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Development of processes and quality procedures for the valorisation of recycled plastics for food contact applications

Final Report Summary - SUPERCLEANQ (Development of processes and quality procedures for the valorisation of recycled plastics for food contact applications)

Executive Summary:
SuperCleanQ was a three-year project, part funded by the European Commission under the Seventh Framework Programme to develop quality control and quality assurance tools and procedures for plastics recycling processing targeted at food contact applications. The aim of SuperCleanQ was:
• The development of important elements within a recycling process to recycle currently unrecyclable black, highly coloured and multi-layer, barrier modified PET
• To create a CEN standard method for the determination of selected organic contaminants in food grade PET products (e.g. products such as bottles)
• The development of a real time in-line monitoring system for the detection of a range of contaminants (e.g. oxybiodegradable polymers) in PET melt processing streams

To meet the Packaging and Packaging Waste Directive 94/62EC and improve sustainability Europe must reuse waste plastics in large high value applications. The largest and highest value market for recycled plastics is packaging, especially in food contact applications. The core concepts of the project were to develop quality control and assurance tools which can be applied to a new process for the recycling of coloured and layered PET into food contact applications that cannot be processed by current PET recycling facilities.

The SuperCleanQ project resulted in:
i. An analytical test method for recycled food contact materials
ii. A sorting technology for black, highly coloured and multilayer PET
iii. A decontamination system for recycling PET
iv. In-line monitoring system for processing lines
v. CEN Technical Specification

The results of the project enable:
• The SME-AG beneficiaries to ensure their members have access to first class European research and quality information
• The members of the SME-AGs to remain effective and continue to meet increasingly stringent European legislation
• The SME partners to transfer the results to their industrial processes
• The partners to increase their competitiveness and demonstrate their innovativeness to their customer base and target industry worldwide
• The promotion of cooperation between different segments of the supply chain
• The improvement of skill levels throughout the supply chain

Project Context and Objectives:

There is an estimated annual 7.7 million tonnes of plastic, mainly packaging, that is currently not recycled in Europe and which could be if the technology and infrastructure were in place to do so. The value of this resource in food contact packaging could be worth up to €7.7 billion. The market demand is there as shown by the high price of recycled PET for food contact applications, which is equal to that of virgin PET. This pricing is driven by the strong demand for food contact recyclates from packaging end-users, especially the Brand owners that are concerned about their corporate image and promoting their environmental responsibilities.
To meet the Packaging Waste Directive 94/62/EC and improve sustainability, Europe must use waste plastics in large high value applications. The largest and highest value market for recycled plastics is packaging, especially in food contact applications, and SuperCleanQ has enabled industry to take advantage of this market opportunity by assisting it in complying with (EC) 282/2008 (Recycled plastic materials and articles intended to come into contact with food) and the other relevant EU regulations such as the Plastics Regulation (EU) 10/2011 and the Framework Regulation (EC) 1935/2004.

The (EC) 282/2008 legislation has opened the market for recyclers to develop new food packaging recycling processes and for plastic converters to develop products containing recyclates in food contact applications. To support this, the objectives of the SuperCleanQ project were to develop quality control and quality assurance tools and procedures for plastics recycling processes targeted at food contact applications. In addition, the project aimed to develop new elements for a process to recycle black, highly coloured and barrier modified PET that cannot be processed by current recycling facilities into food grade material. These elements included a detection system for the sorting stage and a decontamination system for the purification stage.

SuperCleanQ was driven by the SME-AG and Other Enterprises need to develop quality control and quality assurance tools and procedures for plastics recycling processes targeted at food contact applications to enable SMEs to conform to Commission Regulation (EC) 282/2008 on recycled plastic materials and articles to come into contact with food. It aimed to accelerate the development of new recycling processes for the wider food contact materials market and provide quality assurance for converters and end-users of recycled products applications for food contact thereby overcoming barriers and expanding this high value recycling market.

To help companies to comply with the requirements of Commission Regulation 282/2008 and demonstrate to their clients that they are operating good manufacturing practices within a quality assurance framework a new standard was proposed. The establishment of a new standard for the decontamination and quantification of selected contaminants (i.e. marker compounds) in recycled PET for the manufacture of food contact articles is an important addition to the quality control tools that are available to the plastics recycling industry. The standard that was developed by the SuperCleanQ project is a CEN Technical Specification – ‘Plastics – Recycled Plastics – Determination of Marker Compounds in Food Grade Recycled Polyethylene Terephthalate (PET)’.

