Synthesis and characterization of novel polyaspartimides derived from 2,2′‐dimethyl‐4,4′‐bis(4‐maleimidophenoxy)biphenyl and various diamines

A novel bismaleimide, 2,2′‐dimethyl‐4,4′‐bis(4‐maleimidophenoxy)biphenyl, containing noncoplanar 2,2′‐dimethylbiphenylene and flexible ether units in the polymer backbone was synthesized from 2,2′‐dimethyl‐4,4′‐bis(4‐aminophenoxy)biphenyl with maleic anhydride. The bismaleimide was reacted with 11 diamines using m‐cresol as a solvent and glacial acetic acid as a catalyst to produce novel polyaspartimides. Polymers were identified by elemental analysis and infrared spectroscopy, and characterized by solubility test, X‐ray diffraction, and thermal analysis (differential scanning calorimetry and thermogravimetric analysis). The inherent viscosities of the polymers varied from 0.22 to 0.48 dL g⁻¹ in concentration of 1.0 g dL⁻¹ of N,N‐dimethylformamide. All polymers are soluble in N‐methyl‐2‐pyrrolidone, N,N‐dimethylacetamide, N,N‐dimethylformamide, dimethylsulfoxide, pyridine, m‐cresol, and tetrahydrofuran. The polymers, except PASI‐4, had moderate glass transition temperature in the range of 188°–226°C and good thermo‐oxidative stability, losing 10% mass in the range of 375°–426°C in air and 357°–415°C in nitrogen. © 1999 John Wiley & Sons, Inc. J Appl Polym Sci 73: 279–286, 1999     

Fabrication of a poly(N‐vinyl‐2‐pyrrolidone) modified macroporous polypropylene membrane via one‐pot reversible‐addition fragmentation chain‐transfer polymerization and click chemistry

In this study, a macroporous polypropylene membrane (MPPM) was grafted with hydrophilic poly(N‐vinyl‐2‐pyrrolidone) (PNVP) based on a one‐pot reversible‐addition fragmentation chain transfer (RAFT) polymerization and click chemistry. First, we prepared the clickable membrane by bromination and following S_N2 nucleophilic substitution reaction; then, click chemistry and RAFT polymerization were performed in one‐pot to graft PNVP to the MPPM surface. The surface characterizations, including attenuated total reflectance/Fourier transform infrared spectroscopy, X‐ray photoelectron spectroscopy, and field‐emission scanning electron microscopy, illustrated that PNVP was really grafted onto the MPPM surface. The permeation and antifouling characteristics of the MPPMs were measured by the filtration of a bovine serum albumin dispersion; this showed that in contrast to the nascent membrane, the grafted membrane efficiently obstructed protein molecules because of the compactly grafted polymer chains. The hydrophilicity and antifouling properties of MPPM were greatly ameliorated after modification. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42649.     

Investigation of molecular structure of LDPE modified by itaconic acid grafting

Using thermomechanical spectroscopy, the molecular‐weight distribution and relaxation transitions have been investigated in commercial LDPE and grafted by itaconic acid (LDPE‐g‐IA). This grafting in the molten LDPE was done by reactive extrusion with varied content of reactants in the blend under alternating of a shearing rate applied onto the melt. The dependence of structural relaxation changes in LDPE is shown upon the depth of the mechanochemical transformations and the competing reactions at IA grafting, and also on the chemical crosslinking of the macromolecules. The reason for MWD bimodality for LDPE‐g‐IA obtained in dynamic mixing is the raised homogenization degree of the reactive blend and the higher grafted product yield compared with static mixers. The mixer type substantially affects the structure of the LDPE‐g‐IA amorphous phase. The data obtained reflect chemical transformations of LDPE molecules in IA's presence without an initiator of radical reactions (DCP). Most probable is the IA initiation of molecular crosslinking reactions. There could also occur IA thermodegradation and oligomerization. LDPE and IA or products of acid chemical transformations do not agree thermodynamically (the calculated solubility parameters are 16.1 (MJ/m³)^0.5 for polyethylene and 26.4 (MJ/m³)^0.5 for IA). From the above procedure it can be supposed that nongrafted IA (or its oligomers) exerts an antiplastifying effect on LDPE and LDPE‐g‐IA. © 1999 John Wiley & Sons, Inc. J Appl Polym Sci 71: 1771–1779, 1999     

