Synthesis and characterization of ethyl methacrylate‐acrylamide copolymers

Abstract

SYNOPSISFree radical copolymerization of ethyl methacrylate (EMA) and acrylamide ( AA) was carried out in the presence of 2,2'-azobisisobutyronitrile ( AIBN ) in dimethyl formamide (DMF) at 60°C. The percentage composition of the copolymers were established by elemental analysis. The copolymerization reactivity ratios were determined by both FinemanRoss (F-R) and Kelen-Tudos (K-T) methods. The copolymers were characterized by IR, 'H-NMR, thermal, and dielectric studies. Glass transition temperatures ( Tg) have been determined by DSC. The solubility parameter of this copolymer was evaluated by studying the intrinsic viscosity in different solvents. I NTRO DUCT10 NAcrylic copolymers have acquired prime importance in various avenues of industrial application^.'-^ They serve as basic materials for the preparation of formulations that are used as base and top coats in leather industry. Saini et al.4 studied the free radical copolymerization of acrylamide ( AA ) -methyl methacrylate and AA-styrene. Copolymerization of acrylamide with styreneY5 n -butyl acrylate, acrylic acid,7 methyl vinyl ketone,' acrylo nitrile,g and methacrylic acid" were also studied by various workers in the past few years. In our earlier paper, l1 we determined the reactivity ratios of methacrylamide with ethyl methacrylate (EMA) . In the present investigation, reactivity ratios, thermal electrical properties, and solubility parameters of EMA-AA copolymer systems are studied. EXPERIMENTALEthyl methacrylate (Fluka) was purified from inhibitor by washing with 5% sodium hydroxide in water, and dried over calcium chloride and distilled twice under reduced pressure. Acrylamide was crys- tallized from chloroform. 2,2'-Azobisisobutyronitrile ( AIBN) (Fluka) was crystallized from methanol. N,N-Dimethyl formamide (DMF) (Qualigens) was reagent grade product and was dried and purified by distillation before use.All experiments were performed in glass tubes filled with dry monomers, solvents, and initiator. The tubes were then sealed in a nitrogen atmosphere and introduced into the thermostat at desired temperature. The reaction was allowed to go for less than 10% conversion, the reactions were stopped by adding excess volume of water as nonsolvent, and the copolymers were precipitated, washed thoroughly with ether and hexane to remove DMF and unreacted monomer. Reprecipitation was done from acetone solution. The total concentration was kept constant at (1.6 mol/L monomers). The initiator was used at 0.6 g/L solvent.The IR spectra of the copolymers were recorded with Perkin-Elmer model spectrophotometer.'H-NMR spectra were recorded from CDC13 solution using a EM-360 60 MHz spectrometer. The glass transition temperatures, Tg , of the copolymers were determined by differential scanning calorimetry (DSC) at a heating rate of 8OC/min. Thermogravimetric analysis (TGA) was carried out using a Dupont 900 thermobalance in air at a heating rate of 8"C/min.The integral procedural decomposition temperature (IPDT)12 values were determined from a 1521

Nanospheres and nanocapsules of amphiphilic copolymers constituted by methoxypolyethylene glycol cyanoacrylate and hexadecyl cyanoacrylate units

“…Particles, spontaneously formed in the mixer chamber, were evacuated by the outlet jet, and then quenched in 25 mL of water under magnetic stirring. Finally, the acetone was evaporated in Valente et al -eXPRESS Polymer Letters Vol.7, No.1 (2013) [2][3][4][5][6][7][8][9][10][11][12][13][14][15][16][17][18][19][20] a rotating device (30 minutes at room temperature) to obtain an aqueous suspension of nanospheres. Nanocapsules were prepared by the same procedure after adding 200 #L of Miglyol 812 (i.e.…”

“…Amphiphilic molecules of cyanoacrylate have also been widely studied as drug delivery systems. These compounds are now prepared mainly by radical copolymerization reactions in monophasic organic solvents like dimethyl formamide or butanone [6,7], or in two-phase solvents where the monomers dissolve each in one of the two phases [8][9][10]. Another method of preparation of cyanoacrylate amphiphilic copolymers is based on the condensation reaction of methoxy polyethylene glycol cyanoacetate and hexadecyl cyanoacetate with formaldehyde in the presence of an organic solvent like methylamine [11].…”

Compositional Sequence Determination of Acrylamide/Alkyl Acrylate Copolymers by NMR Spectroscopy

“…The 13 C NMR spectra were recorded on a Bruker 300 MHz spectrometer in dimethyl sulfoxide (DMSO)-d 6 at room temperature using tetramethylsilane (TMS) as the internal standard reference. A 2 s relaxation delay was used for 13 C NMR spectra recording.…”

Environmentally‐Friendly Acrylates‐Based Polymer Latices

“…Literature concerned with the free radical polymerization of acrylic resin has been reported by many workers in the fi eld [5][6][7][8]. Th e relative ease of polymerization and the wide range of properties among the acrylic resins have led to the commercial production of many diff erent resins suitable for a broad variety of applications [9].…”