First Results. E4Water Case Studies. Economically and Ecologically Efficient Water Management in the European Chemical Industry.

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1 Economically and Ecologically Efficient Water Management in the European Chemical Industry E4Water Case Studies First Results This project has received funding from the European Union s Seventh Programme for research, technological development and demonstration under grant agreement No

2 imprint Imprint: DECHEMA e.v. Theodor-Heuss-Allee Frankfurt a.m. Germany Dr. Thomas Track & Dr. Christina Jungfer Phone: +49 (0) /-364 Fax: +49 (0) Status Case Studies: January 2015 Disclaimer notice: The European Commission is neither responsible nor liable for any written content in this brochure. 2

3 Economically and Ecologically Efficient Water Management in the European Chemical Industry table of contents Table of contents E4Water project partners 4 E4Water Overview 5 E4Water Case studies: First Results 6 Case Study 1 Dow Case (Netherlands): Mild Desalination Concept 6 Case Study 2 Solvic Case (Belgium): Industrial experimental garden 7 Case Study 3 SolVin Case (Spain): Process continuation by water loop closure 8 Case Study 4 Procter & Gamble Case (Belgium/France/Czech Republic/ ): in-process water loop closure 9 Case Study 5 TOTAL Case (France): Water management in petrochemical industry 10 Case Study 6 Kalundborg Case (Denmark): Symbiotic industrial waste water treatment concept 11 3

4 project partners E4Water project partners Campden BRI United Kingdom CBD Kalundborg Kommune Denmark CEFIC Conseil Européen de l Industrie Chimique Belgium DECHEMA Gesellschaft für Chemische Technik und Biotechnologie e.v. Germany Dow Benelux B.V. Netherlands Danmarks Tekniske Universitet Denmark Evides Industriewater BV Netherlands Fachhochschule Nordwestschweiz Switzerland IVL Svenska Miljöinstitutet AB Sweden Ondeo Industrial Solutions SA France Procter & Gamble Services Company NV Belgium Solvic NV Belgium SolVin Spain SL Spain TNO Nederlandse Organisatie voor Toegepast Natuurwetenschappelijk Onderzoek Netherlands Total Petrochemicals France SA France Technische Universität Berlin Germany Technische Universiteit Delft Netherlands Universidad Complutense de Madrid Spain VITO Vlaamse Instelling voor Technologisch Onderzoek N.V. Belgium 4

5 Economically and Ecologically Efficient Water Management in the European Chemical Industry overview E4Water The Project Chemical industry provides the highest potential for increasing eco-efficiency in industrial water management. E4Water addresses crucial process industry needs to overcome bottlenecks and barriers for an integrated and energy efficient water management. The main objective of E4Water is to develop, test and validate new integrated approaches, methodologies and process technologies for a more efficient and sustainable management of water in chemical industry with cross-fertilization possibilities to other industrial sectors. Expected impacts: Independency from fresh water Less waste water production Less energy use Economic benefit Policy compliance Applicability to other industries WWTP E4Water is envisioning the realization of its concept by: (1) creating water loop interfaces, synergies and symbiosis: (a) in industry (b) with urban & agricultural water management (2) developing and testing innovative materials, process technologies, tools and methodologies for an integrated water management (e.g. closure of industrial water loops; reuse/ recycling of wastewater) (3) providing an open innovation approach for testing E4Water developments with respect to other industries (4) implementing and validating the developments in 6 industrial case studies, representing critical problems for the chemical industry and other process industries, (5) implementing improved tools for process efficiency optimization, linking water processes with production processes, and eco-efficiency assessment. For the realization of the E4Water concept chemical industry along the whole value chain is involved. WWTP Pre-treatment Processes Cooling WWTP Rain water CS1, 2 Symbiotic reuse Pre-treatment Processes CS4 Cooling CS5 integrat WW treatment for recycling & reuse CS1-6 Limited treatment for recycling high conc. streams CS1, 2, 3 Processes Cooling Valuables CS2, 6 Symbiotic reuse Natural water recources: scarcity, pollution and regulatory demands (e.g. WFD) Natural water recources: good quantitive & qualitative status; Industry: reduced demand & discharge, regulatory complience Figure 1: Today s situation with limited recycling/reuse components and limited connections across sectors (the width of arrows is in both figures an indicator for the water demands). Figure 2: The E4Water concept, following an integrated, multi-disciplinary and holistic approach in different industrial scales and across sectors. The dashed lines indicate the impact by E4Water, CS (= case study) indicate where on site industrial pilot testing and demonstration are focused on, the number allows their identification. E4WATER PROJECTS FACTS Project Duration: May 2012 April 2016 Project Consortium: E4water unites in its consortium large chemical industries, leading European water sector companies and innovative RTD centers and universities, active in the area of water management and also involved in WssTP and SusChem and collaborating with water authorities. Project Website: www e4water.eu 5

