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FP7

FLHEA Report Summary

Project reference: 613971
Funded under: FP7-KBBE

Final Report Summary - FLHEA (FLAX AND HEMP ADVANCED FIBER BASED COMPOSITES)

Executive Summary:
Packaging application is the greatest sector for the plastics industry in Europe. One of the main challenges in this industry is the control of wastes after use. In order to reduce the environmental load generated from the disposal of used plastic materials, a growing interest has been focused on biodegradable polymers based materials. However, the use of biodegradable films for food packaging has been strongly limited because of the poor barrier properties and weak mechanical properties shown by natural polymers. A possible strategy to increase its properties is the development of fibre-based biocomposites. In this sense, natural fibres represent an interesting profitable substrate, being most of them plant fibres. Although the demand for natural fibers is growing worldwide and its price is increasing, annual plants such as jute, sisal, kenaf, flax or hemp require further development to provide novel products with improved properties.
The development of FLHEA project has provided a novel range of surface modified reinforcements. The project has been focused on the upscaling and modification of micro/nanoreinforcements based in hemp and flax, and its subsequent processing to obtain composites with improved properties. Extruded sheets have been performed and subsequently thermoforming of food packaging trays. Flax and hemp fibres were selected because their high cellulose contents together with a low lignin content to provide a faster processing route for the isolation for cellulose micro/nanofibres (CMF/CNF) and the extraction of crystalline cellulose regions, as cellulose nanowhiskers (CNW). Different processing routes have been evaluated in order to provide a completely renewable and biodegradable compound based on surface modified nanofibres for packaging applications.
Works carried out in FLHEA project have consisted in developing methods for easy handling and manipulation of cellulose fibres. From these fibres, nanocrystalline cellulose fractions were isolated and chemically modified in order to increase the interaction with the hydrophobic polymer matrices and also to prevent the agglomeration during compounding. Once compounding process parameters were optimized to assure the desired distribution of the reinforcing phase in the polymeric matrix, co-extruded sheets were performed at pilot scale. Industrial up-scaling have been also carried out for thermoforming final trays.

Project Context and Objectives:
Context
Flax and hemp have been used since centuries ago, and have become agricultural commodities cultivated for its application on a wide range of products such as long fibres for fabric, short fibres for paper or felt; seeds and oils for livestock feed, or use as compost, among others. These crops represent an important area on European agricultural sector. According to CELC, 81.300 hectares of flax fibre were cultivated in 2014 on Europe amounting to 80% of the world’s production, accounting for 12.000 direct jobs. China is among the largest producing and exporting countries of hemp textiles and related products, while European Union (EU) has an active hemp market, with production in most member nations.
However, there is a need to develop novel products to offer a differentiated and competitive product as a result of globalised economies. Flax and hemp have been used on the development of bio-composites, leading to innovative new applications and opportunities for these industries. The advantages of flax and hemp reinforcements are based on the development of lower weight and enhanced properties composite materials. During the last years the development of nanocomposites, has led to a novel field of material development. These materials have reinforcements with at least one dimension is below 100 nm, leading to enhanced or novel properties compared to conventional composites reinforcements.
In Europe, packaging applications are the largest application sector for the plastics industry and represent 39.6% of the total plastics demand, which was around 46.3 Mton on 2013, according to latest Plastics Europe analysis. From post-consumer waste, 62% was recovered through recycling and energy recovery processes while 38% still went to landfill. Bioplastics can offer a potential alternative to conventional plastics, based on oil. According to European Bioplastics, about 75 percent of bioplastics will be produced in Asia by 2018. Europe will play its role mainly on research and development, and production capacity will be around 8% worldwide.
However, bioplastic properties or performance are usually below its oil counterparts, and therefore, nanocomposites may offer a potentially applicable route to improve properties.
FLHEA Project scope has been based on the implementation of a technical approach to the upscaling of composites, and specifically, to cellulose-based nanocomposites. This research is based on a previous Project development (Traysrenew), and has been focused on the increase of cellulose isolation and nanowhiskers yield, its modification to enhance compatibility to polymeric matrices, and the production and evaluation of parts at industrial scale.

Objective
The main objective of FLHEA project is the development of industrial scaled-up processes to obtain modified cellulose nanowhiskers, for the development of biocomposites with improved properties to perform thermoformed trays for food packaging applications.
This scope will assure the development of biodegradable fibre-based composites ready for the use and commercialization on packaging industry. FLHEA industrial process will be high-throughput, environmental, and energetic and cost efficient.

