| 1. |
- Nordberg, Åke, et al.
(författare)
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Selective desorption of carbon dioxide from sewage sludge for in-situ methane enrichment : Enrichment experiments in pilot scale
- 2012
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Ingår i: Biomass and Bioenergy. - : Elsevier BV. - 0961-9534 .- 1873-2909. ; 37, s. 196-204
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Tidskriftsartikel (refereegranskat)abstract
- The application of in-situ methane enrichment for upgrading the biogas from anaerobic digestion to vehicle fuel or natural gas quality, has been studied in pilot scale and by computer simulation of the desorption step. Pilot plant experiments have been performed using a 19 m(3) and 15 m(3) continuously stirred tank reactor operating with municipal sewage sludge at mesophilic conditions connected respectively to a 90 dm(3) and 140 dm(3) external bubble column for selective desorption of CO2. The results show that the CH4 yield is unchanged during the experiments, and accordingly there is no evidence that the oxygen in the air used in the desorption of CO2 has a negative impact on the CH4 producing activity. The sludge recirculation system must be designed to avoid leakage of air into the digester, in order to maintain a low N-2 concentration in the biogas. At best, a biogas with a volume fraction of 87% CH4 and (p N-2 = 2% was obtained. The CH4 loss however amounted to 8%, which is unsatisfactory. The experimental results are compared with previous data in the literature and explanations are deducted for the difference in the performance. Computer simulations reveal that the sludge flow rate recirculated through the desorption column should be as low as possible to minimize the loss of CH4. An increased air flow rate through the desorption column and an increased desorption column volume will promote the desorption of CO2 and improve the ratio of CO2 to CH4 desorption.
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| 2. |
- Albero Caro, Jesus, et al.
(författare)
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Semibatch reaction crystallization of salicylic acid
- 2014
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Ingår i: Chemical engineering research & design. - : Elsevier BV. - 0263-8762 .- 1744-3563. ; 92:3, s. 522-533
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Tidskriftsartikel (refereegranskat)abstract
- Reaction crystallization of salicylic acid has been investigated by experiments and modeling. In the experimental work, dilute hydrochloric acid has been added to an agitated aqueous solution of sodium salicylate in 1 L scale, and product crystals have been characterized by image analysis. The results show that the product crystal number mean size at first increases with increasing agitation rate but then gradually decreases again at further increase in stirring rate. At lower stirring rate, larger crystals are obtained when the feeding point is located close to the agitator instead of being located out in the bulk solution. The mean crystal size increases with decreasing feeding rate and with decreasing reactant concentrations. There is a decrease in mean size with increasing feed pipe diameter. These trends in the experimental results show great similarity with previous results on benzoic acid. The experimental results have been examined by a population balance model accounting for meso and micro mixing, and crystal nucleation and growth rate dispersion. It is found that the crystallization kinetic parameter estimation is quite complex, and the objective function hyper surface contains many different minima. Hence, parameter estimation has to rely on a combination of mathematical optimization strategies and a scientific understanding of the physical meaning of the parameters and their relation to current theories. As opposed to our previous work on benzoic acid, it has not been possible to find a set of kinetic parameters that provides for a good description of all experimental data.
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| 3. |
- Bäbler, Matthäus U., et al.