Once it is published the new CEN Technical Specification will be available to any interested stakeholder, for use on a voluntary basis. In addition to assisting with compliance with (EC) 282/2008, it will enable the PET recycling industry to provide its clients with additional confidence that they are able to deliver food grade recycled PET of a consistently high quality and are operating to a good quality assurance system. The Technical Specification provides a stepping stone for other European, or possibly international standards.

The SuperCleanQ consortium is comprised of SME Associations (SME-AGs), Other Enterprises and research partners (RTDs):

SME-AGs:
• The British Plastics Federation (UK)
• Associazione Nazionale Costruttori di Macchine E Stampi per Materie Plastiche e Gomma
(Italy)
• European Plastics Converters (Belgium)

Other Enterprises:
• Dentis SRL (Italy)
• Machinefabriek Otto Schouten BV (Netherlands)
• Extricom Gmbh (Germany)
• S+S Separation and Sorting Technology (Germany)

RTDs:
• Smithers Rapra & Smithers Pira Limited (UK)
• Fraunhofer-Gesellschaft Zur Foerderung Der Angewandten Forschung E.V (Germany)
• The University of Exeter (UK)
• Comite Europeen de Normalisation, represented by NEN (Belgium)
• Aliplast Spa (Italy)

The project has been successfully and widely disseminated to a large audience and the process and tools developed are ready for exploitation by the SME-AG, their members and the Other Enterprises.

Project Results:
Description of main S & T results/foreground

SuperCleanQ has developed a number of quality control and quality assurance tools and procedures for plastics recycling processes targeted at food contact applications to enable SMEs to conform to Commission Regulation (EC) 282/2008 on recycled plastic materials and articles intended to come into contact with foods. The research work that has been carried out during the course of the SuperCleanQ project has resulted in development of four principal exploitable technologies.
1.Development of an analytical test method for recycled food contact materials (to be published as a CEN standard)
2.Development of a sorting technology for black, highly coloured and multilayer PET
3.Development of a decontamination system for recycling of PET
4.In-line monitoring for processing lines

DEVELOPMENT OF AN ANALYTICAL TEST METHOD FOR RECYCLED FOOD CONTACT MATERIALS
An extensive literature search and discussions with the recycling industry enabled a suite of organic contaminants (‘marker compounds’) to be selected that were representative of both the PET material itself and the substances that it has come into contact with during use. The determination of these substances can be used as a measure of the purity of recycled food grade PET and hence the effectiveness of a recycling process. An analytical technique has been developed and validated for the identification and qualification of six of these marker compounds in PET. This method has been drafted into the form of a CEN Technical Specification and submitted to CEN Technical Committee TC 249 (plastics). This draft CEN Technical Specification has been developed by a working group of CEN 249 and is making good progress towards publication in early 2015.

The availability of such a CEN standard for recycled, food grade PET will provide governing bodies, regulators and industry with the capability to determine the purity of such products in a cost-effective and accurate manner. Being able to obtain such data will provide a number of benefits, such as being able to make a judgement regarding the quality of recycled PET of unknown origin, and whether it has been manufactured using an appropriate food grade recycling process. This will assist in ensuring that recycled PET that is brought on to the market in the EU, whether from outside the EU or by a Member State, is fit for purpose with respect to the manufacture of food contact products such as bottles and trays. In this way it will help protect the health of the population of the EU and provide a safeguard to the business interests of companies working in this recycling field. The development of a CEN deliverable also contributes to the dissemination of the project results through the European standardisation system. A CEN deliverable will represent this support which will considerably increase the sustainability of the research.

