KOLOMAZNIK INTERNATIONAL SYMPOSIUM (8TH INTL. SYMP. ON SUSTAINABLE MATERIALS RECYCLING PROCESSES AND PRODUCTS)

Every year, millions of tons of by-products from the metal producing industry are dumped as waste and this amount is continuously rising. As these by-products often contain considerable amounts of valuable metals, a huge quantity of potential metal resources is lost. Not only the loss of value, but also the aspect of environmental care suggests a treatment of this material as it is very often problematic in this regard. The reasons for not treating these residues are very diverse. Two main reasons are: firstly, there is no evaluation procedure available as it is for primary resources (causing little confidence and reliability for investments) and secondly, the lack of applicable technologies. A competence network involving Montanuniversität Leoben and numerous partners from industry was formed in order to treat this topic. The project consists of three areas: characterization and evaluation, process development and optimization, as well as the development of an evaluation procedure for secondary resources. The first two areas represent all steps beginning at the first characterisation of an unknown residue to the treatment in terms of mineral processing and metallurgy, process optimization and a final product and its optimization. In the third area, all of the experience gained is combined and used to develop a procedure that guarantees a serious evaluation of secondary resources. Such a procedure, as it is already in worldwide use for primary resources, will give companies and investors a reliable base for treating such materials. Until now, many different materials, such as steel mill dust, lead slag and hydrometallurgical residues from zinc production have been evaluated and treated successfully up to technical scale. The results are partly already published [1, 2]. As another case study, this paper summarizes the investigations and test results of dust from secondary copper industry. These dusts often contain considerable amounts of zinc, lead, tin and copper [3]. The main methods used are standard techniques such as scanning electron microscopy, electron microprobe analysis and X-ray fluorescence analysis. Besides the characteristics of this residues, a proposal for its metallurgical treatment will be presented as well.

The main task of the production process, where the input material is mainly secondary raw materials, is the production of products with high utility value. Secondary raw materials, often inappropriately called wastes, are characterized by non-standard properties, especially in connection with the composition and consistency, which differ significantly from control procedures, where the starting raw material has standard properties. The design of the optimal control of a recycling technology for the processing of such raw materials must be very flexible with regard to their changing properties and often also the changing quantity of the processed material. Therefore, when designing the management of recycling technologies, we must take into account the specific requirements of the processing technology, which is often not developed or is only recently designed on the basis of various requirements arising in particular from environmental protection. We therefore face two challenges – to solve a new technology and, of course, at the same time to design an automatic control system. Due to considerable concentration of industry, large-capacity units are being built, which are managed by renovated companies that supply most of the world's software. The traffic management system, including computer equipment, is in most cases delivered "turnkey" and the software is often inaccessible to the user, who does not have the opportunity to intervene in the program, change it and possibly supplement it. However, due to the constantly changing properties and composition of the secondary raw material, recycling technologies require the active cooperation of a technologist and an expert in automatic control, who can use modern means of automatic control to solve specific situations, which are often characterized by variable parameters of the controlled object. These means include, for example, intelligent sensors, powerful means of computer technology, intelligent actuators, but also modern methodologies for the design of control algorithms based on adaptive or predictive principles, often supplemented by artificial intelligence methods.
Another specific feature is the fact that most recycling technologies fall into the area of small-scale production. This is due both to the nature of specific primary technologies and to economic reasons that often do not allow the central collection of secondary raw materials. Mobile units are being built that can partially solve this economic problem. Examples of control algorithm designs include total chromium recycling from solid and liquid wastes produced in tanning, modeling of an exothermic rector for the preparation of regenerated tanning salt, and design of raw leather soak control based on a distributed parameter model.

