8 h at 50°C in neutral medium (pH = 7). © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Study on a novel N-functionalized multilithium initiator and its application for preparing star-shaped N-functionalized styrene-butadiene rubber

A novel N-functionalized multilithium (N-M-Li) initiator was synthesized from divinylbenzene (DVB) and lithiohexamethyleneimine (LHMI), and its microstructure and molecular weight distribution were characterized by ¹H-NMR and GPC, respectively. Reaction kinetics of synthesis of N-M-Li was also studied and the apparent propagation rate constants of different monomers in this reaction were obtained. Star-shaped N-functionalized styrene-butadiene rubber (SBR) was prepared by anionic polymerization using N-M-Li as initiator, N,N,N′,N′-tetramethylethylenediamine (TMEDA) as polar additive, and cyclohexane as solvent. The molecular weight distribution of the target product was measured by GPC and the result showed that it contained a certain amount of star-shaped polymers. Three types of SBR were initiated by N-M-Li, LHMI, and n-BuLi, respectively, and then were contrasted in terms of the loss factor (tan δ) by DMA, which demonstrated that N-M-Li initiator could provide rubbers with improved hysteresis characteristics. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Formation of poly(octadecyl acrylate) brushes on a silicon wafer surface

To introduce an ultrahydrophobic polymeric phase onto a silicon wafer, an initiator‐modified silicon wafer was prepared with 2‐bromopropionyl bromide and then surface‐initiated atom transfer radical polymerization of octadecyl acrylate was carried out from the initiator‐grafted silicon wafer using CuBr and N,N,N′,N″‐pentamethyldiethylenetriamine as catalyst precursors. The resultant poly(octadecyl acrylate) [poly(ODA)] brushes were characterized by ellipsometry, X‐ray photoelectron spectroscopy, grazing angle Fourier transform infrared spectroscopy, atomic force microscopy, gel permeation chromatography and water contact angle measurements. Wettability of the poly(ODA) brushes was found to depend on the surface coverage (Γ) and the root mean square roughness. The most hydrophobic surface (Γ = 25.35 mg m^?2 and root mean square roughness 11.9 nm) exhibited a water contact angle of 171.1 ± 0.2°. Copyright © 2011 Society of Chemical Industry     

Starch‐grafted polypropylene: Synthesis and characterization

Graft copolymerization of starch has been carried out onto preirradiated polypropylene (PP) in an aqueous medium using benzoyl peroxide (BPO) as the radical initiator. The maximum percentage of grafting (115%) of starch onto PP was obtained at optimum conditions of BPO concentration, 1.239 × 10⁻³ moles; temperature, 65°C; in 120 min. using 30 mL of water. Swelling studies were carried out in pure, binary, ternary and quaternary solvent systems comprising of water, ethanol (EtOH), dimethylsulphoxide (DMSO), and N,N‐dimethylformamide (DMF) in different ratios. Maximum swelling is observed in DMSO and DMF, followed by EtOH and least in water for true graft. Water retention studies of pristine PP and PP‐g‐Starch (both composite and true graft) were investigated at different time periods, temperature and pH. The composite contains grafted PP, unreacted starch and unreacted PP whereas true graft is the product from which both unreacted polymers have been removed. Maximum % water retention of PP‐g‐Starch (composite) (110%) was observed in 8 h at 50°C in neutral medium (pH = 7). The graft copolymers were characterized by FTIR, DTG, DTA, TGA, and SEM. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Inverse emulsion free‐radical polymerization of acrylamide terpolymer for enhanced oil recovery application in harsh reservoir conditions

