INNOVATION AND NEW PRODUCT DEVELOPMENT IN MEMBRANES – STEPS IN THE DEVELOPMENT OF THE LATEST MEMBRANE PRODUCT FROM SIEMENS – THE ‘N’ SERIES. Christopher Kersten1 1 Siemens Australia Ltd 15 Blackman Crs Windsor NSW 2756 christopher.kersten@siemens.com ABSTRACT Siemens manufactures MEMCOR® ultrafiltration products at its factory in Sydney, Australia. The R&D team at the factory consists of 35 engineers, scientists and technicians working in the areas of membrane formulation, membrane and module design, manufacturing and membrane processes. This paper outlines key stages that a new membrane development goes through, using the example of Siemens’ most recently released membrane formulation, the ‘N’ series. The starting point for the ‘N’ series of membranes was the membrane formulation stage. The ‘N’ product was developed as part of an ongoing project within Siemens to identify and test new membrane materials and manufacturing regimes. The aim of this development work is to identify new membranes with improved hydraulic and durability performance compared to commercially available membranes. Development Phase: Once a promising formulation is identified there are several stages to pass on lab scale manufacturing and testing. Then, pilot scale manufacturing demonstrates the product is manufacturable and products are made for field performance testing at R&D trial sites. Validation Phase: Following successful pilot testing, larger scale manufacturing runs are conducted. These produce membranes for validation testing, typically undertaken at customer sites and on a range of water sources. In parallel, applications for various state and regional approvals are initiated. This includes NSF61 approval in the US for products that come into contact with drinking water, and Regulation 31 approval for contact with drinking water in the UK. Commercialisation Phase: When validation is complete the product moves to commercialisation. This includes the scale-up of manufacturing, which requires new capital equipment or changes to existing manufacturing processes. Other steps include the development of technical documentation and marketing materials, and training of service teams and the sales force, leading up to product launch. C. Kersten MEMBRANE DEVELOPMENT Memcor was one of the early pioneers in the use of membranes for water treatment. This started with the development of polypropylene microfiltration (MF) membranes in the 1980’s and 1990’s, including the M10C membrane module. The M10C is still produced by Siemens today and is used in a number water treatment plants around the world, including two plants supplying the city of Tauranga in the North Island of New Zealand. When Tauranga’s Joyce Road treatment plant was upgraded in 1997 it was the first public sector use of microfiltration membranes in New Zealand (www.tauranga.govt.nz, 21 July 2012). Siemens acquired the ‘Memcor’ and ‘Memtec’ brands as part of its purchase of the ‘US Filter’ business from Veolia Environnement in 2004. Siemens had seen the growth opportunities in the water market and made a decisive move into the water industry. In a joint Press Release with Veolia, then President of the Siemens I&S division Jorgen Ole Haslestad was quoted as saying (www.veolia.com, 12 May 2004), "This acquisition is an important step in the framework of strengthening our Group portfolio. The growing water segment will play a critical role within our industrial activities at Siemens. With it, we will be able to expand our product and service offerings for our customers, in particular within the world's largest water market, the United States." Siemens membranes are manufactured at a 15,000 sq.m facility in Sydney, Australia. The R&D team based within the factory comprises 35 engineers, scientists and technicians, and is continually developing and evaluating new membranes. While polypropylene still makes a well performing membrane, market demand for membranes has shifted towards materials that have higher chlorine resistance. Polyvinylidene difluoride (PVDF) has emerged as one of the preferred materials for MF and UF membranes, due to its superior chemical resistance, as well as improved flexibility and toughness when compared to alternatives such as Polyether Sulphone (PES). Membranes made from PVDF provide excellent chemical resistance, good mechanical properties, and excellent filtration performance. PVDF is widely used in the water treatment industry by a number of membrane manufacturers (Pearce, 2007). Market analysis and customer feedback are the precursor to membrane development at Siemens. These drive the product specification and performance targets that lead to the development and commercialisation of new membranes. A recent series of work at Siemens has culminated in the commercialisation of a new PVDF membrane product – the ‘N’ series of membranes. This comprises a new membrane formulation integrated into some of Siemens existing module configurations. New products include the S10N submerged filtration membrane module, and L10N and L20N pressurised system membrane modules. This paper outlines 3 stages in the development of a new membrane at Siemens – Development, Validation and Commercialisation. These are part of Siemens wider Product Lifecycle Management (PLM) process that exists for each product line from idea conception, through to ultimate obsolescence. Development Phase Drawing on Memcor’s 25 years of experience in membrane technology, new materials and membrane formulations are systematically developed and tested to meet product innovation targets. Formulation design and development are used in conjunction with manufacturing process control to meet product performance criteria such as pore size, filtration performance, hydraulic stability and mechanical stability. By developing, selecting and refining products 2 C. Kersten using a method akin to an ‘innovation funnel’, products are optimised and selected that best meet the product performance targets. The culmination of the development phase is the manufacture of full scale modules in standard configurations. These are operated at Siemens controlled testing facilities located in Sydney and Singapore. Modules are operated over a range of different fluxes and with different backwash conditions. Membrane cleaning regimes are also tested to establish the relative hydraulic performance capability and stability of new formulations in comparison to previous formulations. Figure 1 illustrates some of the pilot testing equipment used to collect product performance data. Figure 2 shows the type of hydraulic performance data that is collected and evaluated on development modules. Figure 1 - Siemens pilot testing equipment Figure 2 - Example of permeability data collected Validation Phase Following a successful test outcome in the development phase, the formulation is moved into validation. Larger production runs of several hundred modules are made. The majority of these will be beta-tested at selected customer facilities. Sites are chosen on a number of criteria including: • customer relationship, • ease of access to site and