scholarly journals Process Analysis of PMMA-Based Dental Resins Residues Depolymerization: Optimization of Reaction Time and Temperature

Energies ◽  
2021 ◽  
Vol 15 (1) ◽  
pp. 91
Author(s):  
Paulo Bisi dos Santos ◽  
Haroldo Jorge da Silva Ribeiro ◽  
Armando Costa Ferreira ◽  
Caio Campos Ferreira ◽  
Lucas Pinto Bernar ◽  
...  

This work aims to optimize the recovery of methyl methacrylate (MMA) by depolymerization of polymethyl methacrylate (PMMA) dental resins fragments/residues. In order to pilot the experiments at technical scale, the PMMA dental resins scraps were submitted by thermogravimetric analysis (TG/DTG/DTA). The experiments were conducted at 345, 405, and 420 °C, atmospheric pressure, using a pilot scale reactor of 143 L. The liquid phase products obtained at 420 °C, atmospheric pressure, were subjected to fractional distillation using a pilot scale column at 105 °C. The physicochemical properties (density, kinematic viscosity, and refractive index) of reaction liquid products, obtained at 345 °C, atmospheric pressure, were determined experimentally. The compositional analysis of reaction liquid products at 345 °C, 30, 40, 50, 60, 70, 80, and 110 min, at 405 °C, 50, 70, and 130 min, and at 420 °C, 40, 50, 80, 100, 110, and 130 min were determined by GC-MS. The morphology of PMMA dental resins fragments before and after depolymerization was performed by scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDX). The experiments show that liquid phase yields were 55.50%, 48.73%, and 48.20% (wt.), at 345, 405, and 420 °C, respectively, showing a first order exponential decay behavior, decreasing with increasing temperature, while that of gas phase were 31.69%, 36.60%, and 40.13% (wt.), respectively, showing a first order exponential growth, increasing with temperature. By comparing the density, kinematic viscosity, and refractive index of pure MMA at 20 °C with those of liquid reaction products after distillation, one may compute percent errors of 1.41, 2.83, and 0.14%, respectively. SEM analysis showed that all the polymeric material was carbonized. Oxygenated compounds including esters of carboxylic acids, alcohols, ketones, and aromatics were detected by gas chromatography/mass spectrometry (GC-MS) in the liquid products at 345, 405, and 420 °C, atmosphere pressure. By the depolymerization of PMMA dental resins scraps, concentrations of methyl methacrylate between 83.454 and 98.975% (area.) were achieved. For all the depolymerization experiments, liquid phases with MMA purities above 98% (area.) were obtained between the time interval of 30 and 80 min. However, after 100 min, a sharp decline in the concentrations of methyl methacrylate in the liquid phase was observed. The optimum operating conditions to achieve high MMA concentrations, as well as elevated yields of liquid reaction products were 345 °C and 80 min.

Author(s):  
Paulo Bisi dos Santos Jr. ◽  
Haroldo Jorge da Silva Ribeiro ◽  
Armando Costa Ferreira ◽  
Caio Campos Ferreira ◽  
Lucas Pinto Bernar ◽  
...  

In this work, the cross-linked PMMA-based dental resins scraps were submitted to pyrolysis to recover MMA (Methylmethacrylate). The thermal degradation of cross-linked PMMA-based dental resins scraps was analyzed by TG/DTG to guide the operating conditions in pilot scale. The pyrolysis experiments carried out in a reactor of 143L, at 345, 405, and 420°C, 1.0 atmosphere. The reaction liquid products obtained at 345°C, physicochemical characterized for density, kinematic viscosity, and refractive index. The chemical composition of liquid products obtained at 345°C, 30, 40, 50, 60, 70, 80, and 110 minutes, at 405°C, 50, 70, and 130 minutes, and at 420°C, 40, 50, 80, 100, 110, and 130 minutes determined by GC-MS. The experiments show that liquid phase yields were 55.50%, 48.73%, and 48.20% (wt.), at 345, 405, and 420°C, respectively, showing a smooth sigmoid behavior, decreasing with increasing temperature, while that of gas phase were 31.69%, 36.60%, and 40.13% (wt.), respectively, increasing with temperature. The liquid products density, kinematic viscosity, and refractive index obtained at 30, 40, 50, 60, 70, 80, and 110 minutes, varied between 0.9227 and 0.9380 g/mL, 0.566 and 0.588 mm2/s, and 1.401 and 1.414, respectively, showing percentage deviations between 0.74 and 2.36%, 7.40 and 10.86%, and 0.00 and 0.92%, respectively, compared to standard values for density, kinematic viscosity, and refractive index of pure MMA at 20 °C. The GC-MS identified in the reaction liquid products at 345, 405, and 420°C, 1.0 atm, esters of carboxylic acids, alcohols, ketones, and aromatics, showing concentrations of MMA between 83.454 and 98.975% (area.). For all the depolymerization experiments, the concentrations of MMA in the liquid phase, between 30 and 80 minutes, reach purities above 98% (area.), decreasing drastically with increasing reaction time after 100 minutes, thus making it possible to depolymerize the cross-linked PMMA-based dental resins scraps by pyrolysis to recover MMA. The optimum operating conditions to achieve high MMA concentrations, as well as elevated yields of liquid reaction products were 345 °C and 80 minutes.


