4.4 Thermochemische Reststoffbehandlung und Wertstoffrückgewinnung
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- 4.4 Thermochemische Reststoffbehandlung und Wertstoffrückgewinnung (106) (entfernen)
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In the near future, phosphorus (P) recycling will gain importance in terms of decreasing primary resources. Sewage sludge (SSL) is an adequate secondary P-resource for P-fertilizer production but it is also a sink for heavy metals and organic pollutants. The present study is an investigation on thermochemical P-recycling of SSL. Various temperatures and amendments were tested regarding their performance to remove heavy metals and polycyclic aromatic hydrocarbons (PAH) and simultaneous increase of the plant-availability of P. The investigations were carried out on two types of SSL originating from wastewater treatment plants with chemical P-precipitation and enhanced biological P-removal, respectively. The results show that thermochemical treatment with chlorine donors is suitable to remove the majority of heavy metals and that a combination of a gaseous chlorine donor (HCl) and sodium additives leads to both high heavy metal removal and high plant availability of P. Furthermore, plant experiments Show that almost all investigated thermochemical treatments can significantly reduce the bioavailability and plant uptake of heavy metals. Furthermore, PAHs are secondarily formed during low-temperature treatments (400–500 ° ), but can be significantly reduced by using sodium carbonate as an additive.
An environmentally friendly and cost efficient way for the management of municipal solid waste incineration (MSWI) fly ash represents its thermal co-treatment together with combustible waste. However, the safe introduction and storage of MSWI fly ash in the waste bunker is challenging and associated with severe problems (e.g. dust emissions, generation of undefined lumps and heat in case of moistened MSWI fly ash). Therefore, the aim of this study is to investigate the suitability of pelletisation as a pretreatment of MSWI fly ash. In particular, MSWI fly ash was characterised after sampling, pelletisation and thermal treatment and the transfer of constituents to secondary fly ash and flue gas was investigated. For this purpose, MSWI fly ash pellets with a water content of about 0.15 kg/kg and a diameter of about 8 mm have been produced by disc pelletiser and treated in an electrically heated pilot-scale rotary kiln at different temperatures, ranging from 450°C to 1050°C. The total contents of selected elements in the MSWI fly ash before and after thermal treatment and in the generated secondary fly ash have been analysed in order to understand the fate of each element. Furthermore, leachable contents of selected elements and total content of persistent organic pollutants of the thermally treated MSWI fly ash were determined. Due to the low total content of Hg (0.7 mg/kg) and the low leachate content of Pb (<0.36 mg/kg), even at the lowest treatment temperature of 450°C, thermally treated MSWI fly ash pellets can be classified as nonhazardous waste. However, temperatures of at least 650°C are necessary to decrease the toxic equivalency of PCDD/F and DL-PCB. The removal of toxic heavy metals like Cd and Pb is significantly improved at temperatures of 850°C, 950°C or even 1050°C. The observed metal removal led to relatively high contents of e.g. Cu (up to 11,000 mg/kg), Pb (up to 91,000 mg/kg) and Zn (up to 21,000 mg/kg) in the secondary fly ash. This metal enriched secondary fly ash might represent a potential raw material for metal recovery (e.g. via acidic leaching). Due to the high content of total dissolved solids observed in the leachate of thermally treated MSWI fly ash pellets, a wet extraction procedure is suggested to enable its safe disposal at non-hazardous waste landfills.
Tantalum and niobium are essential for the development of electronics towards a more and more compact design, but without reducing their performance today. Especially in smart phones and tablets, tantalum and niobium capacitors with high charge densities have already become almost indispensable. However, tantalum as a critical raw material is still a problem for the sustainable production of electronics. Due to this fact, the existence of efficient recycling processes especially in Europe is becoming even more important nowadays.
The Bundesanstalt für Materialforschung und -prüfung (BAM) is currently working on the optimisation of an existing pyrometallurgical tantalum recycling process. Optimisation of this industrial process is carried out in a small-scale electric arc furnace (480 kVA, capacity approx. 150 kg/h) at BAM using a new and innovative equipment for on-line analysis of high temperature processes.