DEVELOPMENT OF A SORTING TECHNOLOGY FOR BLACK, HIGHLY COLOURED AND MULTILAYER PET
A range of spectroscopy-based sorting techniques have been evaluated by the SuperCleanQ project for the separation of items in mixed plastic waste streams. This work has specifically targeted the separation of mixed plastic waste streams containing black/highly coloured PET and PET products manufactured using multilayers. The aim of this research was to provide the recycling industry, both that involved with recycling food grade PET and other sectors of the industry, with a new spectroscopy-based technology for the separation of highly coloured (e.g. dark/black) plastic and barrier-modified plastic products. To assess their capabilities four techniques that are available (NIR, IR, Raman spectroscopy and UV/Vis spectroscopy) were evaluated on the following materials:
i.Mixed waste streams containing polymer such as PET, PETG, PE, PP, ABS /SAN or PS
ii.Uncoloured (i.e. neutral) polymer samples and those that were a dark colour
iii.Multilayer plastics and those that contained coatings and certain additives

All four systems showed some promise in certain areas and the results obtained are shown below:
• Near Infrared Spectroscopy (NIR) – The NIR system was capable of identifying multilayer materials and the presence of some additives
• Infrared Spectroscopy (IR) – IR spectroscopy was capable of identifying black plastics, but difficulties arose due to the presence of coatings, dust or humidity in the sample surfaces
• Raman Spectroscopy – Raman spectroscopy can be used to identify the polymer types present, multilayer structures and the presence of additives
• UV-Vis Spectroscopy – The UV-Vis spectroscopy technique was the least successful and can only be used in some minor applications concerning the identification of certain additives. Nevertheless, it can be used for specialist identification applications.

The results obtained from this work have contributed to the scientific knowledge in this area and will assist in the advancement of any further work undertaken. Industry having access to such a sorting system ensures that mixed waste streams are better utilised and recovery rates of all polymers in the EU are improved.

DEVELOPMENT OF A DECONTAMINATION SYSTEM FOR RECYCLING OF PET
The process that has been developed by the SuperCleanQ project is a novel, extruder-based decontamination system to purify contaminated post-consumer PET. This decontamination process is comprised of an innovative degassing/filter system. Within this scheme, a high efficiency purification process has been established which only requires a low quality of a stripping agent, such as carbon dioxide or water. Also, a number of new filter technologies have been evaluated.

The attributes of this system include:
i.Easy to integrate into existing food-grade PET recycling lines to enhance their purification efficiency
ii.Only requires relatively small amounts of stripping agent that have a low toxicity
iii.Volatile organic carbon (VOC) analysis results obtained on the purified PET have shown that it has achieved very good purification results
iv.No evidence has been obtained to suggest that it reduces the molecular weight of the PET, i.e. no depolymerisation-type degradation takes place

This decontamination system has the potential to be exploited in two areas associated with the recycling of food grade PET:
a)As part of a ‘superclean’ process designed to be used in the recycling of relatively uncontaminated PET such as bottles, back into food grade product
b)As part of a ‘superclean’ process targeted at the large amount of PET that is presently regarded as ‘unrecyclable’ because it is highly coloured or modified back into high quality, food grade PET

Enabling more PET to be recycled and used in food-contact applications rather than virgin PET is one of the environmental benefits of the SuperCleanQ project. Growth in the recycled food packaging market will reduce the waste going to landfill and encourage local authorities to put in place extra measures to collect and reprocess food packaging. In addition, SuperCleanQ has the potential to save energy and reduce CO2 emissions through increased levels of PET recycling.

IN-LINE MONITORING SYSTEM FOR PROCESSING LINES
SuperCleanQ has developed a system that uses Near-infrared spectroscopy (NIR) to detect biodegradable contaminants in the process lines (e.g. injection moulding or extrusion) of two food grade plastics for which recycling is most widely practiced at the present time, namely PET and HDPE. Two specific contaminants within the biodegradable class of contaminants have been targeted:
i.Poly(lactic acid) (PLA)
ii.Oxobiodegradable additives (e.g. the stearate carried and catalyst)

Using multivariate analysis and Partial Least Squares Analysis (PLS), chemometric models in the form of calibration curves were constructed from the offline and online calibration data. These successfully showed that the concentration of either PLA or oxobiodegradable additives could be predicted by measuring the infrared spectrum of the melt in the nozzle region during injection moulding. For example, PLA could be detected in concentrations as low as 0.01%. The injection moulding process was also run with in-line NIR to produce inline calibration data covering the same concentration range as for off-line calibration but with a greater number of concentrations.