(författare)
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Isolation of Pharmaceutical Intermediates through Solid Supported Evaporation. Semicontinuous Operation Mode
- 2012
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Ingår i: Industrial & Engineering Chemistry Research. - : American Chemical Society (ACS). - 0888-5885 .- 1520-5045. ; 51:45, s. 14814-14823
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Tidskriftsartikel (refereegranskat)abstract
- Solid supported evaporation (SSE) is a simple, nonselective method for isolating nonvolatile compounds from a solution. The solution is put in contact with porous polymer beads onto which the compound deposits upon evaporation of the solvent. This brings some advantages over direct evaporation to dryness in terms of safety, thermal decomposition, and solid handling, as the loaded beads form a free flowing granular material that is easily recovered. In this paper, SSE in a semicontinuous operating mode is investigated where the solution is continuously fed to (respectively sprayed over) an agitated bed of dry beads put under vacuum. It is found that under conditions where the solvent evaporation fate is high with respect to the feed rate, high bead loadings can be achieved before extensive sticking of beads and compound to the vessel walls occurs. The type of compound and solvent had little influence on the process performance, and, in cases where this was explored, the bead loading was found to be homogeneous. Based on a balance equation for the solvent fed to the system, a model is developed that results in a simple scale up criterion. The latter was successfully applied for transferring SSE from lab to the kilo lab scale.
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| 4. |
- Croker, D. M., et al.
(författare)
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Isothermal suspension conversion as a route to cocrystal production : One-pot scalable synthesis
- 2014
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Ingår i: Organic Process Research & Development. - : American Chemical Society (ACS). - 1083-6160 .- 1520-586X. ; 18:8, s. 941-946
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Tidskriftsartikel (refereegranskat)abstract
- Isothermal suspension conversion is presented as a suitable method for the manufacture of pure cocrystal products once the ternary phase diagram (TPD) for the cocrystal system in the desired solvent is available. One:one and 3:2 cocrystals of p-toluenesulphonamide/triphenylphosphine oxide were produced in acetonitrile and dichloromethane using this method. Eight individual batches of product were prepared with complete conversion to pure product achieved in seven batches. Product recovery (77-99%), reaction conversion (17-89%), and volumetric productivity (0.03-0.63 g/cm(3)) were calculated for each product batch. These parameters are essentially determined by the batch operating mass fraction composition selected from the TPD, allowing for tailoring of processing conditions to suit process requirements and capabilities by careful selection of the optimum operating mass fraction composition.
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| 5. |
- Croker, D. M., et al.
(författare)
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Nucleation in the p-toluenesulfonamide/triphenylphosphine oxide co-crystal system
- 2013
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Ingår i: Crystal Growth & Design. - : American Chemical Society (ACS). - 1528-7483 .- 1528-7505. ; 13:8, s. 3754-3762
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Tidskriftsartikel (refereegranskat)abstract
- Nucleation has been studied in pure co-crystal and mixed co-crystal phase regions of the ternary phase diagram (TPD) in acetonitrile at 20 C using cooling crystallization experiments. Direct nucleation of each of the co-crystal phases in this system was independently observed in regions of the TPD where each is stable. In mixed regions, regions where either a co-crystal and a coformer, or both co-crystals, are stable, the phase that initially nucleated was a function of the mass composition in that region. The relative amount of each phase nucleating could be controlled by adjusting the relative mass fraction of each component. The kinetic return to equilibrium was also observed as the systems were held over time, with the selected mass fractions always returning to the equilibrium dictated by the TPD after 24 h
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| 6. |
- Croker, D. M., et al.
(författare)
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Solution mediated phase transformations between co-crystals
- 2013
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Ingår i: CrystEngComm. - : Royal Society of Chemistry. - 1466-8033. ; 15:11, s. 2044-2047
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Tidskriftsartikel (refereegranskat)abstract
- A solution mediated transformation between two co-crystal phases has been observed for the p-toluensulfonamide-triphenylphosphine oxide co-crystal system. This system has two known co-crystals with 1 : 1 and 3 : 2 stoichiometry respectively, and the ternary phase diagram (TPD) for the system has been determined in acetonitrile previously. By manipulating the solution composition in this solvent to a region of the TPD where the 1 : 1 co-crystal is stable, the 3 : 2 co-crystal could be observed to convert to the 1 : 1 co-crystal. The corresponding transformation was true for the 1 : 1 co-crystal in a region of the TPD where the 3 : 2 co-crystal is stable; the 1 : 1 co-crystal converted to the 3 : 2 co-crystal.