The slaughterhouses generate a large amount of wastes - byproducts. One of them is waste fatty tissue. Fatty tissues from animals are composed of essentially three main components – water, fat and also proteins. These byproducts can be further processed and well utilized for various applications. [1, 2] It is reasonable to find appropriate utilization especially for byproducts which are not suitable or profitable for utilization in food. Waste animal fats rank among raw materials that can be used for biodiesel production and the processed protein can be used as plants biostimulant. Biodiesel, which can be used in diesel engine, is usually produced from animal fat or vegetable oil by transesterification reaction, in the presence of suitable catalyst and reactants – methanol or ethanol. [3] Protein hydrolysates represent significant category of plant biostimulants and organic nitrogen fertilizers based on a mixture of peptides and amino acids that have received increasing attention due to their positive impact on plant metabolism and crop performance. [4, 5] The goal of our work was to suggest complex processing of the animal waste fat into mentioned valuable products. The processing technology included melting of the raw fatty waste whereas water was evaporated and obtained fat was used as a feedstock for transesterification into biodiesel. The reaction conditions were set at: 1.5% w/w of TMAH as a catalyst, reaction temperature at the reaction mixture boiling point, the feedstock to methanol molar ratio of 1:6, respectively, and the reaction time 210 min. Depending on the composition of the input raw material, the processing of the protein fraction of waste fat was also verified. The raw material has been subjected to hydrolysis catalysed by proteolytic enzyme (alcalase). The final biodiesel fulfills the key requirements prescribed by European standard EN 14 214. The production of protein hydrolysate that can be used as organic nitrogen fertilizer or plant biostimulant is a suitable way of processing the protein fraction lost during fat refining, which also contributed to the overall economy of the process. The overall results served as a basis for technical and economy assessment of the waste processing.

Green chemistry started for the search of benign methods for the development of nanoparticles from nature and their use in the field of antibacterial, antioxidant, and antitumor applications. Bio wastes are eco-friendly starting materials to produce typical nanoparticles with well-defined chemical composition, size, and morphology. Cellulose, starch, chitin and chitosan are the most abundant biopolymers around the world. All are under the polysaccharides family in which cellulose is one of the important structural components of the primary cell wall of green plants. Cellulosenanoparticles(fibers, crystals and whiskers) can be extracted from agrowaste resources such as jute, coir, bamboo, pineapple leafs, coir etc. Chitin is the second most abundant biopolymer after cellulose, it is a characteristic component of the cell walls of fungi, the exoskeletons of arthropods and nanoparticles of chitin (fibers, whiskers) can be extracted from shrimp and crab shells. Chitosan is the derivative of chitin, prepared by the removal of acetyl group from chitin (Deacetylation). Starch nano particles can be extracted from tapioca and potato wastes. These nanoparticles can be converted into smart and functional biomaterials by functionalisation through chemical modifications (esterification, etherification, TEMPO oxidation, carboxylation and hydroxylation etc) due to presence of large amount of hydroxyl group on the surface. The preparation of these nanoparticles include both series of chemical as well as mechanical treatments; crushing, grinding, alkali, bleaching and acid treatments. Transmission electron microscopy (TEM), scanning electron microscopy (SEM) and atomic force microscopy (AFM) are used to investigate the morphology of nanoscale biopolymers. Fourier transform infra-red spectroscopy (FTIR) and x ray diffraction (XRD) are being used to study the functional group changes, crystallographic texture of nanoscale biopolymers respectively. Since large quantities of bio wastes are produced annually, further utilization of cellulose, starch and chitins as functionalized materials is very much desired. The cellulose, starch and chitin nano particles are currently obtained as aqueous suspensions which are used as reinforcing additives for high performance environment-friendly biodegradable polymer materials. These nanocomposites are being used as biomedical composites for drug/gene delivery, nano scaffolds in tissue engineering and cosmetic orthodontics. The reinforcing effect of these nanoparticles results from the formation of a percolating network based on hydrogen bonding forces. The incorporation of these nano particles in several bio-based polymers have been discussed. The role of nano particle dispersion, distribution, interfacial adhesion and orientation on the properties of the eco friendly bio nanocomposites have been carefully evaluated.

