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Development of extraction process for removal of pigments and additives for recycling of polymers

Final Report Summary - CLEARPLAST (Development of extraction process for removal of pigments and additives for recycling of polymers)

Executive Summary:
Of the 13.5 million tonnes p.a. of polyethylene (PE), 15% of this production is scrap of which 35% is coloured. Currently, scrap PE is sorted by type and colour for recycling with the coloured scrap being mixed, carbon black added to generate black or grey products of low-value. Today there is no solution available that has the ability to remove pigments and other selected additives from the recycled material. The Clearplast consortium aimed to develop a Pigment Extraction Process unit to quickly and efficiently enable the plastic recycling companies to remove colour pigments and additives from the cleaned and sorted PE from various waste streams. The preferred method to extract the pigments was by Supercritical Fluid (SCF) Extraction, in particular using CO2.

During the first year of the project good technical progress towards a pigment extraction process was made, although the SFE process did not show convincing evidence of being able to extract the required amount of pigments or additives as needed. As a result a more conventional technology based on solvent extraction was investigated.

At the beginning of the second year the consortium carried out extensive research into alternative scientific and technical approaches to extract pigments and additives without success. In July 2010 the Project Officer (PO) suspended the project, and following the bankruptcy of the coordinator Per Haagensen AS the project was formally terminated in September 2010.

Due to the scientific and technical problems encountered and failure to achieve practical solutions in WP2 on developing extraction technologies, the consortium was unable to complete WP4 (system integration), WP5 (industrial validation) and the patenting, future funding and exploitation planning set out in WP6 (Innovation-related activities).

Project Context and Objectives:
Project Context

Production of PE in Western Europe alone is 13.5 million tonnes p.a. The waste PE from this production is 15% scrap of which 35% is coloured; creating 709 000 tons of off-specification material. Currently, collected polyethylene is recycled by mechanical recycling requiring collection, cleaning and sorting by polymer type and colour. Coloured plastics are usually mixed and carbon black is added to get black or grey plastic for use in narrow range of applications and low-value products. As of today, there is no technical solution available that has the ability to remove pigments and other selected additives from the recycled material. The prospect of a technology enabling removal of pigments and selected additives from scrap opens up a range of possibilities in terms of quality of, and applications for recycled material. In addition, it would have a large impact on the need for virgin material and thus, raw material consumption. Among the drivers are European Commission directives such as 2004/12/EC Packaging and packaging waste, in addition to the strategy on prevention and recycling of waste. Today, China is a large player on the scrap market, buying enormous volumes. China has reduced imports of virgin resin by importing recycled and scrap polymer, increasing the amount of domestic recycling. China is the world’s largest polyethylene customer, importing 5.65 tonnes in 2005, which was well below expectations due to the imports of recycled and scrap polymer. By increasing quality and value of scrap material, less will be exported to China, forcing China to buy virgin at higher price, increasing the competitiveness of European Recyclers by producing recycled material of higher quality.

Objectives

As of today, there is no technical solution available that has the ability to remove pigments and performance enhancing additives from recycled polyethylene to a base material purity that enables it to be re-compounded as an uncontaminated (with additives and pigments) material that can be blended to specific colours and mechanical performance through the reintroduction of specific additives and pigments at specific and accurate compositions.

At the beginning of the project the consortium aimed to develop a simple to use and highly automated additive extraction system that was sufficiently low in cost so as to enable at least 10% of recycling and compounding firms to install it and produce higher value recyclate. This would help the consortium to move into the knowledge based economy through the protectable knowledge (IPR) generated and the subsequent sales of licenses to install and operate such a system. The target for the project participants was to distribute the extraction process to 10% of the SME plastic recyclers during five years after project completion; estimating a turnover of €100M in 2014. There was also a major legislative driver for the project via Directive 2004/12/EC which provided that the Member States should take measures to prevent the formation of packaging waste and encouraged the reuse of packaging. In addition a new strategy on prevention and recycling of waste was proposed by the EC 21.12.2005. This strategy was one of seven thematic strategies programmed by 6th Environmental Action Plan and the EC proposed a revision of the Waste Framework Directive to focus on improving the way resources were used by introducing the life-cycle approach into waste policy and developing waste prevention programs. Another relevant directive was 2000/53/EC on end-of-life vehicles (ELV Directive) with a target of 85% of reuse and recovery, with targets of 80% of reuse and recycling by 1 January 2006, and 95% of reuse and recovery and 85% of reuse and recycling by 1 January 2015.