Project Results:
The performance of FLHEA project has achieved to develop a completely renewable and biodegradable compound based in surface modified nanofibres derived from bast fibres. A homogeneous composite material based on fibres has been performed and it is suitable for packaging applications.
Some specific objectives have been implied and reached in Flhea project development:
• Improve extraction steps of cellulose fraction in bast fibres:
The most adequate raw material has been selected for cellulose extraction and purification. It has been obtained cellulose with low lignin content.
• Nanoreinforcements isolation. Mechanisms to be considered:
The upscaling of the NCC manufacturing by evaluating different purification and isolation techniques have been optimized.
• Enhancement of matrix-fibre interface:
Successfully reached by introducing chemical modifiers in nanocellulose surface. Besides, optimizations of drying techniques and plasticizers addition in composite formulations have been performed.
• To develop a cost effective technology to obtain cellulose from hemp and flax natural fibres:
The most effective method for cellulose pulp drying and storage has been developed.
• Design of a optimised production scheme for nanoreinforcements:
An up-scaling process has been optimized reaching maximum yield, minimum water and energy consumption.
• Adjustment of surface modification reactions:
Different chemical modifiers have been used for optimizing the interface fibre-matrix.
• To develop a sustainable composite material with optimal mechanical, thermal and barrier properties for food packaging applications:
Several PLA based composites have been successfully processed and evaluated for being suitable in food packaging applications.

These objectives have been successfully achieved through the application of different approaches. It has been considered as multiple developments, in which the final product is affected also by the surface modification of cellulose nanofibres and their introduction with different biodegradable polymer matrices.
Work developed within the project has involved a four step approach. First it was to extract and purify cellulose and after nanocrystals were isolated. The second part aimed the study about chemical modifiers for selecting the most appropriate in order to increase the interaction with the hydrophobic polymer matrices. On a third stage, compounding process for introducing modified nanocellulose within PLA and starch-based polymers was optimized at lab and pilot scales. Finally, main efforts were devoted to carry out the implementation at industrial scale for obtaining coextruded sheets and thermoformed trays suitable for food packaging applications.

Below it is presented the main technological results and foregrounds achieved in each work package of the development of the project:

WP1- “CELULOSE PURIFICATION AND ISOLATION”
This work package (WP1) was focused on the selection of the most adequate raw material, cellulose extraction and purification. It was reached and the proposed target was also fulfilled, by obtaining cellulose with the minimum lignin content than possible.
During the development of this work package, large amount of raw materials supplied by Arctic Fiber Company Ltd. were processed to produce bleached cellulose pulp for WP2. For this purpose the optimized sequence reported in deliverable D1.2 was used. The best results in term of cellulose content were obtained with enzymatic-retted flax that presented the major descent in lignin from the raw material (7.6 to 3.15%). Enzymatic retted flax fibres presented diameter value of 19.83 μm and length with values around 300 μm.
In addition, a very effective method for cellulose pulp drying and storage has been developed. In one of the submitted deliverables a brief overview of different drying techniques has been provided, with a special focus on those techniques applied at industrial level and on conventional pulp mills. Among the screened techniques, flash drying provides the tool for a high output product that can be applied in the project development.
The major findings were as follows:
• All raw materials supplied by Arctic Fiber Company Ltd. presented high content of cellulose and low content of lignin.
• The bleached pulps presented less proportion of phenolic compound than commercial cellulose and produced mainly for decomposition of cellulose.
• Different available drying technologies were identified.
• The advantage and inconvenient of these technologies for cellulose pulp drying were identified.
• Impact of the drying on the properties of cellulose was identified.
• Flash drying was selected as the most adapted technology for the project.

