In this work, a hydrogel system was produced via radical polymerization of N,N-dimethylacrylamide and 2-acrylamido-2-methylpropanesulfonic acid in the presence of N,N-methylene-bis-acrylamide as a crosslinker and ammonium persulfate as an initiator. Parameters that impact the conversion of copolymerization (such as initial concentration of monomers, temperature, initiator dose, and time) were studied. The swelling degree of the hydrogel was investigated with the addition of a crosslinker and initiator at different pH levels. A hydrogel with high conversion and high swelling degree was selected to investigate their ability for adsorption of Pb(II) ions from solutions. Adsorption behavior of Pb(II) ions in a hydrogel was examined as a function of reaction time and concentration of lead ions from a solution of Pb(II) ions.
The kinetics of copolymerization is one of the key factors for optimization the process in large scale of production. Copolymerization of N, N‐dimethyl‐N,N‐diallyammonium chloride (DMDAAC) with N,N‐dimethyl acrylamide (DMAA) was studied by a dilatometer technique using ammonium persulfate ([NH4]2S2O8) as an initiator. The effect of the parameters (including molar ratio of DMDAAC to DMAA, concentrations of monomers [M] and initiator [I], and the temperature) on the polymerization rate was analyzed. From these analyses it was found that the polymerization rate (Rp) with the above variables can be represented as the following relationship: Rp∝ [M]2.63; Rp∝ [I]0.40 andRp∝[MDMDAAC:MDMAA]‐0,86.The negative order found in the relationship of the reaction rate and the monomer composition indicated that the DMDAAC concentration in the monomers composition conversely affected the polymerization rate. The overall activation energy for the polymerization rate was 39.56 kJ/mol in the temperature range between 40°C and 60°C. Based on the experimental results, the mechanism of polymerization is discussed in detail. Different thermal properties for DMDAAC and DMDAAC‐DMAA were observed by differential scanning calorimetry (DSC), and thermogravimetry (TG) analysis. Addition of DMAA to DMDAAC lowered the thermal stability relative to the home polymer of DMDAAC.
A detailed synthetic procedure based on the use of urea, dichlorophthalic acid, respective transition metal halides and [NH4]2[MoO4] as a catalyst in the melt or by using 1,2,4-trichlorobenzene as a high-boiling inert solvent is described to gain 2,3,9,10,16,17,23,24-metallooctachlorophthalocyanines (MPcCl8 compounds with M=Mn, Fe, Co, Ni, Cu). In cases that a first purification by subsequent treatment of the crude materials with HCl, NaOH and HCl would not give rise to analytically pure compounds, a second novel purification by using pyridine is described. The degree of purity, exceeding always 98%, is determined by thermogravimetric analysis. Comparative IR, UV/Vis and PXRD studies of the MPcCl8 compounds are reported.
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