6 FIRST RESULTS: CASE STUDY 1 Dow Case (Netherlands) Mild desalination of water streams for optimum reuse in industry or agriculture at affordable costs SITUATION As a chemical site Dow Terneuzen (The Netherlands) has a significant demand for fresh water with major applications in cooling and heating (via producing steam) to run its processes. Situated at the river Scheldt estuary, the region where Dow is located suffers from an intrinsic lack of fresh water. Therefore Dow and its partners are exploring alternative water sources to meet its fresh water demand. OBJECTIVE Produced water for end users in industry or agriculture has to meet the quality specifications of the targeted application. Typically many applications in both sectors require water with a salinity (expressed as electrical conductivity) of less than 1 ms/cm. The objective is to reach a production cost below 0.4 /m 3 at a volume of 3-4 million m 3 of potential reuse water. E4WATER ACTIVITIES AND FIRST RESULTS Various water streams currently discharged to the river Scheldt have been selected on their reuse potential, both from a quantitative and qualitative point of view. These comprise both industrial water streams, like excess treated wastewater and cooling tower blow down streams, rural streams originating from farm land run-off, municipal discharges, and rain. However, all streams contain varying amounts of inorganic salts, which make them unfit for direct usage in industrial applications or agriculture. Hence, the E4Water Case Study 1 demo (CS1) is designed, build and operated by Evides Industriewater to develop commercial applications for a mild desalination of these different raw water streams. The required degree of desalination depends on the specifications for the final application of the produced water by the end-user, which can either be industry (Dow or any other nearby facility) or agriculture. OpenStreetmap The first results show that both the rain/surface water and treated wastewater tolerate a fairly modest pretreatment consisting of a coagulation/flocculation step to remove suspended solids and residual organics followed by ultrafiltration (UF). Cooling tower blow down water apparently is more challenging, due to the nature of the constituents present in the water. OUTLOOK The demo and supporting RTD work at partner institutes will yield data that can be used to scale up mild desalination units to produce water from various sources at affordable costs. These data comprise among others the definition of suitable pre-treatment, energy requirement, achievable water quality, and feed source flexibility. The set-up of the pilot comprises two parallel treatment trains at the demo site, one consisting of NF (Nanofiltration), the other based on EDR (Electrodialysis Reversal), proceeded by a combined robust raw water pre-treatment. As feed streams to the pilot three different brackish water sources were directly connected to the pilot unit. These were 1) Collected rain/ surface water, 2) Treated process wastewater, and 3) Blow down from process cooling towers. The major focus after the startup was on defining the appropriate pre-treatment conditions to enable stable operation of the subsequent desalination step. 6