A free‐radical inverse emulsion polymerization formulation has been developed for preparation of acrylamide (AAm)/sodium 2‐acrylamido‐2‐methylpropanesulfonate (AMPSNa)/N‐vinylpyrrolidone (VP) terpolymers. An aqueous solution of a blend of monomers is emulsified in n‐decane using Tween 85 (Tw85). Ammonium persulfate (APS) and dicumyl peroxide (DCP) were used as initiators for water and oil phases, respectively. The reactions were catalyzed by temperature and by a redox pair; the former is achieved at 60°C and the latter by adding tetramethylethylenediamine (TEMED) and sodium bisulphite (BisNa) to activate the initiator in water and oil phase, respectively. The emulsion type, stability, conversion, and rate of polymerization were analyzed. The obtained terpolymer was characterized by elemental analysis, infrared spectroscopy (FTIR), ¹³C nuclear magnetic resonance (NMR), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), gel permeation chromatography (GPC), and rheology. Thermal catalyzed emulsion polymerization initiated with DCP showed the best performance as viscosity control agent and as polymeric precursor for in situ gel forming, for water mobility control and flow diversification, respectively. Both application for enhanced oil recovery purposes in harsh oil reservoir conditions are presented. POLYM. ENG. SCI., 57:1214–1223, 2017. © 2017 Society of Plastics Engineers     

Microstructure and glass‐transition temperature of novel star N‐SIBR

In this study, a polymeric N‐functionalized mutilithium (N‐M‐Li) compound was prepared from commercial divinylbenzene (DVB) and lithiohexamethyleneimine (LHMI), and star‐shaped copoly(styrene–butadiene–isoprene) was obtained by anionic polymerization using preformed N‐M‐Li as initiator, tetramethylethlenediamine (TMEDA) as polar modifier, and cyclohexane as solvent. The microstructure and the glass–transition temperature (Tg) of copolymers were characterized by ¹H NMR and differential scanning calorimetry (DSC), respectively. It showed that the non‐1,4‐structure content and the Tg of copolymers increased with the increase of TMEDA dosage or the decrease of polymerization temperature; however, the effects of the initiator concentration and DVB dosage on them were not obvious. We also obtained the relationships between the non‐1,4‐structure content of copolymers and the Tg of copolymers respectively, and between the ln(T/Li) (TMEDA/N‐M‐Li, mole ratio) and the non‐1,4‐structure content of copolymers, as follows: Tg (°C) = 0.6258C_{non 1,4}?55.93 and C_{non 1,4} = 20.79 ln K+59.11, where K is T/Li value. Therefore on the basis of experimental results, we realize polymer design according to our practical requirements. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 102: 5848–5853, 2006     

Synthesis and swelling properties of the copolymer of acrylamide with anionic monomers

A series of novel superabsorbent copolymers of acrylamide (AM), sodium allylsulfonate (SAS), sodium acrylate (AA), and N,N′-methylenebisacrylamide (BisA) were synthesized using potassium persulfate (KPS)/N,N,N′,N′-tertramethylethylenediamine (TMEDA) as the initiator. The influences of synthetic variables (monomer concentration, temperature, initiator concentration, and pH) on the polymerization conversion (y°) and swelling properties were studied in detail. These gels should have potential application as water super-absorbents. © 1996 John Wiley & Sons, Inc.     

Synthesis of tercopolymer BA–MMA–VTES and surface modification of nano‐size Si3N4 with this macromolecular coupling agent

A new macromolecular coupling agent butyl acrylate (BA)‐methyl methacrylate (MMA)‐vinyl triethoxy silane (VTES) tercopolymer was synthesized using solution polymerization initiated by free radical initiator benzoyl peroxide (BPO) and dicumyl peroxide (DCP). Dodecylthiol is choosed as the chain transfer to control the molecule weight of this tercopolymer. The terpolymer's molecular structure was confirmed by FTIR and NMR, and its average molecular weight was determined by GPC. In this work, the tercopolymer BA–MMA–VTES is used for surface modification of silicon nitride (Si₃N₄) nanopowder. The structure surface properties and thermal stability of modified nano‐Si₃N₄ were systematically investigated by FTIR, TGA, TEM, and size distribution analyzer. The results show that the macromolecular coupling agent bonds covalently on the surface of nano‐sized Si₃N₄ particles and an organic coating layer is formed. The optimum loading of this macromolecular coupling agent BA–MMA–VTES tercopolymer is 5% (wt %) of nano‐sized Si₃N₄. TEM also reveals that modified nano‐Si₃N₄ possesses good dispersibility. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