Synthesis and properties of polyamides based on 5,5′‐bis[4‐(4‐aminophenoxy)phenyl]‐hexahydro‐4,7‐methanoindan

A new diamine 5,5′‐bis[4‐(4‐aminophenoxy)phenyl]‐hexahydro‐4,7‐methanoindan ( 3 ) was prepared through the nucleophilic displacement of 5,5′‐bis(4‐hydroxylphenyl)‐hexahydro‐4,7‐methanoindan ( 1 ) with p‐halonitrobenzene in the presence of K₂CO₃ in N,N‐dimethylformamide (DMF), followed by catalytic reduction with hydrazine and Pd/C in ethanol. A series of new polyamides were synthesized by the direct polycondensation of diamine 3 with various aromatic dicarboxylic acids. The polymers were obtained in quantitative yields with inherent viscosities of 0.76–1.02 dl g⁻¹. All the polymers were soluble in aprotic dipolar solvents such as N,N‐dimethylacetamide (DMAc) and N‐methyl‐2‐pyrrolidone (NMP), and could be solution cast into transparent, flexible and tough films. The glass transition temperatures of the polyamides were in the range 245–282 °C; their 10% weight loss temperatures were above 468 °C in nitrogen and above 465 °C in air. © 2000 Society of Chemical Industry     

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     

Effects of glycerol and PE‐g‐MA on morphology,thermal and tensile properties of LDPE and rice starch blends

The effects of glycerol and polyethylene‐grafted maleic anhydride (PE‐g‐MA) on the morphology, thermal properties, and tensile properties of low‐density polyethylene (LDPE) and rice starch blends were studied by scanning electron microscopy (SEM), differential scanning calorimetry, and the Instron Universal Testing Machine, respectively. Blends of LDPE/rice starch, LDPE/rice starch/glycerol, and LDPE/rice starch/glycerol/PE‐g‐MA with different starch contents were prepared by using a laboratory scale twin‐screw extruder. The distribution of rice starch in LDPE matrix became homogenous after the addition of glycerol. The interfacial adhesion between rice starch and LDPE was improved by the addition of PE‐g‐MA as demonstrated by SEM. The crystallization temperatures of LDPE/rice starch/glycerol blends and LDPE/rice starch/glycerol/PE‐g‐MA blends were similar to that of pure LDPE but higher than that of LDPE/rice starch blends. Both the tensile strength and the elongation at break followed the order of rice starch/LDPE/glycerol/PE‐g‐MA blends > rice starch/LDPE/glycerol > LDPE/rice starch blends. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 92: 344–350, 2004     

Compatibilizer in waste tire powder and low‐density polyethylene blends and the blends modified asphalt

With the increasing ratio of waste tire powder (WTP) to low‐density polyethylene (LDPE), the hardness and tensile strength of the WTP/LDPE blends decreased while the elongation at break increased. Five kinds of compatibilizers, such as maleic anhydride‐grafted polyethylene (PE‐g‐MA), maleic anhydride‐grafted ethylene‐octene copolymer (POE‐g‐MA), maleic anhydride‐grafted linear LDPE, maleic anhydride‐grafted ethylene vinyl‐acetate copolymer, and maleic anhydride‐grafted styrene‐ethylene‐butylene‐styrene, were incorporated to prepare WTP/LDPE blends, respectively. PE‐g‐MA and POE‐g‐MA reinforced the tensile stress and toughness of the blends. The toughness value of POE‐g‐MA incorporating blends was the highest, reached to 2032.3 MJ/m³, while that of the control was only 1402.9 MJ/m³. Therefore, POE‐g‐MA was selected as asphalt modifier. The toughness value reached to the highest level when the content of POE‐g‐MA was about 8%. Besides that the softening point of the modified asphalt would be higher than 60°C, whereas the content of WTP/LDPE blend was more than 5%, and the blends were mixed by stirring under the shearing speed of 3000 rpm for 20 min. Especially, when the blend content was 8.5%, the softening point arrived at 82°C, contributing to asphalt strength and elastic properties in a wide range of temperature. In addition, the swelling property of POE‐g‐MA/WTP/LDPE blend was better than that of the other compalibitizers, which indicated that POE‐g‐MA /WTP/LDPE blend was much compatible with asphalt. Also, the excellent compatibility would result in the good mechanical and processing properties of the modified asphalt. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Ionic liquid‐catalyzed aminolysis of poly(ethylene terephthalate) waste