7 Economically and Ecologically Efficient Water Management in the European Chemical Industry SOLVIC Case (Belgium) FIRST RESULTS: CASE STUDY 2 Enhance the water reuse by global management and synergy identification on a multi-company site SITUATION The Solvic site Lillo is located in the Port of Antwerp (Belgium), a coastal region that faces pressure on fresh water uptake by regulatory demands (Flanders Integral Water Policy and Rainwater Decree ). OBJECTIVE The aim is to come to a water management concept that is close to zero salt waste and zero liquid discharge. The focus of the Solvic Case is the production of high quality process water from wastewater and cooling water streams with inorganic loads (up to > 5000 mg/l salts) and variable flows ( m³/h) and enables synergistic effects with neighboring industries in the Port of Antwerp Chemical Cluster. The Solvic Case serves as an Industrial experimental garden (figure) to enhance innovation with regard to water reuse in the chemical sector leading companies to a symbiotic cooperation. Solvic works in close collaboration with its partners: Evides Industriewater and VITO (Vlaamse Instelling voor Technologisch Onderzoek). Experimentation and demonstration of different technologies is being done in an environment shielded from the hazards of testing in a production environment and is under specific conditions accessible for external users. The testbed is being used as a proof of concept or when a new module is tested apart from the program/ system it will later be added to. Apart from demonstration of new technologies, the testbed is also used to demonstrate advanced water loop closure and to produce high flow high-quality process water for internal use. The Solvic Case is also being used for research (mild and extensive demineralization technologies, reuse of value products etc.). They provide input from their testbed for the other partners. water (± µs/ cm) and producing 12 m³/h demin water (< 5 µs/cm). Demo unit 3 is testing the recycling of a wastewater (8 14% NaCl) from an external company X in the process of Solvic. It is now in commissioning phase at the supplier site and afterwards at Solvic site. OUTLOOK In the future, Solvic will keep working on its water management concept. With the results of the different pilot plants on site Solvic can achieve its goal to come close to zero salt waste and zero liquid discharge. Demo units 1 and 2 can be served as basis for a full scale unit and demo unit 3 can be transported and used on other multi-company site to test the possibility of recycling waste water in the same process. The Solvic experimental garden will provide a platform for demonstration scale testing of technologies that allow improved water and salt reuse in the chemical industry. Further it incorporates industrial symbiosis by using wastewater from neighbouring companies to produce high quality process water and reusing salty wastewater in the chlor-alkali process. E4WATER ACTIVITIES AND FIRST RESULTS At Solvic site different water sources are available for reuse and recycling (figure). The technological and operational support for demo units 1 and 2 is done by Evides Industriewater. Demo units 1 and 2 are reverse osmosis based desalination installations that aim to produce high quality process water. Demo unit 3 that is supported by Solvic will use external wastewater with high salt concentration for the chlor-alkali process. The status of the Solvic Case after two years is as follow: The demo unit 1 has been operational for 2 years but due to some problems with quantity and quality of the feeding water the pilot recently had a shutdown. Membranes have been replaced and the pilot is currently started up again. It produces 20 m 3 /h water (< 10 µs/cm) from 30 m 3 /h mixed wastewater (± 2000 µs/cm). The demo unit 2 is currently taking in 30 m 3 /h brackish surface Wastewater Rain water Brakish surface water Concentrated wastewater Wastewater company X Wastewater company X Industrial Experimental Garden Modular Demo Unit Module 3 Pilot test Pilot test Module 2 Module 1 Concentrates Pilot test Product Process water 7