The aim of this project is to identify the best timing for an optimum slag tapping, when the slag is lower than minimum targeted tantalum concentration. Hence, LIBS (Laser induced breakdown spectroscopy) is used to identify the chemical composition of the slag layer and during slag tapping. The on-line-LIBS prototype of BAM enables an in-situ measurement of the element distribution in the melt after calibration on the slag system.
First results of this joint research project will be presented including on-line-LIBS-measurements and thermodynamic and kinetic aspects of the process.
Wastewater contains a diverse array of organic and inorganic compounds and its complex composition strongly depends on the location and the connected dischargers. However, municipal wastewater as a carrier of feces and urine generally contains considerable amounts of the main nutrients nitrogen and phosphorus. The latter is in the focus of the discussions about the recovery potential of wastewater due to the relatively high mass flows of phosphorus in wastewater and the finite nature and decreasing quality of phosphate rock reserves. But due to the presence of the whole periodic table of elements, wastewater might contain further valuable components of interest for recovery including those defined as critical raw materials by the European Commission. Phosphorus and most of the other critical raw materials are fixed in the sewage sludge and after incineration in the sewage sludge ash (SSA). This is accompanied by high concentration factors from wastewater via sludge to ash. However, the mass fractions of the majority of elements in sewage sludge are comparable to those of the earth crust, indicating no relative enrichment. Nevertheless, enrichment factors of 100 or higher are given for phosphorus, copper, zinc, cadmium, silver, tin, lead and the platinum group elements indicating an anthropogenic input. An economic value of sewage sludge was estimated to $460,-/t calculated on the basis of the respective market prices for high purity elements – a theoretical value. A German survey of sewage sludge ashes showed that the mass fractions and the mass flows of most of the elements present in SSA are probably too low for an economic recovery. In most cases the mass flows are rather small compared to the imports and the chemical forms are not suitable for recovery. An exception is phosphorus that is present in high mass fractions up to 13% and that bears a high substitution potential. If the application of P-recovery technologies lead to a further concentration of valuable elements e.g. as by-products in side streams of the process, it would probably make also the recovery of other elements of economic interest.
During the last decades the material composition of buildings has become increasingly diverse. However, largely sorted material flows are needed for generating high quality secondary building materials. The use of secondary building materials can meet the requirements of sustainability in several ways: the extended time availability of primary raw materials and, thereby, the preservation of natural resources as well as the conservation of landfill sites.
Recycling of gypsum (calcium sulfate) can be a good example for the environmental benefits of closed-loop recycling. The content of sulfates in other secondary building materials, in particular in recycled concrete aggregates, should be minimized for quality reasons. In contrast, separated gypsum can also be used in gypsum production if the high quality requirements for the recycled gypsum are met. Since almost all processing steps in the recycling process are associated with environmental impacts, an environmental evaluation of the use of recycled gypsum as a substitute in gypsum production has to be carefully conducted.
This paper focusses on the techniques for generating recycled gypsum from gypsum plasterboards, the related quality requirements and a comprehensive environmental evaluation of the complete process.
The present study shows the potential of high-resolution imaging and nano-Fourier-transform infrared (nano-FTIR) spectroscopy for corrosion science. The protective oxidation layers of different chlorine-gas treated silicon
carbides (SiCs) were characterized with these techniques. A nitrified SiC showed the highest resistant strength against chlorine corrosion at 1000 °C compared to the other SiCs. Nano-FTIR spectroscopy with a lateral resolution below 40 nm detected differences in the crystallinity of the bulk-SiC and in the transitional region to the protective layer. Furthermore, high-resolution imaging provides deep insight in the interfacial layer between bulk-SiC and the protective oxidation layer on sub-micrometer scale.