1980 ◽  
Vol 45 (10) ◽  
pp. 2728-2741 ◽  
Author(s):  
Pavel Fott ◽  
Petr Schneider

Kinetics have been studied of the reaction system taking place during the reaction of thiophene on the cobalt-molybdenum catalyst in a gradientless circulation flow reactor at 360 °C and atmospheric pressure. Butane has been found present in a small amount in the reaction products even at very low conversion. In view of this, consecutive and parallel-consecutive (triangular) reaction schemes have been proposed. In the former scheme the appearance of butane is accounted for by rate of desorption of butene being comparable with the rate of its hydrogenation. According to the latter scheme part of the butane originates from thiophene via a different route than through hydrogenation of butene. Analysis of the kinetic data has revealed that the reaction of thiophene should be considered to take place on other active sites than that of butene. Kinetic equations derived on this assumption for the consecutive and the triangular reaction schemes correlate experimental data with acceptable accuracy.


1969 ◽  
Vol 47 (22) ◽  
pp. 4175-4182 ◽  
Author(s):  
B. D. Boss ◽  
R. N. Hazlett

The 5-h oxidation of n-dodecane at 200 °C by air at 1 atm is reported for experiments in a borosilicate glass reaction chamber equipped with a gas bubbler. The rate of reaction was limited by the rate of oxygen diffusion from the gas phase due to the rapid reaction of dissolved oxygen. The reaction products were analyzed in aliquots taken periodically from the reaction chamber. Chemical analyses, gas–liquid phase chromatography (g.l.p.c.), tandem g.l.p.c.-mass spectroscopy, infrared, and ultraviolet were used to identify products accounting for 98% of the oxygen reacted. The isomer distribution of the dodecenes, dodecanols, and dodecanones formed, as well as the distribution of carboxylic acids, were determined. Three classes of intramolecular reaction products, cyclic ethers, cyclic hydrocarbons, and lactones, were detected. Many volatile products were detected. A filterable precipitate obtained after 10 h of oxidation was studied using infrared attenuated total reflectance techniques. A reaction mechanism is discussed based on current knowledge of other systems, the products identified, and the stoichiometry of the reaction.


1997 ◽  
Vol 2 (3) ◽  
Author(s):  
Michael G. MacNaughton ◽  
James R. Scott

AbstractAn engineering study was performed to evaluate the use of ultraviolet light and hydrogen peroxide to destroy caustic-neutralized VX nerve agent in the U.S. chemical agent stockpile as an alternative to incineration. Whereas caustic neutralization completely destroys VX, (3-ethyl-S-2-(diisopropylamino)ethyl methylphosphonothiolate, the reaction leaves a complex two-phase mixture containing organic phosphates and organosulfur compounds which require treatment prior to ultimate disposal. Studies performed in laboratory-scale (320-mL), bench-scale (10-L) and pilot-scale (20-L) reactors demonstrated that the principal products of the caustic neutralization-ethyl methylphosphonic acid (EMPA), methylphosphonic acid (MPA), 2-(diisopropylamino)ethyl sulfide (RSR), disulfide (RSSR) and the other mixed sulfides-could be oxidized to inorganic sulfate, phosphate, ammonia and carbon dioxide. The reaction was zero order above 1000 mg/L and pseudo first order below. To mineralize 10,000 lb of VX per day to less than 10 mg/L organic carbon would require more than 1100 lamps of 30 kW each.


2009 ◽  
Vol 130 (22) ◽  
pp. 221101 ◽  
Author(s):  
Diego Alejandro Carvajal Jara ◽  
Mateus Fontana Michelon ◽  
Alex Antonelli ◽  
Maurice de Koning

2007 ◽  
Vol 39 (12) ◽  
pp. 1290-1294 ◽  
Author(s):  
Yoshihisa Fujii ◽  
Hironori Atarashi ◽  
Norifumi Yamada ◽  
Naoya Torikai ◽  
Toshihiko Nagamura ◽  
...  

1989 ◽  
Vol 67 (5) ◽  
pp. 862-866 ◽  
Author(s):  
Guenter A. Scholz ◽  
S. Roy Morrison

The methanation reaction on MoS2 exfoliated to a thickness of a few layers or less and adsorbed onto alumina is found to be very small. However, by calcining and resulfiding the exfoliated MoS2 catalysts, greatly improved performance is achieved that is at least equal to the commercial catalysts based on ammonium heptamolybdate. The creation of molybdenum oxysulflde surface species therefore appears to be a necessary step toward producing significant methanation rates with exfoliated and supported MoS2. The methanation products are almost exclusively CO2 and CH4, their mole ratios near unity, with otherwise only very much smaller amounts of longer chain hydrocarbons. The activation energy for methanation is generally observed to be near 100 kJ/mol, with the overall reaction being first order in the carbon monoxide concentration and third order in the hydrogen concentration. In contrast to the transition-metal catalysts, no water could be detected in the reaction products of the molybdenum based catalyst. Keywords: methanation reaction on MoS2, exfoliated and supported MoS2 as catalyst.


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