8 FIRST RESULTS: CASE STUDY 3 SolVin Case (Spain) Ensure process continuation by closing the water loop and minimizing fresh water use SITUATION SolVin Spain S.L. is located in Martorell (Spain), a region where the water scarcity is a fact since one or two decades. Thus, both water abstraction and disposal are regulated by law and permits, having stringent limitations which cannot be trespassed. OBJECTIVE The mother water is qualified as a complex organic load and high flow (in the case of Martorell approx. 100 m 3 /h). The PVC production unit under consideration uses about 33 % of the total on-site water consumption. The aim is to close further the water loop for this production and to realize additional water savings of 25 %. E4WATER ACTIVITIES AND FIRST RESULTS A pilot MBR (Membrane BioReactor) unit followed by a reverse osmosis treatment by two pass has been installed in the SolVin site in Martorell (Spain) with the aim to treat wastewater from the PVC process. A submerged hollow fibre membrane is being used for the ultrafiltration step since this membrane was tested at semi-pilot scale during almost nine months with good results in terms of filtration performance and recovery of permeability and flux after chemical cleanings. The treated water is meant to reach the quality specifications for recycling back to the original process, this means some target values must be reached at the MBR outlet: PolyVinylAlcohol (PVA) < 1 mg/l, N-NH 4 + < 2 mg/l and a complete removal of the BOD; and at the RO outlet : TOC < 10 mg/l, Al < 0.1 mg/l and conductivity < 10 µs/cm. The MBR pilot has been working for about twelve months. The PVC effluent is cooled prior to MBR treatment in order RO pass and stages detail to reduce temperature from 45ºC to < 35 C (biomass requirement) or even < 25 C (RO requirements). Before the heat exchanger, a 600-micron filter has been installed for avoiding solids retention in the MBR. Biosludge from an existing biological WWTP of SolVin site was used to seed the MBR. Two weeks later, a second seeding was done using biosludge from a municipal WWTP located in Martorell with the aim to improve nitrification/denitrification process and increase the solid content in the bioreactor. During the first weeks of operation the PVA removal rates were around 50 %. After one month of treatment, an almost total acclimatization of biosludge was achieved, with PVA removals higher than 98%. After twelve months of treatment, COD and BOD removals are in the range of % and > 95%, respectively. The flux has been optimized by increasing its value from 1 to 1.8 m 3 /h which means working at a maximum flux equal to 26 LHM. Ultrafiltration/Backpulse (UF/BP) cycles of seconds are done along with daily CIP cleanings (cleaning in place) in the membrane tank. After recovery cleanings, permeability has been very well recovered. Regarding RO performance, good quality permeate is being obtained after two pass treatment for being reused in the polymerization step, with conductivities in the range of 2-4 μs/cm, TOC values lower than 1 mg/l and Al content below detection limits. In order to increase final recovery of the system, first pass reject is being partially recirculated to the first pass without significant pressure increases. In parallel, a lab-scale MBR is being tested at Solvay site in Brussels (Belgium) with the aim to check the replication potential of the treatment route by testing different PVC effluents qualities applying the same commercial membrane quality. OUTLOOK In the future, SolVin will keep working on its water management concept at different production sites throughout Europe. With the results of the different pilot plants on site of Martorell, SolVin will demonstrate the further closing of the loop in the PVC process industry and the challenging recycling of waste water in the same process. MBR pilot 8