The overall Project Objective was to develop a Pigment Extraction Process unit to quickly and efficiently enable the plastic recycling companies to remove colour pigments and additives from the cleaned and sorted PE supplied by municipal waste management companies and industrial PE waste. The preferred method to extract the pigments was by Supercritical Fluid (SCF) Extraction, in particular using CO2. Application of Supercritical Fluid Extraction (SFE) had been used for removing polymer additive samples from polyethylene. However, a process of extracting colour pigments had not been developed and industrialized. Due to the fact that scCO2 today was utilized for adding pigments to polymers, and because it was possible to remove additives by SFE, the consortium believed that SFE was a promising method for removal of colour pigments in polyethylene also. Alternative extraction methods based on more conventional technology, such as solvent assisted recrystallisation and filtration, were to be considered as well and evaluated together with SFE before a final decision is taken based on factors such as the ability to industrialise, cost and environmental impact. The following extraction process based on SFE was proposed (see attached diagram).

The proposed prototype would be able to process 20kg/hr of material and would be directly scalable to an output of 140kg/hr. The specific technical specification for the prototype system to remove pigments and additives resulting in clear polyethylene were as follows:

• A time per batch of less than 30 minutes and processing volume of 20 kg/hour
• An ability to be scaled up to 140kg/h and with a capital purchase cost of less than €200k
• A separation process cost of less than €400/tonne PE at140kg/h output
• An additive re-compounding and pigmenting cost of €100/tonne at140kg/h output
• A quality and consistency of colour and mechanical/physical/thermal performance of that yields a sales price of the recycled PE material of €1090/tonne




Project Results:
Description of Main S & T Results/Foregrounds

During the first year of the project focused on achieving the scientific objectives and on collecting relevant data and information on the recyclates targeted in the project. It also prioritized work towards a ‘proof of principle’ technical study, trying different extraction parameters for SFE, as well as pigment removal from the surfaces of plastics. Good technical progress towards a pigment extraction process was made, even though the SFE process did not show convincing evidence of being able to extract the required amount of pigments or additives as needed. Instead, a more conventional technology based on solvent extraction was investigated and the initial results led to an early patent application by the consortium to be explored.

At the end of Reporting Period 1 (RP1) the main achievements in the project were:
• A method for removing surface deposited pigments onto PE was established.
• A recrystallisation based extraction process for organic pigments in PE was established.
• Work towards a universal pigment type extraction process based on filtration was initiated.
• A method for extraction of inorganic pigments in an acidic solvent was established and a patent application was started.

In addition, software algorithms for process control systems, a prototype of sensing and control systems and a control system for the SPE process were established and reported (combined deliverables D3.1 3.2 and 3.3)

A Consortium Agreement was signed and submitted and a website established (reported in D6.1)

In the second year of the project, the consortium addressed its failure to remove colour pigments from PE using the initial SFE process. In a new deliverable report (D2.4) the consortium reported on its investigations into possible alternative methods for extracting pigments from PE scrap.

The work focussed on:
• Developing new parameters for the SFE process, using supercritical CO2
• Adapting the SFE process to try different supercritical solvents
• Using physiochemical techniques based on high pressure and high temperature filtration.
• Using surfactants to agglomerate the pigments

Unfortunately, none of the alternative techniques (as follows) showed any promise.

• A revised set of parameters for the sc-CO2 extraction showed no improvement in results. Using C2F6 and n-butanol produced practical improvement in extraction. As these alternative solvents were expensive, they offered no practical alternative for the project.
• Using high pressure and high temperature filtration led to some improvement in extraction, resulting in the removal of a significant fraction of carbon black and other filler particles. However, substantial fractions of these substances were not blocked by the filters used in this study and the consortium considered the grey material produced was of little added value to the recycled plastics sector.
• Several attempts to agglomerate carbon black with a variety of surfactants, the addition of polymers and grafting with maleic anhydride were unsuccessful. If such an agglomeration had been achieved, separation of carbon black by melt filtration would have been possible.

A literature review and discussions with electrical engineering experts highlighted electrical field agglomeration as an avenue for further study. However, this promising lead was not investigated.

The project was suspended on 12 July 2010 (Month 20) by the Project Officer, due to concerns about its technical direction. The Coordinator was informed but this information did not pass to the consortium. In August, the Coordinator (Per Haagensen AS) filed for bankruptcy. As messages were returned unanswered, the Project Officer terminated the project on 16th November 2010 (Month 24 - although according the REA, the formal termination dates from 4th September 2010 – the date of formal notification).