A pot experiment was carried out with maize to determine the phosphorus (P) plant-availability of different secondary P-fertilizers derived from wastewater. We analyzed the respective soils by P K-edge X-ray absorption near-edge structure (XANES) spectroscopy to determine the P chemical forms that were present and determine the transformation processes. Macro- and micro-XANES spectroscopy were used to determine the chemical state of the overall soil P and identify P compounds in P-rich spots. Mainly organic P and/or P adsorbed on organic matter or other substrates were detected in unfertilized and fertilized soils. In addition, there were indications for the formation of ammonium phosphates in some fertilized soils. However, this effect was not seen in the maize yield of all P-fertilizers. The observed reactions between phosphate from secondary P-fertilizers and cofertilized nitrogen compounds should be further investigated. Formation of highly plant-available compounds such as ammonium phosphates could make secondary P-fertilizers more competitive to commercial phosphate rock-based fertilizers with positive effects on resources conservation.
The challenge of the project ASHES is focused on the recycling of nutrients from residues of thermochemical processing of by-products of sugar cane industry (bagasse/straw) in Brazil to increase the energy efficiency of thermal conversion and to enable the recycling of process ashes as fertilisers. Dry lignocellulosic biomass (straw, bagasse) are combusted, gasified and subsequently combined with post-thermochemical treatment in the AshDec process to increase the plant availability of phosphorus. Different fertilizer formulations are granulated/pelletized and tested regarding their storage/handling characteristics.
A new sewage sludge ordinance was set in force in Germany in 2017 that makes phosphorus recovery from sewage sludge mandatory. The technological possibilities for P-recovery from waste water, sewage sludge and sewage sludge ash were presented.
Tantalum and niobium are essential for the development of electronics towards a more and more compact design, but without reducing their performance today. Especially in smart phones and tablets, tantalum and niobium capacitors with high charge densities have already become almost indispensable. However, tantalum as a critical raw material is still a problem for the sustainable production of electronics. Due to this fact, the existence of efficient recycling processes especially in Europe is becoming even more important nowadays.
The Bundesanstalt für Materialforschung und -prüfung (BAM) is currently working on the optimisation of an existing pyrometallurgical tantalum recycling process. Optimisation of this industrial process is carried out in a small-scale electric arc furnace (480 kVA, capacity approx. 150 kg/h) at BAM using a new and innovative equipment for on-line analysis of high temperature processes.
The aim of this project is to identify the best timing for an optimum slag tapping, when the slag is lower than minimum targeted tantalum concentration. Hence, LIBS (Laser induced breakdown spectroscopy) is used to identify the chemical composition of the slag layer and during slag tapping. The on-line-LIBS prototype of BAM enables an in-situ measurement of the element distribution in the melt after calibration on the slag system.
First results of this joint research project will be presented including LIBS-measurements and thermodynamic and kinetic aspects of the process.
A wide range of methods are used to estimate the plant-availability of soil phosphorus (P). Published research has shown that the diffusive gradients in thin films (DGT) technique has a superior correlation to plant-available P in soils compared to standard chemical extraction tests. In order to identify the plant-available soil P species, we combined DGT with infrared and P K- and L-edge X-ray adsorption near-edge structure (XANES) spectroscopy. This was achieved by spectroscopically investigating the dried binding layer of DGT devices after soil deployment. All three spectroscopic methods were able to distinguish between different kinds of phosphates (poly-, trimeta-, pyro- and orthophosphate) on the DGT binding layer. However, infrared spectroscopy was most sensitive to distinguish between different types of adsorbed inorganic and organic phosphates. Additionally, also intermediates of the time-resolved hydrolysis of trimetaphosphate in soil could be analyzed. Furthermore, infrared and XANES microspectroscopy make it also possible to analyze P compounds on the binding layer with a lateral resolution down to 1 µm2. Therefore, P species of a spatial soil segment (e.g. rhizosphere) can be mapped and analyzed.
The SCALE Project is a Horizon2020 Project (GA°730105) that aims to develope a secure supply chain for Scandium in Europe. To achieve that, the whole value chain is investigated and new methodologies and techniques are being developed. In BAM we are characterizing potential Scandium-bearing industrial by-products.