Biodiesel is a renewable fuel produced from vegetable oils such as rapeseed oil, sunflower oil, and soybean oil, as well as used cooking oils and animal fats [1]. Biodiesel production is, in fact, a complex process in which the glycerin that is generated as a byproduct during the production process can be used for both technical and pharmaceutical applications [2]. The availability of raw glycerin has been increasing significantly in recent years, but the demand for the product has largely remained unchanged. This excess supply and limited demand have caused the raw glycerin prices to stay low. As a result, it is important to find new applications and alternatives for the valorization of this byproduct generated from biodiesel industry [3]. Several studies have been reported aiming to transform glycerol into added-value products. However, little research has been performed on glycerol oxidation using Fenton´s oxidation process. In this work, Fenton catalyst was used to perform the oxidation of glycerol under controlled conditions of temperature, H₂O₂ flow rate addition and Fe₂SO₄/H₂O₂ ratio. Samples were taken after the addition of H₂O₂ at different intervals of time and were analyzed by High Performance Liquid Chromatography. Glyceraldehyde was quantified as the main oxidation product (32% conversion and 45% selectivity) after 70% of glycerol conversion using 0.5% H₂O₂ added at a flow rate of 5ml/min with a ratio of FeSO₄/H₂O₂ (mol/mol) between 4 and 0,33. Additional compounds detected were dihydroxyacetone, glyceric acid and glycolic acid.

The demand for the reduction of food waste in Oman has been increased during recent years. The rapid development of economic growth is throwing impact on the work-of-art of the solid waste. Food waste is generated from residential, industrial, commercial, and institutional sectors. Due to growing population and increasing consumption, the amount of solid waste is increasing. In arid region of Oman, solid waste generation was 19,100 ton/d in 2005. Generation of solid waste is expected to reach 30,000 tons/d in 2020. The high food waste content in MSW leads to its separation for use in anaerobic treatment in the available highest sources of VFA 2.89 g/l and SCOD 1980 mg/l. Biogas and methane yield were recorded to a maximum of 1.364 l/g-CODremoved.d (r=0.87), 0.912 L/g-CODremoved.d (r=0.99) and average methane content of biogas was 69%. The reactor was fully acclimatized at 55oC and achieved stability with high removal efficiency of COD, biogas production and emission reduction of CO2 of 89%. Thus, at 55oC temperature and OLR of 12.5 g-COD/L.d with 8 d HRT support a maximum biogas production of 1.37 L/g-CODremoved.d.

Strategic, critical or high-tech metals are indispensable ingredients for the development of technologically sophisticated products. Modern cars, flat-screen televisions, mobile phones, and countless other products rely on a range of materials, such as cobalt, lithium, PGM’s, tantalum, tungsten, gold, gallium and more particularly REE. This group of high-tech metals is also fundamental to new environmentally friendly products, with electric cars requiring lithium and neodymium, turbine wind with neodymium and dysprosium, high performance aluminium alloys, lighting or hard ceramics requiring scandium, and computer/mobile phones with tantalum, gold, palladium and rare earths. To meet the challenges of dwindling resources and the growth of needs, as well as in a perspective of a secure supply approach, three options are considered today based on the extraction of metals from primary resources (old mines or new deposits), from secondary resources (mining and industrial wastes) or from end of life materials (urban mine). Understanding this challenges facing strategic metals supply today requires consideration not only of the sources (whether from mines or waste streams), but of the development of eco-friendly and always more efficient processes. Here, we propose a process based on the use of ionic liquids such as N-butyl-N-ethyl-piperidinium bis(trifluoromethylsulfonyl)imide (EBPiP-NTf2), N-octyl-N-ethyl-piperidinium bis(trifluoromethylsulfonyl)imide (EOPiP-NTf2) for the extraction and the recovering of tantalum, palladium and gold initially contained in the capacitors and connectors of printed circuit boards [1-3]. The perfect extractability of ILs for Ta, Au and Pd was demonstrated and under the experimental conditions, the more promising properties have been highlighted for EOPiP-NTf2. Back extraction of Ta followed by precipitation with an ammonia solution or direct electodeposition from the loaded ionic liquid phase was also performed and showed that quantitative recovery of metals was possible, allowing thus to recover the Ta, Pd and Au, and to recycle the ionic liquid.