WP2- “MICRO/NANOFIBRE UP-SCALING”
This work package was focused on isolation and production of Nano Crystalline Cellulose (NCC or CNC) from purified hemp and flax fibers. The main aim was to optimize the upscaling of the NCC manufacturing by evaluating different purification and isolation techniques.
During the first period of the project, the work carried out was concentrated in improving the NCC production yield obtained in Traysrenew project. Then, during the second period of WP2, the work was focused on the final step in the NCC production-washing of the suspension, in order to improve the total yield.
With this project development, production conditions of NCC from bleached flax and hemp at pilot scale were optimized. Finally, higher production yield was obtained by using Melodea’s protocol in which some optimization was performed to Flhea development project. Also an optimization of lab pilot scale production, in terms on reducing energy and water consumption, has been performed.
Some analyses were performed in both gel and dry form of NCC, produced from flax and hemp such as: Transmission electron microscopy (TEM), Scanning Electron Microscopy (SEM), Atomic Force Microscopy (AFM), Thermogravimetric analysis (TGA), Fourier transformed infrared spectroscopy (FTIR), Rheology measurements. These analyses served as tools to improve the NCC production in order to obtain high solids content solution or powdered material through drying for the next stage in the process in which the nano crystals are modified, pumped and extruded. To optimize the NCC form needed for applying surface modification, different forms of NCC were delivered for testing by Organoclick AB.
Since flax fibers have a significant higher α-cellulose content compare to hemp, they were a preferable candidate to produce NCC in pilot scale and gain by that a higher production capacity and therefore more cost effective compare to hemp.
The main target of this work package was established, and NCC production yield compare to Traysrenew (less than 30%) was improved significantly. The average yield obtained by Melodea up scaled production is 65.4±3.7%.
More than 54 litres of NCC suspension were prepared and delivered for the following step in the process, surface modification implementation.
As well as isolated nanocrystals were prepared for subsequent chemical modification, these samples were evaluated by different drying methods, and the most applicable ones were based on spray drying. Spray drying is a widely used industrial process for particle formation and drying. This technique is suited for a continuous production of dry solids in powder or agglomerated particles form from a liquid feedstock, providing precise quality standards such as particle size distribution, residual moisture content, bulk density and particle morphology. The drying proceeds until the desired moisture content is reached in the sprayed particles and the product is then separated from the air. Different parameters were optimized and average yield obtained increased from 62 to 86%.

WP3- “CELLULOSE MICRO/NANOFIBRES MODIFICATION”
The three different surface modifications of nanocellulose have been the introduction of a primary alkylamine (APTES), biopolymer based complex (PEC) and vinyl functional groups. These types of modifications have successfully conducted by finding FDA approved chemicals, reactive enough and with an acceptable economy to modify acidic non-sonicated flax nanocellulose.
After optimization of the reaction conditions the time was spent on scaling up the reactions from 10 gram scale to 100 gram scale and subsequently to 200 gram scale dry modified nanocellulose.
The modified nanocellulose films have been evaluated using contact angle measurements (40-90°) and FTIR analysis. Additionally, suitable scaled up conditions have been identified and successfully synthesized to obtain ∽1.5 kg dry modified nanocellulose. The products were delivered for the evaluation of drying procedures and also the compatibility with the polymeric matrix.
An adjustment on CNW spray drying process has been evaluated to reduce remaining moisture in dried particles and also to increase production yield. Once spray drying parameters were optimized, samples of modified CNW suspensions supplied by Organoclick were spray dried and subsequently characterized.
An alternative route of spray drying technique has been proposed and developed in this project to provide a suitable route to improve handling. The use of carrier systems has been evaluated to provide a valuable alternative to decrease the energetic requirements and potential aggregation of fibers. Such carriers should be compatible with selected polymeric matrices to enhance the composite properties

WP4- “FIBRE COMPOSITE PROCESSING”
After evaluating different strategies, finally two processing routes has been defined to introduce cellulose nanowhiskers in PLA and STARCH matrices. One of them consists on spray-drying process to obtain CNW in powder shape. The other alternative is the use of a plasticizer as a carrier to introduce CNW in polymer matrix. Once PLA and STARCH based composites were processed, mechanical, thermal and barrier properties have been evaluated, and then the best formulation to develop required composites was selected.
Regarding PLA matrices, composite manufacturing has been achieved through twin screw processing, based on the dispersion of modified cellulose nanowhiskers on a plasticizer that will act as a carrier besides its effect on polymer properties.
Respecting bio based starch-PLA polymers, some matrices were evaluated and then different cellulose dispersions were added through twin screw processing.

WP5- “FINAL PACKAGING VALIDATION”
Processing parameters have been adjusted to provide improved dispersion of cellulose nanowhiskers on the polymeric matrices, leading to optimized composites. Coextruded PLA sheets have been successful developed and subsequently thermoformed at pilot and industrial scale. It has been demonstrated the viability of thermoforming the new materials by processing trays with two different depth.
In this work package an extend analysis has been carried out in up-scaled materials and also in final developed packaging. Transparency, thermal and mechanical properties have been studied, and also a food contact evaluation has been done.
The main conclusions obtained from these analyses are summarized below:
• An increase in crystallinity degree of PLA containing modified nanocellulose is observed due to its nucleating effect.
• Developed trays have been subjected to compression test and an increase on the range of 100% in stiffness was determined in higher depth trays when mCNW was added. In case of low depth trays, the effect on mechanical properties was not as high when nanofibres are included in composites; nevertheless it is shown an increase around 60%.
• The introduction of modified CNW in PLA matrix containing plasticizer produces an increase around 30% in oxygen barrier properties.
• The materials employed in the Flhea project fulfil the requirements of the Plastic Regulation (UE) 10/2011 concerning composition.