9 Economically and Ecologically Efficient Water Management in the European Chemical Industry Procter & Gamble Case (Belgium/Italy/Czech Republic...) FIRST RESULTS: CASE STUDY 4 Enhance in-process water loop closure by integrating biocidal with wastewater treatment technologies P&G SITUATION The manufacturing sites of Procter & Gamble have a long history of improving water efficiency. In the last decade, water consumption was reduced by 50 % (per production volume) on average across the globe. Further progress is very challenging since the remaining high COD loaded concentrated wash water streams are difficult to treat and can not be discharged in the public sewer system. In several cases, these streams need to go to external incineration which increases the cost and as such blocks any further progress in water efficiency. This case study is focusing to develop innovative ways to recycle water streams generated during cleaning and sanitization in household chemicals production. These are small flows of water with high organic load (COD 20,000 50,000 mg/l). OUTLOOK In the upcoming period, some final lab testing will be done to finalize the design criteria for the Tubular membranes. the treatment system (Tubular Nanofiltration + MBR) will be tested in Procter & Gamble plants with different types of surfactant containing products. lab testing with different types of technologies on the 3 th innovation pathway (use of biocidal technologies) will be done to define the technology to be able to reuse/recycle chemicals which are inside the wash water. OBJECTIVE Three innovation pathways are investigated and partly combined: The aim is to combine segregation and separation technologies (e.g. sensors, membranes, evaporators, etc) with traditional wastewater treatment technology and biocidal technologies (e.g. sterilization/pasteurization). The aims are to: Reduce the overall cost of wash water handling, which is the bottleneck to increase water efficiency; Where possible: recycle/reuse the chemicals which are inside this wash water; Where possible: recycle the treated water back into the process. E4WATER ACTIVITIES AND FIRST RESULTS The second period has mainly been focused on testing the individual performance of different types of technologies in the first 2 innovation pathways (1: segregation and separation technologies (e.g. sensors, membranes, evaporators etc.)/ 2: use of traditional wastewater treatment technology for this kind of water). These tests being done on several products to see how the technologies interact with different types of surfactants which can be present in household chemical products (anionic, cationic, non-ionic and amphoteric surfactants). Based on these test results, a treatment system has been defined, combining Nano Filtration Tubular membranes with MBR. This treatment system will reduce the overall cost of wash water handling and will allow treated water to be recycled into the process as cooling tower feed water. Plan of the 6 ton/day membrane unit for the Procter & Gamble E4Water pilot site 9

10 FIRST RESULTS: CASE STUDY 5 TOTAL Case (France) Towards integrated water management system in a petrochemical site SITUATION Tests at the Case Study 5 (CS5) took place at the TOTAL Gonfreville Plant a petrochemical installation in Normandy, France from June 2013 to January It aimed at assessing techniques for water reuse in a petrochemical site which is key to address both water quality and quantity issues. OBJECTIVE 3 treatment lines were operated onsite: 1. the extended wastewater treatment plant: ozonation, biofiltration, ultrafiltration (UF) and reverse osmosis (RO), 2. the cooling water circuit treatment line: sand filter and an alternative disinfection unit (UV light or ozonation), 3. the cooling water blowdown treatment line: UF and RO. E4WATER ACTIVITIES AND FIRST OUTCOMES On the cooling water circuit, the sand filter was the first pilot to be operated (Oct 2013). It showed a protection of total suspended solids of 5 mg/l. Downstream, the UV pilot and the ozone disinfection, whose objective was to control biofouling inside a loop designed on purpose, indicated that microorganisms in a circulating water system were effectively inactivated provided the use of UV at 350 mj/cm 2 or of ozone at dose as low as 0.5 mg/l. The circulating water disinfection took place while biofilm growth was controlled as suggested by the stabilization of the Legionella spp on the material surface. organics and organics has been observed between inlet and outlet RO. Blowdown of cooling water was also tested with membrane techniques between January and February The cooling water has been treated with a UF membrane, allowing to decrease suspended solids to 4 mg/l. The filtered water was then used on a RO membrane, showing a concentration factor of 2 3 on inorganic compounds. Parallel reflections began in 2013, with the aim of treating effluents considered as complex streams. This includes brines generated by RO or highly charged streams that potentially will not be routed anymore to conventional biological treatment due to the new water scheme (spent caustics). Lab works have started during summer TNO is responsible of treatment on 2 aromatics effluents while UCM assesses the impact of brines on biological treatments, with or without in-between pre-treatment. In addition, a life cycle analysis (LCA) based on a water reuse scheme is on-going thanks to a collaboration with IVL. OUTLOOK 2015 will be mainly dedicated to the finalization of results obtained onsite, to the progression on complex streams and the completion of the LCA. On the extended wastewater treatment plant, a biofilter associated with an upstream ozone pre-treatment were operated from January 2014 to January Performances of combined techniques allow full discharge of wastewaters according to the current emission limits values. In particular, BTEX and PAHs were efficiently eliminated from wastewater during treatment via a biofilter (93 to 98 %). Nonylphenols were removed at 30 % efficiency. UF and RO membranes were integrated to the treatment line in August On the UF, filtration flux, chemical enhanced backwashes (CEB) and coagulant were adapted to stabilize the Trans Membrane Pressure around [ mbar] by setting a filtration flux of 65 l/m 2 /h, one CEB/day and 2 ppm of coagulant. On the RO, a single pass on the RO membrane did not allow to reach the Boiler Feed Water quality, but multiple pass will. A concentration rate of 3 4 for in- Wastewater Wastewater Ozonation Biofiltration Cooling water Cooling water Sand filtration Cooling blowdowns Blow down water UF UF Ozonation UV RO RO 10