retrieval of site data, • time to installation, • any regulatory limitations, and • exposure to feedwater sources or applications of interest Testing occurs over 6 to 12 months. During this time, plant hydraulic performance is monitored, and modules are periodically removed and returned for autopsy analysis including fouling resistance, membrane permeability and integrity. At the end of the initial testing phase modules are normally left in place to develop a longer term data set. This testing is used to validate the performance of the new membrane, and also forms part of a set of case studies to support the sale of the new product. In parallel with this beta-testing, applications are made for regulatory approvals in established markets such as the United Kingdom and USA. Some Asian countries are also starting to develop a regulatory framework to control what products and manufacturers are able to 3 C. Kersten supply into these markets. Some might expect this be an activity undertaken during Commercialisation rather than Validation, but regulatory approvals for contact with drinking water are a key precursor to being able to launch a new product in these major markets. They also can take a long time to complete, so these approvals are initiated as soon as possible after the product design development stage is completed. Regulatory approval in the US starts with NSF/ANSI Standard 61 Drinking Water System Components (NSF61). NSF uses a 7 step approach (www.nsf.org, 21 July 2012) from application submission, a review of formulation information, initial plant audits, sample testing and a toxicological evaluation. The NSF61 accreditation covers not only Siemens manufacturing processes, but also those of the raw material suppliers. The timeline for an NSF61 accreditation can range from 3 to 12 months from the time an application is submitted. The N series membrane obtained NSF61 approval in August 2011. For the United Kingdom, approvals for materials to be used in contact with drinking water are obtained from the Secretary of State, under Regulation 31 of the Water Supply (Water Quality) Regulations 2000 (DWI, June 2012a). Their decision is aided by advice and testing co-ordinated by the Drinking Water Inspectorate (DWI). For water filtration membranes there is a 2 step testing process (DWI, June 2012b). The first step is an assessment of any effects on water quality from the materials used in the filter. This can be achieved by testing each material to the requirements of BS6920 and/or listing by the Water Regulations Advisory Scheme (WRAS). The second step is a leaching study where a complete unit is tested. The timeline for UK approval is typically more than 6 months from the time an application is submitted. For the N series membrane, the second step – full unit testing – has not yet been completed in the UK, and as such the product cannot yet be used for drinking water applications in that region. In Australia and New Zealand, Standard AS/NZ 4020 – Testing of products in contact with drinking water provides guidance but is not a regulatory approvals process. Historically, NSF61 approval has been viewed positively by customers in Australia and New Zealand. In contrast there is a growing trend to regulating the waste water recycling sector. All States in Australia have endorsed the 2006 Australian Guidelines for Water Recycling (AGWR) (McCormick, 2010), though some States such as Victoria are more advanced in introducing legislation that reflects this than others. The AGWR adopts a HACCP style approach to risk management for each process stage in a treatment plant, using a 3 step approach – Validation, Monitoring and Verification (McCormick, 2010). In this case Validation involves challenge testing to establish a conservative minimum Log Removal Value (LRV) rating for bacteria and virus for each membrane type. Commercialisation Phase As of August 2012 the ‘N’ series product is in the Commercialisation Phase. There are both internal and external aspects to Commercialisation. On the internal side, one of the key focus areas is the ramp up of new product activity. This includes commissioning of new or upgraded capital equipment and identifying and troubleshooting any issues that impact on staff safety, quality and throughput. Bills of Materials (BOM’s) for the new products need to be developed and validated, and any new materials incorporated into the production planning, supply chain and Material Resource Planning (MRP) systems. QC specifications and Work Instructions are developed for any new or modified production processes, and manufacturing staff undertake training on these. Internal sales force training is undertaken to make staff aware of the 4 C. Kersten performance parameters of the new membrane and the value proposition of the product to the end users of the technology. Internal documentation such as process design and project costing tools need to be updated for the new product. On the external side, product specific documentation is developed to support the new product, as well as case studies of some of the Validation test work. An example of such documentation is the product specification sheet for the L20N membrane shown in Figure 4 below. There are also product manuals, sales brochures and other documentation that need to be revised. As part of production planning, existing backlog orders are reviewed for suitability to convert to the new product, and internal and external discussions are held about if and when specific projects could transition to the new product. A limited release of the N series modules on selected projects and customers has begun to utilise existing manufacturing capacity, while the factory tools up to produce the new membrane in larger quantities. Figure 3 shows some L20N modules in progress in the factory. Figure 4 - Product Specification Sheet Figure 3 - L20N modules in the factory Conclusion There are 3 key stages in Siemens development of a new membrane product. The first is membrane development and performance testing at our research facility in Sydney, Australia. The second stage is validation of a chosen membrane formulation, including testing at pilot level and full scale testing at customer sites. This is carried out in parallel with regulatory approvals. The final stage is commercialisation, where the factory is tooled up for full scale production and larger numbers of membranes are put into service. Longer term monitoring of initial validation sites is also undertaken in this stage. The timeframe from concept to final commercialisation is product dependent, but can typically range from 12 to 24 months. 5 C. Kersten References DWI, June 2012a. Advice Sheet 1, Overview of the application process and general requirements, Version 6.4 http://dwi.defra.gov.uk/drinking-water-products/advice-and-approval/Advicesheet1.pdf DWI, June 2012b. Advice Sheet 6, Approval of membrane filtration systems & associated equipment, Version 1.7 http://dwi.defra.gov.uk/drinking-water-products/advice-and-approval/Advicesheet6.pdf McCormick, A. 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