Aminolytic depolymerization of poly(ethylene terephthalate) (PET) bottle waste with ethanolamine and hydrazine hydrate under atmospheric conditions was investigated in the presence of room temperature ionic liquids. 1‐Hexyl‐3‐methylimidazolium trifluoromethanesulfonate (Hmim.TfO) and 1‐butyl‐3‐methylimidazolium hydrogen sulfate (Bmim.HSO₄). (Hmim.TfO) was found to be the most efficient catalyst to obtain high yields of the aminolysis products bis(2‐hydroxy ethylene) terephthalamide and terephthalic dihydrazide using ethanolamine and hydrazine hydrate, respectively. These products were characterized by IR spectroscopy, ¹H NMR, ¹³C NMR, mass spectroscopy, and differential scanning calorimetry. The influence of experimental parameters, such as the amount of catalyst, reaction time, molar ratio of ethanolamine, and hydrazine hydrate with respect to PET was investigated. This protocol proves to be efficient and environmentally benign in terms of high yields (>84%) and low reaction times (up to 30 min). © 2012 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Synthesis and characterization of new poly(amide‐imide)s based on 1,4‐bis(trimellitimido)‐2,5‐dichlorobenzene

A series of new aromatic poly(amide‐imide)s were synthesized by the triphenyl phosphite‐activated polycondensation of the diimide‐diacid, 1,4‐bis(trimellitimido)‐2,5‐dichlorobenzene (I), with various aromatic diamines in a medium consisting of N‐methyl‐2‐pyrrolidone (NMP), pyridine, and calcium chloride. The poly(amide‐imide)s had inherent viscosities of 0.88–1.27 dL g⁻¹. The diimide‐diacid monomer (I) was prepared from 2,5‐dichloro‐p‐phenylenediamine with trimellitic anhydride. All the resulting polymers were amorphous and were readily soluble in a variety of organic solvents, including NMP and N,N‐dimethylacetamide. Transparent, flexible, and tough films of these polymers could be cast from N,N‐dimethylacetamide or NMP solutions. Cast films had tensile strengths ranging from 92 to 127 MPa, elongations at break from 4 to 24%, and initial moduli from 2.59 to 3.65 GPa. The glass transition temperatures of these polymers were in the range of 256°–317°C, and the 10% weight loss temperatures were above 430°C in nitrogen. © 1999 John Wiley & Sons, Inc. J Appl Polym Sci 73: 271–278, 1999     

Structure and properties of polyamide 6 blends with low‐density polyethylene grafted by itaconic acid and with neutralized carboxyl groups

A comparative study of the structure and properties of two‐phase blends of polyamide 6 (PA6) and low‐density polyethylene (LDPE) modified in the course of reactive extrusion, by grafting of itaconic acid (IA) without neutralization of carboxyl groups (LDPE‐g‐IA) and with neutralized carboxyl groups (LDPE‐g‐IA^?M⁺) was carried out. It was shown that 30 wt % of LDPE‐g‐IA^?M⁺ introduced to PA6 resulted in blends of higher Charpy impact strength compared with that of PA6/LDPE‐g‐IA blends. The maximum increase was achieved when Mg(OH)₂ was used as a neutralizing agent. The blend morphology has a two‐phase structure with blurred interphases because of increased adhesion between the phases. The neutralization of carboxyl groups in grafted IA did not lead to two‐phase morphology of blends, which had a negative influence on the mechanical properties. It is believed that the differences in the impact strength were caused by the influence of the added neutralizing agents on the structure of interphases, which depends on both the interfaces adhesion and structural effects resulting from the nucleating behavior of the neutralizing agent. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 92: 1702–1708, 2004     