11 Economically and Ecologically Efficient Water Management in the European Chemical Industry Kalundborg Case (Denmark) FIRST RESULTS: CASE STUDY 6 Bioextraction technology in a symbiotic industrial wastewater treatment concept creating added value SITUATION Direct interfaces and synergies among process industries within a symbiotic network will be developed and tested in the Kalundborg Industrial Symbiosis (Denmark). The Kalundborg Symbiosis is an industrial ecosystem, where the by-product residual product of one enterprise is used as a resource by another enterprise, in a closed cycle. An industrial symbiosis is a local collaboration where public and private enterprises buy and sell residual products, resulting in mutual economic and environmental benefits. The focus of the Case Study Kalundborg is to develop an innovative symbiotic treatment concept for organic wastewater streams coming from industrial fermentation processes. OBJECTIVE The objective is to deliver an industrial wastewater treatment system, based on microalgae, where the maximum removal of nutrients equals maximum added value: Maximize nutrient removal from waste streams via microalgae growth Define the best method for separation of the resulting biomass from the purified water Characterize the biomass components to identify added value targets Evaluate extraction technologies for the different targets Access and evaluate the overall bio-extraction technology in an industrial symbiosis wastewater treatment concept. Symbiosis industry. Tests were performed in a large-scale photobioreactor (4.000 liter) combined with initial tests on pre-treatment of the process water (mechanical sterilization) and post-treatment of the generated algae biomass (dewatering/harvesting) based on selected technologies. Analytical protocols have been established for biochemical composition of microalgae biomass and for the microplate screening procedure validated to mesoscale. Chemical analysis has been performed on the process water before and after treatment and on the generated biomass, in order to identify the potential in nutrient removal and biomass quality generated as a result of a low nutrient based process water growth media, a freshwater microalgae strain and winter process conditions (low light and temperatures). OUTLOOK Large-scale trials in multiple batch reactors and combined continuous configuration, on pre-gasified and mechanical sterilized high nutrient industrial process water. Process optimization and evaluation on bioextraction concept combined with an industrial symbiosis approach. Potentials from added value evaluated with reference to downstream processing in a suggested biorefinery concept Commercialisation potentials of the Kalundborg concept Business Case E4WATER ACTIVITIES AND FIRST RESULTS On Case Study the Kalundborg activities have been focusing on the building phase working towards the establishment of the microalgae facility for treatment of industrial wastewaters. A screening of technologies for pre- and post-treatment activities has been initiated along with the development of the integrated symbiotic concept around eco-efficient recycling of water from the chemical industry and creating added value from microalgae production. Suitable wastewaters for microalgae production has been selected and best microalgae candidates have been suggested for wastewater treatment based on a high-throughput screening method in microtiterplates coupled to a fluorescence plate reader. Green House at the Kalundborg Symbiosis Activities resulted in the completion and official opening of the RTD microalgae facility at the WWTP in Kalundborg, Denmark, which was taken into operation on 8 October First initial tests on biomass production and nutrient removal were performed on one of two screened process water stream identified and made available from the Kalundborg Photobioreactor 11

12 This project has received funding from the European Union s Seventh Programme for research, technological development and demonstration under grant agreement No