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Periodic Report Summary 1 - ECOFLOC OPTIMIZE (Combining an eco-friendly approach and a product performance approach to develop novel flocculation strategies)

Marie Curie Initial Training Networks (ITN) – European Industrial Doctorate (EID) - FP7-PEOPLE-2013-ITN- 604825
Combining an eco-friendly approach and a product performance approach to develop novel flocculation strategies - ECOFLOC Optimize

The main objectives of the project can be summarized as follows: development of new, more eco-friendly flocculants and to follow a product performance approach to establish a map of product effectiveness versus flocculant characteristics to enable the development of predictive models for the flocculation process, which allow more informed choices of flocculants for each specific process/application.
Regarding the first objective two approaches are proposed: development of polymers based on natural resources, namely cellulosic wastes (WP2) and development of new synthetic polymers using either new, more eco-friendly monomers and/or synthesized using more health friendly oils, reducing the VOC component in the synthesis (WP3). The first topic of these objectives constitutes the theme of the research plan of ESR1, while the second one is the theme of the research work of ESR2.
As for WP5, "Developing a map of flocs structure versus flocculant characteristics", the ultimate objective of this WP is to construct a structure map to facilitate informed selection of flocculants to attain targeted flocs structures. The flocculants developed in WP 2 and 3 will be tested in this WP, regarding their performance in pre-selected model systems. The construction of the map of flocs structure versus flocculant characteristics will be based on an experimental design methodology, which will help in preparing better the performance tests, as well as on the identification of the most important variables for the response.
Also, the ultimate objective of the project is to graduate two PhD students, combining an academic with an industrial environment during their training.
Two ESRs have been recruited by the project who share their contract time between the University of Coimbra (Portugal), Aqua+Tech (Switzerland) and the Associated Partner, Universilty of Leeds (UK). The Research Plans for the two ESRs have now been completely defined as follows:
ESR1 - Development of polymers/polyelectrolytes based on renewable resources
ESR2 - Development of novel flocculants to treat oily waters using health-friendly processes
Recruitment of the two ESRs, Kinga Grenda (Polish, MSc in Chemistry, Lodz University) and Anita Lourenço (Portuguese, MSc in Biochemistry, New University of Lisbon) took place during the first semester of the project.
Both ESRs registered for PhD in Chemical Engineering in the University of Coimbra, having spent the first 3 months of their contract completing several courses from the curricula of the Doctoral Program in Chemical Engineering. Also, during the first period of the project (1st 24 months) they were offered several short courses on complementary skills such as: Communication Skills; Entrepreneurship and Advanced Statistics.
During this first period of the project research was focussed mainly on WP2 (Modifying natural polymers and natural by-products for coagulation and flocculation purposes) and WP3 (Synthesis of novel flocculants based on oil-free processes or novel monomers).
Regarding WP2 the work has been directed to obtaining cheaper but effective, natural based flocculants form cellulose wastes and also performing modification on tannins to obtain natural coagulants for effluents treatment from different possible industries (e.g. pulp and paper mills and textile industries). It was possible to modify tannins from different origins which were tested with positive results in decoloration of model coloured effluents and in an industrial water. One of the points which needs further consideration is the variability of the raw material even when the origin is kept constant. Additionally, at UC the main objective has been to obtain cellulosic polyelectrolytes for effluents treatment, the focus being again on polyelectrolytes which can be used for decoloration of industrial effluents. Modification of cellulose extracted from bleached pulp fibres (eucalyptus fibres) or eucalyptus wood wastes, or direct modification of bleached pulp fibres was attempted. So far it was possible to cationize with success cellulose extracted from bleached pulp as well as the bleached pulp itself, producing, in both cases, soluble polyelectrolytes. Those polyelectrolytes were tested with a range of dyes, very good results having been obtained, mainly when compared with the use of traditional flocculants.

So far, it was also possible to obtain anionic cellulose (soluble polyelectrolyte) starting from extracted cellulose recovered from bleached pulp. These polyelectrolytes are still under testing.

Regarding WP3 the work has been focussed on the development of new flocculants to treat oily waste waters, mostly organic in nature, using health-friendly processes in their synthesis. The goal is to produce a specific product to treat a defined wastewater, avoiding the problems of having to overdose polymers designed for other types of waters. New health-friendly oils with reduced VOC emissions were used as synthesis media. These oils were first used to synthesize well-known polymers (acrylamide co-polymers) which allowed us to choose the two health-friendly oils with better performance. These two oils were then used for the synthesis of new co-polymers which are expected to perform better in the treatment of oily waste waters. Both cationic and anionic polyelectrolytes with a range of charge densities have been produced, which presented good performance in the treatment of three different types of industrial oily effluents: dairy effluent, fried snacks company effluent and olive oil mill effluent. At present, work is being directed to the synthesis of terpolymers, based on the co-polymers already developed, and containing a hydrophobic monomer (in different percentages) in order to increase the affinity of the polyelectrolyte to the oily phase.

In the next period the research work of the ESRs will be mainly directed to WP5 (Construction of a map of flocs structure versus flocculant characteristics). For that, besides the performance tests already conducted, a specific test will be developed to assess the characteristics of the flocs produced when the characteristics of the polymer change. That test will be based on the assessment of the flocs characteristics (size and structure) using Laser Diffraction for that purpose. An experimental design strategy will be used to construct that structure map.
Besides the work in WP5, some future work will still be conducted in relation with WP2 and WP3: WP2 - scale-up of the tannins modification process and finalize the modification of cellulose obtained from eucalyptus wood chips, checking the influence of lignin on that modification; WP3 - Synthesize terpolymers containing an hydrophobic monomer.
Also, in the next period, the two ESRs will have a one month stay at the Associated Partner (University of Leeds), to complement their training and to perform some complementary tests which will allow understanding better the behaviour and flocculation mechanism of the polymers produced. Additionally, another two short courses on complementary skills will still be offered during the coming period (IPR Management and Life Cycle Assessment).
Dissemination will be another task to go on developing during the next period, namely by producing a video about the project to be included in the project website, and finalizing, according to the project dissemination plan, with the organization of a final project workshop under the topic of “Polyelectrolytes and Water Treatment”, which will be open to the research community, companies, and PhD students, among others.

It is expected that the outputs of this project can have positive impacts in different European priorities. The first targeted impact is directed to the development of more eco-friendly aids for effluents and water treatment, which are essential to preserve water quality, one of the first line European priorities. However, the polymers being developed, namely the ones derived from cellulose, are expected to have application in different sectors and/or products, such as additives in papermaking, including filters production, cosmetics and food industry, either due to its biodegradable nature or to their enhanced properties. Also, the perspective of defining the polymer architecture based on the application and function envisaged, using product engineering tools and leading, in the end, to a structure map, is, altogether, an innovative approach for the development of these materials, which, if successful, can be applied to the development of polymers for other applications.
Finally, the training of highly qualified human resources (PhD graduates) in a mixed environment, joining academic and private sector, constitutes a benchmark for this type of training having a positive economic impact, since it will allow access of the private sector to better qualified human resources, most important, qualified according to the private sector needs. The new training methodology proposed here is highly innovative and it is believed will spread in the future with benefits for both the public and private sectors.

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Life Sciences
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