Waste generation is an unavoidable consequence from any industrial process. Among these wastes, the red mud, generated by the Bayer process in alumina refining, is one of the most challenging wastes in metallurgy, due to its caustic nature, combined with the vast quantities in which it is produced. Historically, the method of managing red mud is to store it in containment ponds, but this approach is far from perfect. However, economically viable commercial processes for the recovery and the reuse of it are not yet available. Industrial Ecology conceptualizes industry as a man-made ecosystem that operates in a similar way to natural ecosystems, where the waste or by product of one process is used as an input into another process. Industrial ecology interacts with natural ecosystems and attempts to move from a linear to cyclical or closed loop system. On this approach, Industrial Ecology seeks to emulate mature ecological systems in order to reduce environmental impacts through maximized efficiency of energy and resource inputs and the minimization of unutilized waste. Through these initiatives, industry has found ways to increase efficiency and turn waste into useful products. In this paper, this approach is proposed as a case study that put together a hypothetical, but typical, alumina refinery and a non-integrated ironmaking plant as the core of an industrial complex. In it, effluents of one plant are inputs to the other, leading to the total consumption of the red mud generated. Complementarily, some other selected side industries are included, and will constitute, together with the core plants, the proposed Industrial Ecology Complex.
As will be shown, the main goal is towards the zero waste generation from the Complex. It must be pointed out that the figures presented in this work are hypothetical, but coherent to those from actual plants. For that, any apparent similarity to existing plants wouldn’t be but a coincidence.

The world is increasingly turning to the use of Li-ion batteries in electric vehicles; therefore, there is a growing need for lithium (Li). I propose new method for recovering Li from used Li-ion batteries by using Li separation method by ionic conductor; LiSMIC. Li ionic conductor is functioned as a Li separation membrane. This innovative LiSMIC involves the use of an Li separation membrane whereby only Li ions in a solution of used Li-ion batteries permeate from the positive electrode side to the negative electrode side during electrodialysis; the other ions, including Co, Al, and F, do not permeate the membrane. Li0.29La0.57TiO3 (LLTO) was selected as the Li separation membrane. The positive side of the dialysis cell was filled with used Li-ion battery solution, and then the negative side was filled with distilled water. In this study, the platinum (Pt) electrodes are bonded to the right and left faces (the two main faces) of the LLTO, respectively. The applied dialysis voltage was 5 V, and the electrode area was 16 cm2 and 4 cm2 as new Li separation membrane. The Li recovery ratio increased with LiSMIC time. Furthermore, Li permeation speed was not depended on the electrode area, and I succeeded in the development of new Li separation membrane with small area electrode. After LiSMIC, the Li recovery water was bubbled by CO2 gas to produce lithium carbonate (Li2CO3) as a raw material for Li-ion batteries. The high purity Li2CO3 powder was easily generated under CO2 gas bubbling method.
Thus, LiSMIC is most suitable for the Li recycling of used Li-ion batteries.

Numerous studies indicate fair ability of water soluble polysaccharides including their blends and nanocomposites to form organized structures in solutions and gels [1]. E. g., fibrillar structure and network formation was found in aqueous solutions and gels of methylcellulose (MC) while even thermo-reversible fibrillation of MC/cellulose nanocrystal-based hydrogels was found [2]. Surprisingly, formation of these structures in rigid polysaccharides (mostly films) and their impact on mechanical performance were reported less frequently. The presented study deals with an unknown unexpected effect of 2-hydroxyethylcellulose (HEC) on structure and mechanical performance of methylcellulose (MC) films. This leads to synergistic as well as antagonistic effects [3] on mechanical performance in dependence on modifiers content and ratio. The values of modulus of MC containing 5 and 10 % HEC exceed those of the linear model, which indicates synergistic effect consisting in formation of ordered structures. At the same time, higher content of HEC leads to worse properties indicating dominant contribution of its lower parameters. In spite of absence of direct insight into the structure, combination of XRD, polarized light microscopy and rheology indicates a high effect of small content of HEC on formation of favorable ordered structures and a slight hindering effect of GO on this process. Rheological evaluation indicates ability of HEC to support formation of ordered structures in MC also in water-solution. Important result is that unlike high reinforcing effect of low graphene oxide (GO) content on single MC and HEC components, its presence in blends decreases mechanical properties as a result of disturbing of HEC-induced structural transformations. Further unexpected feature is that negative effects of higher HEC content on mechanical performance are enlarged by GO. The results confirm complex effect of blending and GO on structure and properties of the MC/HEC system.

The paper deals with selected authors' solutions of recycling technologies for the processing of industrial by-products. The presented technologies specifically include refinery hydrogenation, recycling of wastewater produced by a dairy farm and waste-free processing of solid waste from the leather and food industries [1,2,3]. Proposals of control algorithms based on economic optimization of washing processes are presented [4]. The introduced solutions are briefly supplemented by the theory of transport processes and heterogeneous reaction kinetics, which were involved in projects and industrial implementations [5,6].

