Browsing by Author "Sasia, Pedro M."
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Item Semicontinuous copolymerization of 80/20 wt % [2-(acryloyloxy)ethyl] trimethyl ammonium chloride/acrylamide in an inverse microemulsion at high comonomer concentrations(2009-12-01) Ochoa-Gómez, José R.; Escudero-Sanz, Francisco J.; Sasia, Pedro M.; Río, Francisca; Nieto-Mestre, Javier; Torrecilla, Jesús; Katime, Issa A.; Tecnalia Research & Innovation; VALORIZACIÓN DE RESIDUOS; SGThe semicontinuous inverse microemulsion copolymerization of 80/20 wt % [2-(acryloyloxy)ethyl]trimethylammonium chloride/acrylamide in an isoparaffin solvent at high comonomer concentrations (30-42 wt %) was studied with a mixture of nonionic surfactants (Crill 43 and Softanol 90) as the emulsifier and sodium metabisulfite as the initiator. The influence of the total comonomer concentration (TCC), emulsifier concentration (EC), hydrophilic-lipophilic balance (HLB), isopropyl alcohol (chaintransfer agent) concentration (IPC), and crosslinking agent concentration (CAC) on the weight-average molar mass (M w), absolute viscosity (BV), and viscometric structuring index (VSI) of the obtained copolymers was analyzed. Mw and BV increased with TCC and HLB and decreased with EC. At the higher TCC, Mw decreased with IPC; meanwhile, at the lower TCC, Mw increased with IPC above 0.5 wt %. VSI increased with TCC, HLB, and IPC and decreased with EC. VSI increased dramatically with CAC, whereas BV showed a peak at the CAC of 10 ppm. In the absence of both chain-transfer and crosslinking agents, Mw increased linearly with VSI, and this suggests that linear copolymers of very high M w values cannot be obtained by inverse microemulsion copolymerization, at least for high TCCs. The results are explained in terms of both the collapsed state of the copolymer chains inside the latex particles and changes in the interface structure and composition.Item Stability of inverse microemulsions of acrylamide-based anionic flocculants: Evidence about the need of unsaturated surfactants(2008-02-20) Ochoa G, José R.; Marta Muñoz, H.; Reinoso, Diego; Sasia, Pedro M.; Escudero, Francisco J.; Río, Francisca; Mestre, Javier Nieto; Torrecilla, Jesús; ECONOMÍA CIRCULAR; VALORIZACIÓN DE RESIDUOS; SGInfluence of surfactant structural characteristics on stability of inverse microemulsions of acrylamide-based anionic flocculants (40% (w/w) sodium acrylate and 60% (w/w) acrylamide, based on total amount of comonomers) has been studied by using 17 surfactant blends consisting of two non ionic surfactants with different length of hydrophobic chains, different number of hydrophobic chains per molecule, and with and without double bonds on their hydrophobic chains. Experimental evidence shows that unsaturated emulsifiers are needed for obtaining stable inverse microemulsions of acrylamide-based anionic flocculants and that presence of double bonds on the hydrophobic tails of a surfactant is its major structural characteristic to stabilize this kind of polymeric inverse microemulsions (PIM).Item Synthesis of cationic flocculants based on acrylamide and [2-(acryloyloxy)ethyl]trimethylammonium chloride co polymers by semicontinuous inverse microemulsion co polymerization. Part I: Criteria for selection of comonomer formulation(2006-06-01) Ochoa, G. José R.; Río, Francisca; Sasia, Pedro M.; Katime, Issa A.; Escudero, Francisco Javier; Díaz De Apodaca, Elena; Mestre, Javier Nieto; ECONOMÍA CIRCULAR; Alimentación Sostenible; VALORIZACIÓN DE RESIDUOSThe influence of surfactant blend composition, organic solvent (oil) structure and cationic charge density (CCD) on stability of comonomer inverse microemulsions of acrylamide and [2-(acryloyloxy)ethyl]trimethylammonium chloride has been studied in order to obtain criteria for selecting comonomer inverse microemulsions before copolymerization resulting in copolymer inverse microemulsion useful as flocculants. Results show that optimum HLB can be explained by cohesive energy ratio theory and it increases with CCD; the higher the hydrophobic chain length of surfactants in surfactant blend, the lower the minimum surfactant blend concentrations (SBCm) needed to obtain stable inverse microemulsions; and linear