On 2nd November 2011, RTD partner Nor-Tek was nominated as Coordinator, after a majority vote of partners. On 25th January 2012, a formal Request for Amendment to the contract was sent to REA, asking for this change to be formalised to allow completion of reporting up to the point of project termination. In April 2014 a letter from the REA was sent out to partners informing them that the decision had been made not to accept this amendment due to the date the project had finished (31 October 2010), the situation of poor performance not resolved and termination of the grant agreement. REA requested in this letter, that the consortium appoint ,within the consortium, someone to take over the role of primary coordinator contact in order to complete the final reporting process. Getting hold of all concerned partners took some time but by the end of June 2014 most beneficiaries had been contacted and had appointed Nor-Tek's LEAR, Ian Claris, for this role. Although the summer holiday period may slow down the process, the aim is to submit completed outstanding reports and cost claims as quickly as possible with Nor-Tek keeping the EC informed on progress.

Due to the scientific and technical problems encountered and failure to achieve practical solutions in WP2 on developing extraction technologies, the consortium was unable to complete WP4 (system integration), WP5 (industrial validation) and the patenting, future funding and exploitation planning set out in WP6 (Innovation-related activities).

Potential Impact:
Project impact:

The expected final results were to have a system in place to remove pigment from PE and a working prototype for the partners to develop further. The project would have had a strong impact on the SME participants by increasing their competitive position, increase their profit and allowing them to expand their markets by participating in the supply chain for a brand new and higher value range of colour matched PE recyclates. In addition their increased profit would go beyond the process sale of this improved material itself, as it will allow them to move towards knowledge based economy through the creation, protection and sale of IPR related to the plant design and control.

The recycling market is increasing due to improved infrastructures on collection and sorting from municipal waste sources driven by directives and more focus on environmental problems on a political level in towns and cities. Mechanical recycling of plastics waste increased by 11.3 % between 2001 and 2002, with a similar increase in 2002, maintaining the mechanical recycling rate of about 14% in 2003. The post-use consumer PE waste sorted by local authorities or sub-contracted waste management services from municipal sources is 1.8M tonnes/pa. Currently most of this is reground into multi-coloured recyclate then re-compounded/extruded into pellets with the addition of carbon black and a number of performance enhancing additives, notably to increase MFI (Melt-Flow-Index). The value of this material, which has variable mechanical and physical properties and is only available in black and grey, is around €1050 per tonne, compared to €1200 per tonne for virgin.

After the end of the project, Per Haagensen and the further licensee recyclers had planned to build a database of additive and pigment formulations to develop a range of PE recyclate approximations to specific PE virgin grades. As the early part of the project progressed, market research with the moulders and extruders in the project and with their colleague processors (through the Danish Plastics Federation and the British Plastics Federation) led the consortium to the conclusion that the specially compounded grades of ClearPlast recyclate would achieve a process price of €400 per tonne by 2012. With a supply base of 20 European municipal waste management organisations, networked by Grønt Punkt through the European Association of Plastics and Recycling (EPRO), 14 waste management companies, the consortium believed it could have access to around 94 500 tonnes per annum and at the forecast sales price of €1100/tonne. A market of €104M per annum by 2012 was projected.

The final economic benefit that would have been provided by the project relates to the cost savings made by moulders and extruders who use the high-quality ClearPlast recyclate to reduce their purchase of virgin materials. Based on the price difference between virgin at €1200/tonne and ClearPlast at €1100/tonne on the forecast sales of 94 500 tonnes/pa, these savings would have amounted to €9.4M pa for moulders and extruders. The totals costs of recycling cost for ClearPlast process were estimated at €930/tonne and so with a market price of €1100/tonne this would have led to a profit margin of about 15% for the recyclers.

Hence, the total economic impact of the project would have been the sum of the sales in ClearPlast recyclate for the recyclers and distributors plus the costs savings made by the end users as they used it to reduce their virgin material costs. This was predicted to have amounted to €133M/pa by 2012, with an additional €16M of plant sales by the same year.

List of Websites:
Consortium members:

Beneficiary: Short name:
1. Per Haagensen AS (Coordinator) PHaag
2. Atecsol Soldaduras, S.L. Atecsol
3. PG Instruments Ltd PGI
4. SAGA Automatización Industrial S.L. SAGA
5. Plasticos Torrijos PT
6. A-Fax Ltd A-Fax
7. Grønt Punkt Norge AS GPN
8. Nor-Tek Teknologisenter AS Nor-Tek
9. Association pour la Recherche et le Développement des Méthodes et Processus Industriels (Armines) Armines

Project website:
This publishable summary and other public information about the ClearPlast project can be found on the website: http://www.clearplast.net