Temperature‐responsive alginate‐g‐poly(N,N‐diethylacrylamide) copolymer: Synthesis,characterization, and swelling behavior

Temperature‐responsive polymers have recently gained importance due to their applications in drug delivery. Herein, temperature‐responsive graft copolymer (Alg‐g‐PDEAAm) of alginate and N,N‐diethylacrylamide was synthesized by microwave‐assisted copolymerization using potassium persulfate/N,N,N′,N′‐tetramethylethylenediamine initiator system. The reaction conditions for the best grafting (331%) have been optimized by changing microwave irradiation time, temperature, N,N‐diethylacrylamide, and alginate concentrations. The spectroscopic characteristic, thermal properties, and surface morphology of the copolymers were investigated by FTIR, ¹H‐NMR, DSC/TGA, XRD, gel permeation chromatography, and SEM. Furthermore, low critical solution temperatures of Alg‐g‐PDEAAm copolymers were detected by UV spectroscopy. Swelling ratio of graft microspheres was carried out at 25, 32, and 37 °C, and microspheres were found exhibiting temperature‐responsive property. Cytotoxicity test indicated the Alg‐g‐PDEAAm copolymer and its microsphere were biocompatible. Therefore, based on the results the synthesized temperature‐responsive copolymer could be considered as a promising biomaterial. © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2018 , 135, 46688.     

Poly(styrene‐co‐N‐butylmaleimide) macroinitiators by controlled autopolymerization and related block copolymers

Autopolymerization of styrene‐N‐butylmaleimide mixtures at 125 or 140°C in the presence of a stable nitroxyl radical [2,2,6,6‐tetramethylpiperidin‐1‐yloxyl (TEMPO)] was found to proceed in a pseudoliving manner. Unimolecular initiators, which were originated by trapping self‐generated radical species with TEMPO, took part in the process. Under the studied experimental conditions, the TEMPO‐controlled autopolymerization with a varying comonomer ratio provided virtually alternating copolymers of narrow molecular weight distributions. The molecular weights of the copolymers increased with conversions. The obtained styrene‐N‐butylmaleimide copolymers containing TEMPO end groups were used to initiate the polymerization of styrene. The polymerization yielded poly(styrene‐co‐N‐butylmaleimide)‐polystyrene block copolymers with various polystyrene chain lengths and narrow molecular weight distributions. The compositions, molecular weights, and molecular weight distributions of the synthesized block copolymers and the initial poly(styrene‐co‐N‐butylmaleimide) precursors were evaluated using nitrogen analysis, gel permeation chromatography, and ¹H‐ and ¹³C‐NMR spectroscopy. © 1999 John Wiley & Sons, Inc. J Appl Polym Sci 74: 2378–2385, 1999     

Chemorheological study of compatibilized blends of low‐density polyethylene and polydimethyl siloxane rubber

Compatibilization of the blends of polydimethyl siloxane (PDMS) rubber and low‐density polyethylene (LDPE) was achieved through reactive processing during extrusion in a Monsanto Processability Tester (MPT). The chemorheological characteristics of 50 : 50 LDPE : PDMS blends with varying proportions (0–8 wt %) of ethylene comethyl acrylate (EMA) were investigated at three different temperatures (170, 190, and 210°C) and four different shear rates (61.3, 122.6, 306.6, and 613.1 s^?1). It was found that EMA reacts with vinyl groups of PDMS rubber at a temperature of 190°C during extrusion through the capillary of MPT, forming EMA‐grafted‐PDMS rubber (EMA‐g‐PDMS), which acts as the compatibilizer for the blend systems. The results are based on IR spectroscopy, melt rheology, and phase morphology of the blends. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 12: 2810–2817, 2003     