Phosphorus (P) plays an essential role in the global food security. However, the global P reservoirs have a statistic lifetime of about 385 years only. Due to the scarcity of P and the increasing world population an efficient and sustainable recycling management is required. A few biogenic waste materials are high in P contents such as sewage sludge and meat and bone meal. Thus, they are suitable for P recycling and fertilizer production. But besides the high P content sewage sludge is often highly contaminated with organic pollutants and toxic heavy metals which have to be eliminated before agricultural field application. In this presentation we show the potential of sewage sludge as secondary resource for fertilizers. This includes our developments in thermochemical processes for the production of novel P-fertilizers from recycled materials. Furthermore, for these novel P-fertilizers common extraction tests to determine the plant-available P are often unusable. Therefore, we successfully applied the Diffusive gradients in thin-films (DGT) techniques to analyse the plant-availability of P-fertilizers from recycled materials.
Jährlich entstehen in Brasilien ca. 2 bis 10 Millionen Tonnen Aschen aus der Verbrennung von Zuckerrohrbagasse. Die Aschen enthalten schwankende Zusammensetzungen an mineralischen Nährelementen und könnten daher zu Düngezwecken verwendet werden.
Allerdings ist (i) die Nährstoffverfügbarkeit gering, (ii), die entsprechende Nährstoffzusammensetzung nicht optimal für die Nutzung der Aschen als Düngemittel für die Hauptanbaukulturen in Brasilien und (iii) weisen die Aschen aufgrund häufig schlechter Verbrennungsqualitäten hohe organische Kohlenstoffgehalte auf. Im Rahmen des Forschungsprojekts ASHES („Rückführung von Nährstoffen aus Aschen von thermochemischen Prozessen mit Bagasse bzw. Zuckerrohrstroh“), arbeiten 7 deutsche und 4 brasilianische Partner an der Optimierung der thermochemischen Verwertung von Rückständen aus der Zuckerproduktion in Brasilien, inklusive der Formulierung von optimierten Düngemischungen auf Basis der generierten Aschen. In dieser Veröffentlichung wird die Verarbeitung dieser optimierten Mischungen zu Pellets und Granulaten unter Verwendung verfügbarer regionaler Reststoffe wie Filterkuchen (Vinasse-Presskuchen) sowie Hühnertrockenkot beschrieben. Zur Untersuchung der Handlingeigenschaften wurden die produzierten Pellets und Granulate hinsichtlich ihrer mechanischen Stabilität und des Wasseraufnahmevermögens untersucht. Dafür wurden geeignete Prüfverfahren angepasst und entsprechende Versuche durchgeführt.
Small-scale variations in mineral chemistry, textures, and platinum group element (PGE) mineralization were investigated in the Lower and Middle Group chromitite layers LG6, LG6a, MG1, MG2, and MG2 II from vertical drill core profiles at the Thaba mine in the northwestern limb of the Bushveld Complex. We present detailed geochemical profiles of chromite composition and chromite crystal size distribution curves to shed light on the processes of chromite accumulation and textural modification as well as mineralization. Multiple samples within each layer were assayed for PGE concentrations, and the respective platinum group mineral association was determined by mineral liberation analysis (MLA).
There is strong evidence for postcumulus changes in the chromitites. The crystal size distribution curves suggest that the primary chromite texture was coarsened by a combination of adcumulus growth and textural equilibration, while compaction of the crystal mush played only a minor role. Mineral compositions were also modified by postcumulus processes, but because of the very high modal amount of chromite and its local preservation in orthopyroxene oikocrysts, that phase retained much primary information. Vertical variations of chromite composition within chromitite layers and from one layer to another do not support the idea of chromite accumulation from crystal-rich slurries or crystal settling from a large magma chamber. Instead, we favor a successive buildup of chromitite layers by repeated injections of relatively thin layers of chromite-saturated magmas, with in situ crystallization occurring at the crystal mush-magma interface. The adcumulus growth of chromite grains to form massive chromitite required addition of Cr to the layers, which we attribute to downward percolation from the overlying magma.
The PGE concentrations are elevated in all chromitite layers compared to adjacent silicate rocks and show a systematic increase upward from LG6 (avg 807 ppb Ir + Ru + Rh + Pt + Pd + Au) to MG2 II (avg 2,062 ppb).