This paper focused on the modeling of ecological treatment of printed circuit boards (PCB). Due to the high increase in the production of electronic waste, which contains a whole range of usable components, it is necessary to recycle it. We have proposed a solution for the separation of conductive paths from plastics, taking into account the legislative approaches,the existing methods of PCB separation, the composition, and the production of PCBs and also the binders used in PCBs. We used the knowledge of process engineering to design a mathematical description of temperature fields in PCBs and the stress. To a great extent, we have devoted ourselves to the simulation experiments of PCB heating and cooling and the determination of temperature fields and the corresponding temperature-dependent cyclic mechanical stresses. The simulation was performed in the Pro / ENGINEER and COMSOL Multiphysics® software environments, because of the possibility of solving multiphysical problems. The outputs from computer simulations are the initial stage for the design of an eco-friendly way of recycling PCBs. In the future, we will focus on the more complicated issue of recycling multilayer PCBs. The development of new criteria for PCB recycling has opened new possibilities for the treatment of the used materials.

In recent years, concerns have been raised over excessive use of pesticides [1], their toxicity and the potential to pollute the environment. In this context, the interest for innovation in biostimulants and fertilizers with systemic effect on plant metabolism has increased [2], as an alternative for pesticide and synthesis fertilizer reduction.
The goal of the paper is to review the main achievements in the designing and application of new biostimulants and fertilizers based on leather industry, aquaculture and sheep breeding by-products.
Collagen and keratin have been extracted, solubilized, refined and conditioned by the processing of collagen and keratin based by-products such as: hide fleshings, leather shavings, fish skins or unmarketable wool [3]. For this purpose, chemical and chemical-enzymatic hydrolysis processes allowed new products to be adapted to the nutritional needs of different plant species. Thus, wheat seeds were treated with low amounts of pesticides in admixture with collagen hydrolysates [4]. Greenhouse and field experiments have shown that plants are more resistant to climate change and extreme soil pH. The formulation and experimentation of mixtures of collagen hydrolysates, keratin and essential oils for foliar fertilization of cereal plants has led to substantial production increases for wheat crops. Another direction of research was that of crosslinked collagen-based products with long-term nitrogen releasing that have been experimented with promising results for treating seeds and leguminous plants. The elastic properties of fish collagen have been exploited to cover rapeseed pods in order to improve the indehiscence and reduce production losses [5]. The versatility of collagen and keratin extracts was proved and the premises for biomass recovery and reuse in agriculture open the door for increased circularity of many economical domains.
Keywords: bio based fertilizers, sustainable agriculture, protein hydrolysates

KEYWORDS: Collagen, Keratin, By-products, Circular Economy Industrial and agricultural by-products represent an important resource of raw materials and added value, whose processing and introduction into the economy, produces a significant reduction of the environmental impact. The leather industry generates a large amount of collagen and keratin by-products, which are generous energy sources for biostimulation and organic fertilization of plants [1], soil enrichment, but are also suitable for industrial applications: biodegradable packaging, adhesives, surfactants, auxiliaries for leather processing [2] etc. The literature information in this field refers to the study of specific properties for individual application. In connection with our new research in valorisation of collagen and keratin from by-products, we have investigated the structural and textural properties of protein composites obtained from leather industry by-products, in order to identify the complementary properties, for directing the same composites obtained with minimum manufacturing costs to several applications. This paper presents results obtained in the analytical investigation of gelatin extracts, collagen and keratin hydrolysates and proteinic composites made on the basis of these extracts. For this purpose, texture analyses were performed by the TEX'AN equipment provided with tools for the analysis of gels and films, structural analyses by FTIR-ATR, particle size distribution by Dynamic Light Scattering. It has been found that collagen and keratin extracts contain sufficient proportions of small and medium size components size, of the order of 1-100 nm and of 100-1000 nm, specific for free amino acids and small oligopeptides. The small peptides usually show better bioactivities than larger peptides [3] and can penetrate plant cell membranes and induce immediate systemic effects on biostimulation and protection. However, collagen and keratin extracts contain large size components, over 1000 nm, in considerable proportions, which provide film-forming properties with controlled biodegradability and thus a delayed release of amino acids, for a gradual nutrition of plants in vegetation. In industrial applications, small and medium-sized compounds are associated with the surfactant properties [4], while large molecular compounds induce the adhesive and film-forming properties [5].