Thermoresponsive and biocompatible poly(vinyl alcohol)‐graft‐poly(N,N‐diethylacrylamide) copolymer: Microwave‐assisted synthesis,characterization, and swelling behavior

Novel thermoresponsive poly(vinyl alcohol)‐graft‐poly(N,N‐diethylacrylamide) (PVA‐g‐PDEAAm) copolymers were prepared by microwave‐assisted graft copolymerization using a potassium persulfate/N,N,N′,N′‐tetramethylethylenediamine (KPS/TEMED) initiator system. The structures of PVA‐g‐PDEAAm copolymers were characterized by ¹H‐NMR, Fourier transform infrared spectroscopy, differential scanning calorimetry/thermogravimetric analysis, gel permeation chromatography, X‐ray diffraction, and scanning electron microscopy. The effects of various process parameters on grafting were systematically studied: microwave power, KPS, monomer and PVA concentrations, and ultraviolet irradiation. Under optimal conditions, the maximum grafting percent and graft efficiency were 101% and 93%, respectively. Furthermore, a lower critical temperature of copolymers was measured in the range 29–31 °C by ultraviolet spectroscopy. The swelling behavior of graft membranes was carried out at various temperatures, and the results showed that the swelling behavior of membranes was dependent on the temperature. In vitro cell culture studies using L929 fibroblast cells confirmed cell compatibility with the PVA‐g‐PDEAAm copolymer and its membrane, making them an attractive candidate for drug delivery systems. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2018 , 135, 45969.     

Polystyrene composites of single‐walled carbon nanotubes‐graft‐polystyrene

Single‐walled carbon nanotubes (SWCNTs) dispersed in N‐methylpyrrolidone (NMP) were functionalized by addition of polystyryl radicals from 2,2,6,6‐tetramethyl‐1‐piperidinyloxy‐ended polystyrene (SWCNT‐g‐PS). The amount of polystyrene grafted to the nanotubes was in the range 20‐25 wt% irrespective of polystyrene number‐average molecular weight ranging from 2270 to 49 500 g mol^?1. In Raman spectra the ratios of D‐band to G‐band intensity were similar for all of the polystyrene‐grafted samples and for the starting SWCNTs. Numerous near‐infrared electronic transitions of the SWCNTs were retained after polymer grafting. Transmission electron microscopy images showed bundles of SWCNT‐g‐PS of various diameters with some of the polystyrene clumped on the bundle surfaces. Composites of SWCNT‐g‐PS in a commercial‐grade polystyrene were prepared by precipitation of mixtures of the components from NMP into water, i.e. the coagulation method of preparation. Electrical conductivities of the composites were about 10^?15 S cm^?1 and showed no percolation threshold with increasing SWCNT content. The glass transition temperature (T_g) of the composites increased at low filler loadings and remained constant with further nanotube addition irrespective of the length and number of grafted polystyrene chains. The change of heat capacity (ΔC_p) at T_g decreased with increasing amount of SWCNT‐g‐PS of 2850 g mol^?1, but ΔC_p changed very little with the amount of SWCNT‐g‐PS of higher molecular weight. The expected monotonic decrease in ΔC_p coupled with the plateau behavior of T_g suggests there is a limit to the amount that T_g of the matrix polymer can increase with increasing amount of nanotube filler. Copyright © 2012 Society of Chemical Industry     

Analysis of low‐density polyethylene‐g‐poly(vinyl chloride) copolymers formed in poly(vinyl chloride)/low‐density polyethylene melt blends with gel permeation chromatography and solid‐state 13C‐NMR

Gel permeation chromatography (GPC) and solid‐state ¹³C‐NMR techniques were used to analyze the structural changes of poly(vinyl chloride) (PVC) in blends of a low‐density polyethylene (LDPE) and PVC during melt blending. The GPC results showed that the weight‐average molecular weight (M_w) of PVC increased with LDPE content up to 13.0 wt % and then decreased at a LDPE content of 16.7 wt %, whereas the number‐average molecular weight remained unchanged for all of LDPE contents used. The ¹³C‐NMR results suggest that the increase in M_w was associated with the formation of a LDPE‐g‐PVC structure, resulting from a PVC and LDPE macroradical cross‐recombination reaction during melt blending. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 92: 3167–3172, 2004     