There are also significant internal variations in all layers, with enrichments at hanging and/or footwalls. The enriched nature of chromitites in PGEs compared to host pyroxenites is a General feature, independent of the layer thickness. The MLA results distinguish two principal groups of PGE mineral associations: the LG6, LG6, and MG1 are dominated by the malanite series, laurite, and PGE sulfarsenides, while the MG2 and MG2 II layers are characterized by laurite and PGE sulfides as well as Pt-Fe-Sn and PGE-Sb-Bi-Pb alloys. Differences in the PGE associations are attributed to postcumulus alteration of the MG2 and MG2 II layer, while the chromitites below, particularly LG6 and LG6a, contain a more pristine association.
The use of secondary building materials can meet the requirements of sustainability in several ways: the extended time availability of primary raw materials and, thereby, the protection of natural ressources as well as the conservation of landfill sites. Regarding the predicted decrease of gypsum supply in Germany, particularly the recycling of gypsum (calcium sulfate) is of growing importance. Currently, the gypsum demand is fulfilled (at least 60%) by gypsum as side product from coal-fired power plants (FGD Gypsum). Germany’s natural gypsum deposits fulfil the remaining gypsum demand. Due to national climate protection goals the gypsum supply from coal power plants will decrease significantly in the future.
In addition, the content of sulfates in other secondary building materials, in particular in recycled concrete aggregates, should be minimized for quality reasons. Separated gypsum can be used in gypsum production if the high quality requirements for recycled gypsum are met. Accordingly, there have been significant advancements in the processing of gypsum residues in the last years. Since almost all processing steps in the recycling process are associated with environmental impacts, an evironmental evaluation of the use of recycled gypsum as a substitute in gypsum production has to be carefully conducted.
The presentation focusses on the techniques for generating recycled gypsum from gypsum plaster boards, the related quality requirements and a comprehensive environmental evaluation of the complete process.
Specific co-fertilization of nutrients can enhance their plant-availability and thus the yield of plants. To investigate this effect, we performed a pot experiment with three different P-fertilizers and ammonium nitrate sulfate as a co-fertilizer, without and with a nitrification inhibitor (NI), and analyzed the form of nitrogen (N) in the soil via novel X-ray spectroscopic method. The application of NI with the N fertilizer led to a higher dry matter yield of maize. Novel N K-edge micro-X-ray absorption near-edge structure (micro-XANES) spectroscopy identified that the application of a NI promotes the temporary formation of a non-exchangeable N in detectable hot-spots in the soil. The subsequent slow release and prolonged availability of N during plant growth leads to higher yield. It can be concluded that NIs lead to a temporary fixation of ammonium-N in a pool that can be accessed by plant roots. Those types of available nutrient pools meet the idea of so-called “next generation fertilizers” as plants have access to nutrients according to their current demand.
Tricalcium-silicate (C3S) or Alite is the most important mineral in Portland cement. Since pure tricalcium-silicate is only stable above temperatures of 1250 °C, its decomposition has to be prevented technically by fast cooling after the sintering process. At room temperature, the decomposition velocity is very slow so that metastable tricalcium-silicate is obtained.
Although the mechanisms of clinker phase formation during burning process of Portland cement in a rotary kiln were solved and improved over the years, in view of possible economic and ecological benefits current projects aim to produce clinker phases from metallurgical slags. Recent studies discovered that the mineral phase which remained after a reducing treatment and separation of formed metallic iron from molten Linz-Donawitz (LD-) slags contained about 60 wt.% Alite despite it was cooled slowly. Because the results could be verified using slags from different origins and varying cooling velocities a chemical stabilisation of the Alite can be assumed. First tests in mortars indicate that workability, hardening and solid state properties are comparable with an ordinary Portland cement. An application of the observed phenomenon in cement production requires enhanced knowledge about formation and stabilisation conditions of Alite during crystallisation from melts in contrast to the sintering reactions in conventional Portland cement production. Therefore, this study focuses on the stabilisation mechanisms of Alite in consolidating melts. Samples from different melting experiments are analysed to determine stabilising factors.