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| 7. |
- Croker, Denise, et al.
(författare)
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Understanding the p-toluenesulfonamide / triphenylphosphine oxide crystal chemistry: a new 1:1 cocrystal and ternary phase diagram
- 2012
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Ingår i: Crystal Growth & Design. - : American Chemical Society (ACS). - 1528-7483 .- 1528-7505. ; 12:2, s. 869-875
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Tidskriftsartikel (refereegranskat)abstract
- A novel 1:1 cocrystal between p-toluenesulfonamide and triphenylphosphine oxide has been prepared and structurally characterized. This 1:1 cocrystal was observed to form during solid state grinding experiments, with subsequent formation of a known 3:2 cocrystal in the presence of excess sulfonamide. Both cocrystals are stable in the solid state. The ternary phase diagram for the two coformers was constructed in two different solvents: acetonitrile and dichloromethane. Examination of these diagrams clarified solution crystallization of both the newly discovered 1:1 cocrystal and the previously reported 3:2 cocrystal, and identified regions of stability for each cocrystal in each solvent. The choice of solvent was found to have a significant effect on the position of the solid state regions within a cocrystal system.
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| 8. |
- Forsberg, Kerstin, et al.
(författare)
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Crystallization of metal fluoride hydrates from mixed hydrofluoric and nitric acid solutions, Part I : Iron (III) and Chromium (III)
- 2010
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Ingår i: Journal of Crystal Growth. - : Elsevier BV. - 0022-0248 .- 1873-5002. ; 312:16-17, s. 2351-2357
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Tidskriftsartikel (refereegranskat)abstract
- Crystallization from hydrofluoric acid/nitric acid solutions supersaturated with Fe(III) and Cr(III) has been investigated. Iron and chromium crystallizes into a solid solution in the form of Cr(Fe)F-3 center dot 3H(2)O, which is isostructural with CrF3 center dot 3H(2)O and alpha-FeF3 center dot 3H(2)O. By seeded isothermal desupersaturation experiments, the growth rate of beta-FeF3 center dot 3H(2)O crystals at 50 degrees C has been studied in hydrofluoric acid and nitric acid solutions containing Cr(III). It is found that the growth rate of beta-FeF3 center dot 3H(2)O is essentially uninfluenced by the presence of 5 g/kg Cr(III). At 50 degrees C and a supersaturation ratio of 2 (c(FeF3)(free)/c(s)(FeF3)(free)), the growth rate is (0.8-2.2) x 10(-11) m/s in 3 mol/(kg solution) HFfree and 3 mol/(kg solution) HNO3.
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| 9. |
- Forsberg, Kerstin, et al.
(författare)
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Crystallization of metal fluoride hydrates from mixed hydrofluoric and nitric acid solutions, part II : Iron (III) and nickel (II)
- 2010
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Ingår i: Journal of Crystal Growth. - : Elsevier BV. - 0022-0248 .- 1873-5002. ; 312:16-17, s. 2358-2362
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Tidskriftsartikel (refereegranskat)abstract
- Crystallization of nickel fluoride hydrate from mixed pickle acid and the influence of Ni(II) on growth rate of beta-FeF3 center dot 3H(2)O have been studied. Iron and nickel crystallize into an unidentified Fe/Ni fluoride hydrate crystal having the overall mol ratio of Ni, Fe, and F equal to 1:2:8, which is in accordance with the number of fluoride ions needed to balance the positive charges of Ni and Fe. The most probable empirical formula of this material is (FeF3)(2)NiF2(H2O)(6-10). By seeded isothermal desupersaturation experiments, growth rate of beta-FeF3 center dot 3H(2)O crystals at 50 degrees C has been studied in a hydrofluoric acid and nitric acid solution containing Ni(II). It is found that the growth rate of beta-FeF3 center dot 3H(2)O is essentially uninfluenced by the presence of 4 g/kg Ni(II).
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| 10. |
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