Considering the balance between rapidly growing global tire demand and scarcity of natural resources, recycling and reclaiming techniques of tire rubber have become the state of the art. Herein, we set out to implement a self-designed thermo-oxidative reactor for the exfoliation of carbon black (CB) from ground tire rubber, which is efficiently functioned under a thermo-oxidative reclaiming condition without any additive. The exfoliation of CB from rubber vulcanizate was realized by scission of main chain, and of cross-linked network. The degree of scission was discussed through gel permeation chromatography and using Horikx theory. Sol fraction tremendously increased to 66.0 % after thermo-oxidative reclamation at 200 ºC for 20 min. Thermo-oxidative scission underwent through the oxidative cleavage of main chain, and of sulfur cross-links, proved by Fourier transform infrared spectroscopy. The ultrafine exfoliation of CB from rubber proved by field emission scanning electron microscopy. The exfoliation was further improved by two roll milling. Exfoliated rubber was incorporated within tire rubber composites as a reinforcing material due to the core-shell structured CB, which was observed with increased effects to the rubber composites. This work presents a potential contribution to the industrial recycling for future applications and to control the pollution of waste tires.

Three-dimensional (3D) bioprinting has been employed in recent years as an attractive method for tissue engineering. [1] Using a 3D bioprinter allows proper distribution and positioning of biomaterials and cells to create desired constructs. [2] One of the major challenges associated with 3D bioprinting is the development of materials that can be used as suitable bioink. Namely, hydrogels formed by biopolymers (collagen, gelatine, hyaluronan, etc.) are of particular interest because of their capability to mimic the cell’s extracellular matrix (ECM). [3]
The present work is aimed at the preparation and direct embedding of cells in 3D printed materials. Although native collagen is the major structural component of ECM, this biopolymer is less applicable for hydrogel preparation suitable for microextrusion due to its lower viscosity as well as accessibility to chemical modification. [4,5] Therefore, bovine or rabbit gelatines prepared from industrial collagen by-products (waste) were used in this study. Moreover, gelatines were mixed with hyaluronan and chemically cross-linked by glutaraldehyde to acquire materials with appropriate properties for 3D bioprinting. During the cross-linking, forming hydrogels were mixed with fluorescently stained fibroblasts and printed. Finally, cell distribution within the printed material was investigated using fluorescent imaging. In conclusion, chemically cross-linked hydrogels composed of biopolymers were prepared as a potentially promising bioink with application in 3D printing.

Yeasts, especially Saccharomyces cerevisiae species and similar, are used in food technologies for centuries. Even though they are produced commercially, they present in many cases abundant by-products or even waste. It is estimated that spent brewer’s yeasts account for approximately 2 % of the overall beer production [1]. They are usually used to some extent in animal feed; however, large quantities are disposed [1, 2]. Bakery or brewery yeasts present available source of proteins and functional peptides, minerals, trace elements, vitamins and even rich source of β-glucans, among others [2]. Processing of yeasts is a key factor determining the yield of valuable compounds like proteins, digestibility and nutritive value of the prepared functional food components [2, 3]. Hydrolysis is one of the common and perspective methods of protein fraction isolation from yeasts [2]. In addition, hydrolysed proteins of lower molecular weight are advantageous in food supplements for athletes and in the field of special nutrition [2, 3, 4]. Despite the fact that many technically feasible procedures for yeast processing have been proposed, it is usually the economic viability of the technology that is crucial for its practical application in the industrial scale [2]. The aim of our work was to investigate protein fraction isolation from yeasts via hydrolysis catalysed by lactic acid and assess the possibility of the process scale-up. The key operation is the reaction mixture filtration, which was used to separate the liquid fraction with extracted proteins from the solid residues. The effect of reaction temperature (100 – 140 °C) on the yield of soluble dry matter, protein and on filtration parameters was evaluated. It was shown that it is possible to reach a dry matter yield of more than 80 % and the amino acid composition of the final hydrolysate was determined. In addition, gained results clearly documented the impact of hydrolysis conditions on scale-up of the reaction mixture filtration.

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