Linear calibration curves in the range 0.01-1% and 0.07-0.1% were obtained for PLA and in the range 0.1-1% for oxobiodegradable additives. The results obtained also showed that the system was very sensitive to changes in the composition of the polymer melt, thereby demonstrating the principle of providing an early warning of noncompliance in processed recycled polymer. This NIR in-line system can detect degradable contaminants in polymer melt processing streams at concentrations below that which is likely to cause any significant deterioration in the mechanical properties of the PET. The system developed by the project is also capable of detecting other contaminants, such as the marker compounds (i.e. contaminants), limonene and toluene.

The successful development of this technique for in-line detection and measurement of biodegradable contaminants during the processing of PET and HDPE can lead to improved and consistent quality control when processing recycled plastic. The in-line system can also detect other contaminants such as limonene, methyl salicylate, toluene and ethylene glycol, which will improve general confidence in the industry, and by extension society, in the safety of recycled plastic for food use. The new system will provide an early alert to non-compliance in the feedstock during processing, which will provide an economic benefit by reducing both wastage and processing costs.

With regards to its other potential capabilities, the system can also be used to give real-time quality control of polymer additives in plastic compounding and process lines. It can also benefit any industry, such as pharmaceutical industries, with an interest in producing polymers impregnated with specific active compounds, especially where more than one compound is added. There is considerable scope for this technique in these types of applications and end-products.

ADDITIONAL RESULTS
Life Cycle Assessment (LCA) and Life Cycle Costing (LCC) of the SuperCleanQ processes were completed. The LCA and LCC were performed using a combination of publically available data and data provided by the project partners. Two main reports were produced – the first to provide an overview and explanation of the LCA data collated and processed into data sets for the impact to the environment of the SuperCleanQ processes and production steps developed in the project. The second report shows the technical benefits as well as an economic evaluation of the process.

The final ‘Plan for Dissemination and Use of Foreground’ was completed and contains a detailed description of all the exploitation activities undertaken by all the partners. In addition, there is a thorough investigation of the technological and economic potential and value and how the project results can be exploited in each sector. Finally, specific opportunities for the project partners were identified and included in the PUDF.

The results of SuperCleanQ were disseminated to SMEs, Large Enterprises and SME- Associations across Europe and to a wider audience with the aim of marketing the technology and processes developed during the project. Through the dissemination activities the partners were able to gain feedback from their potential customer bases. SuperCleanQ was widely disseminated via: 2 posters, 1 postcard, 8 flyers, 87 events, 13 published articles, 13 press releases and 4 case studies. In addition, the project website (available at www.supercleanq.eu) was regularly updated to reflect the current status of the project. A project video was added to provide visitors with a clear and easy way of finding out more about the project.

Potential Impact:
Potential impact and main dissemination activities and exploitation results

The four technologies developed in SuperCleanQ represent clearly identifiable opportunities for industry to benefit financially. This can occur in a number of ways for example:
a) using the technologies to improve the efficiency with which an existing process operates
b) using the technologies to reduce risk to the business by improving quality assurance procedures
c) improving and increasing capability to increase existing market share
d) moving into a new market via the launch of a new product with novel, high-value capabilities

Indirect ways in which industry could benefit include the enhancement of a company’s standing in the market place due to the adoption of a more rigorous quality assurance process and the maintenance of client relationships.

The four technologies can be viewed as being associated with three broad areas of the recycling process for plastics. These are:
i.The sorting systems that are employed during the earlier stages of material recycling facilities (MRF), or mixed plastic recycling facilities (PRF), to separate products that have been manufactured from different generic plastic types (e.g. PET from PE)
ii.The sophisticated physio-chemical recycling processes which are used to decontaminate the target plastic (e.g. PET) in a waste stream once this has passed through the various segregation, separation and purification steps to remove other plastics and non-plastics, such as metal, textiles, cellulosic material and inorganic material.
iii.The large number and range of quality control and quality assurance processes, systems and methods that are used to ensure that recycled products, materials and articles are fit for purpose in that they are free of contamination. In the context of the SuperCleanQ exploitable results, this contamination in rPET takes a number of forms:
a.Chemical compounds due to the degradation of the PET itself (e.g. acetaldehyde)
b.Chemical compounds due to the substances that the PET has come into contact with during first use (e.g. limonene)
c.Biodegradable polymers, such as PLA
d.Chemical constituents that catalyst the oxobiodegradation of polymers such as polyethylene

The decontamination system that has been developed by the SuperCleanQ project has the potential to be exploited in two areas associated with the recycling of food grade PET:

i.As part of a ‘superclean’ process designed to be used in the recycling of relatively uncontaminated PET, such as bottles, back into food grade product
ii.As part of a ‘superclean’ process targeted at the large amount of PET (7.7 million tonnes) that is presently regarded as ‘unrecyclable’ back into high quality, food grade PET because it is black, blended with other polymers or contains barrier layers, coatings etc.