organic solvents allow a decrease of the SBCm required for stabilizing comonomer inverse microemulsions.Item Synthesis of cationic flocculants based on acrylamide and [2-(acryloyloxy)ethyl]trimethylammonium chloride copolymers by semicontinuous inverse microemulsion polymerization. Part II: Influence of initiator addition conditions, initial temperature, pH and comonomer concentration on flocculating performance(2006-07-14) Sasia, Pedro M.; Ochoa G., José R.; Río, Francisca; Escudero, Francisco J.; De Apodaca, Elena Díaz; Nieto, Javier; Torrecilla, Jesús; Katime, Issa; ECONOMÍA CIRCULAR; Alimentación Sostenible; VALORIZACIÓN DE RESIDUOS; SGThe influence of initiator concentration, specific flow rate of initiator addition (Qsp), initial copolymerization temperature (Ti), aqueous phase pH and total comonomer concentration (TCC) on flocculating performance of latex particles of acrylamide and [2-(acryloyloxy)ethyl]trimethylammonium chloride copolymers with a cationic charge density of 40%, obtained by inverse microemulsion copolymerization by using a surfactant blend of Arlacel 83 and Softanol 90 as emulsifier and Rolling M-245, a mixture of n-decane and n-tetradecane in about 40/60 weight ratio, as oil phase, has been studied for high TCC, ranging from 28 to 34.5% (w/w). Comonomer inverse microemulsion copolymerizations were carried out in the semicontinuous mode by adding continuously an aqueous solution of sodium metabisulfite as initiator into stirred inverse comonomer microemulsions. Initiator concentration has a strong influence on viscosity, viscometric structuring degree (VSI) and average weight molar mass (Mw) of copolymers in the range from 5 to 25 g/L. Both viscosity and Mw decrease with increasing initiator concentration. Best flocculating performance is obtained from 10 to 20 g/L, values at which VSI shows a minimum. Under the experimental conditions used, Qsp (153 to 310 mL/h/kg of comonomer), Ti (25 to 35°C) and aqueous phase pM (2.5 to 4.5) have almost no influence on both viscosity and VSI and, hence, on flocculating performance. On the contrary, ICC has a slight influence on copolymer viscosity but a strong one on VSI which increases dramatically with TCC, being the worst flocculating performance obtained at the highest TCC studied (34.5% (w/w)). Flocculating performance results are explained in terms of copolymer structuring degree and collapsed state of copolymer chains inside latex particles as well as in terms of the composition drift with conversion.Item Synthesis of cationic flocculants based on acrylamide and [2-(acryloyloxy)ethyl]trimethylammonium chloride copolymers by semicontinuous inverse microemulsion polymerization. Part III: Influence of HLB and surfactant blend concentration on flocculating performance(2007-05-31) Rio, Francisca; Ochoa, José R.G.; Sasia, Pedro M.; Escudero, Francisco J.; De Apodaca, Elena Díaz; Nieto, Javier; Katime, Issa; ECONOMÍA CIRCULAR; Alimentación Sostenible; VALORIZACIÓN DE RESIDUOSThe influence of HLB (hydrophilic-lipophilic balance) and surfactant blend concentration (SBC) on flocculating performance of latex particles of acrylamide and [2-(acryloyloxy)ethyl]trimethylammonium chloride copolymers with a cationic charge density of 40%, obtained by inverse microemulsion copolymerization by using a surfactant blend of Arlacel 83 and Softanol 90 as emulsifier and Rolling M-245, a mixture of n-decane and n-tetradecane in about 40/60 weight ratio, as oil phase, has been studied for a total comonomer concentration of 32.5% (w/w). Comonomer inverse microemulsion copolymerizations were carried out in the semicontinuous mode by adding continuously an aqueous solution of sodium metabisulflte (SMB) as initiator into stirred inverse comonomer microemulsions. From 7.75 to 8.26, HLB has a strong influence on average molar mass (M w) and flocculating performance (FP), the higher the HLB the higher the FP. A small decrease in SBC causes a dramatic increase in Mw, and a decrease in FP although the influence on copolymer viscosity is small. Results are explained in terms of copolymer structuring degree and collapsed state of copolymer chains inside latex particles as well as in terms of the observed composition drift with conversion.