Synthesis and characterization of 4,5‐bis(4‐fluorobenzoyl)‐1‐methylcyclohexene and its polyethers

A new difluoride 4,5‐bis(4‐fluorobenzoyl)‐1‐methylcyclohexene (DFKK) has been prepared with fumaryl chloride, fluorobenzene, and 2‐methyl‐1,3‐butadiene as starting materials through two steps of reactions. This DFKK monomer undergoes reaction with 2,2‐(p‐hydroxyphenyl)‐iso‐propane (BPA) in the presence of excess anhydrous potassium carbonate in sulfolane to give a high molecular weight reactive poly(ether ketone ketone) (PEKK) that is very soluble in solvents such as chloroform and N,N‐dimethylformamide at room temperature, has glass transition temperature of 182°C, and is easily cast into flexible and bale ivory film with tensile strength of 64 MPa. The 5% weight loss temperature is 407°C. Ring‐closing reaction of PEKK with hydrazine gives cyclized PEKK (CPEKK) with improved thermal stability and reduced solubility. © 2002 Wiley Periodicals, Inc. J Appl Polym Sci 84: 1866–1871, 2002; DOI 10.1002/app.10454     

A Simple Copper‐Catalyzed Cascade Synthesis of 2‐Amino‐1H‐indole‐3‐carboxylate Derivatives

We have developed a simple and efficient copper‐catalyzed method for the synthesis of 2‐amino‐1H‐indole‐3‐carboxylate derivatives via cascade reactions of substituted N‐(2‐halophenyl)‐2,2,2‐trifluoroacetamide with alkyl 2‐cyanoacetate or malononitrile under mild conditions, and the method is of wide practical application.     

Synthesis and characterization of novel silver/L‐phenylalanine‐based optically active polyacrylate nanocomposite

Novel bioactive and optically active poly(N‐acryloyl‐L ‐phenylalanine) (PAPA) was synthesized by atom transfer radical polymerization. PAPA‐silver (Ag) nanocomposites have been successfully prepared via in situ reducing Ag⁺ ions anchored in the polymer chain using hydrazine hydrate as reducing agent in an aqueous medium. By controlling of the amount of Ag⁺ ions introduced, we have produced an organic/inorganic nanocomposite containing Ag nanoparticles with well controlled size. Nanocomposites were characterized by X‐ray diffraction (XRD), UV–Vis spectrophotometry, transmission electron microscopy, and Fourier transform infrared. XRD pattern showed presence of Ag nanoparticles. The PAPA/Ag nanocomposites with 1 : 10 silver nitrate (AgNO₃) : PAPA ratio revealed the presence of well‐dispersed Ag nanoparticles in the polymer matrix. All of these Ag nanoparticles formed are spherical and more than 80% of them are in the range of 15–25 nm. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Synthesis of Nano‐γ‐Ferric Oxide by Thermolysis of the 2‐Mercapto‐5‐Methylpyridine‐N‐Oxide‐Iron(III) Complex via Factorial Design

2‐Mercapto‐5‐methylpyridine‐N‐oxide (MMPNO) and its sodium salt (NaMMPNO) were synthesized. The reaction of the latter with Fe³⁺ generates Fe(MMPNO)₃ chelate. The thermolysis of this chelate at 350 °C yielded highly pure reddish‐brown γ‐Fe₂O₃ nanocrystallites with an average particle size of 6.2 nm, a particle size range of 4.2 to 14.8 nm, and a specific surface area of 51.5 m²g^–1. The thermolysis process was optimized using the 2² fractional design. Quantitative tests and characterization of products were carried out by UV‐vis spectroscopy, XRD, LLS, SEM, TGA, BET, TEM, FT‐IR, elemental microanalysis, and classical analytical measurements.