In addition, the SuperCleanQ analytical method (CEN standard) is a quality control tool that will enable companies, and in particular recyclers, to save money by:

i.Helping to avoid the unnecessary re-application of the far more expensive and disruptive EFSA ‘Challenge Test’ to the complete recycling process
ii.By enabling the detection of poor quality rPET within the recycling facility, and before it leaves the site, this would stop it being supplied to a converter and so prevent a potentially much bigger problem occurring if it was used to manufacture food contact products
iii.By enabling the detection of poor quality rPET granules which have originated from other sources, e.g. those that have been imported into the EU.

With regard to the novel sorting technology, although the work carried out by SuperCleanQ has not resulted in a final, marketable product, the work carried out has contributed to the scientific knowledge in this area which, when brought to a conclusion, will enable companies to make money by:

i. Enabling them to separate and exploit the large quantities of plastic waste, food grade and other types such as WEEE products, that are highly coloured or black and which cannot be separated at present.
ii. Helping them to reduce the amounts of landfill taxes that they pay in EU countries such as the UK
iii. Enabling them to substitute recycled plastic for virgin plastic in a wider range of new products

Finally, SuperCleanQ has developed a system that uses Near-infrared spectroscopy to detect biodegradable contaminants in the two food grade plastics for which recycling is practiced the most frequently at the present time, namely PET and HDPE.

The successful development of this technique for in-line detection and measurement of biodegradable contaminants during the processing of PET and HDPE can lead to improved and consistent quality control when processing recycled plastic. The in-line system can also detect other contaminants such as limonene, methyl salicylate, toluene and ethylene glycol, which will improve general confidence in the industry, and by extension society, in the safety of recycled plastic for food use.

This in-line monitoring system for processing lines will therefore, enable companies to save money by the same types of routes and mechanisms as those described for the SuperCleanQ analytical method (CEN standard) – see above.

In conclusion, the results of SuperCleanQ will allow the beneficiaries to gain entry into this growing and lucrative market, as well as improving their industrial processes and quality control.
The project has been successfully and widely disseminated to a large audience and the tools are ready for exploitation by the partners. Case studies, best practice guides and protocols have been prepared as supporting materials.

DISSEMINATION & EXPLOITATION
Dissemination was an important part of the consortiums’ strategy to widely exploit the results of the project. The dissemination strategy was divided into different stages starting with initial awareness raising through to preparation for exploitation following the project end. All partners contributed to the dissemination efforts and maximised the use of different dissemination channels to ensure the successful future industrial adoption of the SuperCleanQ processes and tools.

Posters, flyers and postcards were made available at the start of the project (and updated regularly throughout) to raise awareness of SuperCleanQ at conferences, exhibitions and workshops.

To support the future exploitation stages, case studies were developed to provide examples of the tools. This was further supported by the production of a project video which was made available via the project website and YouTube. Social media was also exploited and a LinkediN Group set up to promote SuperCleanQ and provide an interactive platform for interested parties.

A detailed market report was prepared as part of D7.2: Final Plan for Dissemination and Use of Foreground and covers market potential and value, growth sectors, future trends and competing technologies of the SuperCleanQ results. This information provides the beneficiaries with supporting data for their organisations and future business planning.

The SuperCleanQ results will support the SME-AGs and Other Enterprises within the project to compete in a growing and increasingly competitive marketplace. Supporting materials such as case studies and a promotional video have been produced to assist with marketing activities, and Best Practice Guides and Protocols written to support with future exploitation. The work carried out in the SuperCleanQ project was led by the SME-AGs who ensured the technical direction of the project.

List of Websites:
The SuperCleanQ website is available at www.supercleanq.eu.

Project Coordinator: Tim Marsden, British Plastics Federation (UK) – tmarsden@bpf.co.uk