Synthesis and characterization of dextrin‐grafted polypropylene

We carried out the graft copolymerization of the water‐soluble natural polymer dextrin onto preirradiated polypropylene (PP) in an aqueous medium using benzoyl peroxide (BPO) as the radical initiator. PP was irradiated by γ rays from a Co⁶⁰ source at a constant dose rate of 3.40 kGy/h to introduce hydroperoxide linkages, which served as the sites for grafting. The graft copolymerization was studied as a function of different reaction parameters, and the maximum percentage grafting (P_g; 55%) of dextrin onto PP was obtained at optimum conditions of [BPO] = 5.165 × 10⁻² mol/L, temperature = 60°C in 120 min with 15 mL of water. Different grafting parameters, such as the percentage apparent grafting, percentage grafting, and percentage true grafting have been evaluated. The graft copolymers were characterized by Fourier transform infrared spectroscopy, thermogravimetric analysis, and scanning electron microscopy. Swelling studies were carried out in pure, binary, ternary, and quaternary solvent systems composed of water, ethanol (EtOH), dimethyl sulfoxide (DMSO), and N,N‐dimethylformamide (DMF) at different ratios. The maximum swelling percentage PP‐g‐dextrin (both composite and true graft) was observed in pure DMSO and DMF followed by EtOH and water. Water‐retention studies of PP and PP‐g‐dextrin (both composite and true graft) were investigated at different time periods, temperatures, and pH values. The maximum percentage water retention of PP‐g‐dextrin (composite, 124%) was observed at 8 h and 50°C in a neutral medium (pH 7). © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Graft copolymerization of styrene and acrylonitrile onto EPDM

Acrylonitrile–EPDM–styrene (AES) graft copolymers were synthesized by solution graft polymerization of styrene (St) and acrylonitrile (AN) onto EPDM in an n‐hexane/benzene solvent with benzoyl peroxide (BPO) as an initiator. The structure changes were studied by an FTIR spectrophotometer. The grafting parameters were calculated gravimetrically. The influence of the polymerization conditions, such as the reaction time, concentration of the initiator, EPDM content, and weight ratio of St/AN, on the structure of the products was investigated. It was found that a proper initiator concentration and EPDM content will give a high grafting ratio of the AES resin. The thermal property of the copolymer was studied using programmed thermogravimetric analysis (TGA). The results showed that the copolymer has a better heat‐resistant property than that of ABS, especially for the initial decomposition temperature (T_in) and the maximum weight loss rate temperature (T_max). Also, the mechanism of the graft reaction was discussed. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 86: 428–432, 2002     

A study toward the physicochemical properties of graft copolymer (partially carboxymethylated guar gum‐g‐N,N′‐dimethylacrylamide): Synthesis and characterization

Unreported graft copolymer of N,N′‐dimethylacrylamide (DMA) with partially carboxymethylated guar gum (CmgOH) has been synthesized and the reaction conditions have been optimized for affording maximum grafting using a potassium peroxymonosulphate (PMS)/thiourea (TU) redox initiators under nitrogen atmosphere. The study of graft copolymerization has been performed to observe maximum value of grafting parameters except percentage of homopolymer by varying the concentrations of DMA, PMS, and TU. The grafting parameters increase continuously on increasing the concentration of DMA from 8 × 10^?2 to 24 × 10^?2 mol dm^?3, PMS from 5 × 10^?3 to 21 × 10^?3 mol dm^?3, and TU from 1.6 × 10^?3 to 4.8 × 10^?3 mol dm^?3. The optimum temperature and time for grafting of DMA onto CmgOH were found to be 35°C and 120 min, respectively. The water‐swelling capacity of graft copolymer is investigated. Flocculation property for both coking and noncoking coals is studied for the treatment of coal mine waste water. The graft copolymer is characterized by Fourier transform infrared spectroscopy and thermogravimetric analysis. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010