Potential Impact:
• Potential impact, exploitation
At present, the looming effects of climate change have resulted in a renewed interest in materials derived from natural resources, like natural fibers. Although the demand for natural fibers is growing worldwide and its price is increasing, annual plants such as jute, sisal, flax or hemp require further development to provide novel products with improved properties.
Packaging industry has a huge interest in reducing packaging materials and associated wastes, biodegradable materials have been evaluated for this application. There is no larger market segment in the plastics industry than the packaging segment. More than a third of all plastics are transformed into packaging, approximately 100 million tones worldwide. In industrialized countries such as the United States or the European Union, 50 percent of all goods are packaged in plastics.
However, the use of biodegradable materials for food packaging has been strongly limited because of the poor barrier properties and weak mechanical properties shown by natural polymers.
The packaging industry needs advanced technical material properties and functionalities in order to achieve benefits such as increasing product attractiveness due mainly to its biodegradability, development of additional and new market applications, more competitive solutions than other competitors in the market and potential cost reduction.

➢ Our innovative solution
The use of nanocellulose materials reinforced by natural fibers in packaging is the major technological advancement in the improvement of properties in current packaging materials for market applications. Therefore, FLHEA project is an opportunity to compete in the PLA packaging market addressing main challenges of the packaging industry, first improving properties and second saving costs.
FLHEA Project proposes the development of industrial scaled-up processes to obtain modified cellulose nanofibres for the development of biocomposites with improved properties. This technology, demonstrated in the research project-TRAYSRENEW, will enable to commercialize the first sustainable food package with suitable mechanical and barrier properties that will open new market applications and represent a solution for the packaging industry.
The potential impact on technical innovation and business competitive advantages are listed as shown:
• The use of renewable and biodegradable material.
• Sustainable composite material with optimal properties: thermal, mechanical and barrier properties.
• Product differentiation: composite material from natural fibers, compared to neat material.
• Cost-effective technology.
• Better packaging solution that avoids food waste. This point could be a condition in future commercial contracts.
• New market opportunities by having a new and differentiate product in the portfolio.
• The new package improves consumer perception (increase the sales).
• To improve sustainability image (brand recognition) due to the reduction of food waste.

➢ The attractiveness of the target market
A market analysis has been performed considering three types of markets: provider (cellulose nanofibers), competitive (PLA market) and end-use (Poultry meat) market.
• Provider market: Cellulose nanofibers
Global revenues for nanofiber-enabled products were an estimated US$382.1 million in 2011, growing to around $852.3 million by 2017. Main markets for polymer nanofibers are in air and water filtration, composites and textiles. Global market potential of cellulose nanomaterials is expected to reach 35 million metric tons. The applications having the most important increase in volume of cellulose nanomaterials are paper and packaging.
• Competitive market: PLA market
According to Grand View Research, Inc., global PLA market is expected to reach 1,205 ktons and $4,312 million by 2020, growing at a rate of 18.8%. PLA demand for packaging products accounted for 59.6% of the overall PLA market in 2013 and is expected to remain the relevant application segment over the years. Among the application segment, food and beverage packaging held the largest market share.
• End-use market: Poultry Meat Industry
The poultry meat is one of the fastest growing meat sectors in terms of production and consumption. In 2013, the global poultry meat production reached 108 million tonnes and it is estimated to be worth over 128 million tonnes in 2022, growing at a rate of 2% each year from 2013. The North American region contributed to the global poultry meat production with 18.9 million tonnes in 2013, growing at a rate of 1.7% each year and the European meat production is expected to reach 13 million tonnes at a rate of 0.8% per year. Other countries contributing to the growth of global poultry meat production are Brazil, and China.
This favorable market as well as the innovation factor provides a very positive scenario for the FLHEA project.

Economic Impact of the BusinessThe European market considered for this business is the fresh packaged poultry market. According to Organisation for Economic Cooperation and Development (OECD) and Food and Agriculture Organisation of the United Nations (FAO) projections, the potential market size is 6,100 million of trays for the first year in the European poultry meat packaging market. Taking a conservative market share, the targeted packaging with reinforcements for poultry tray market will reach over 300 million.
Furthermore and according to the Smithers Pira report, around one-third of the fresh food consumed is packaged. Nevertheless, there has been an increase in the proportion of packaged fresh food, largely as a result of consumer demand for convenience and the growing influence of major food retailers. Different countries have very different packaged shares. The highest packaged shares tend to be in northern Europe, particularly Germany and the UK, and the lowest shares are in southern, central and Eastern Europe.
This business will allow gaining a strong position in a growing European market and will provide a high economic impact to the partners involved. Companies see a great opportunity to increase their economic benefits with the new solution. To highlight this impact, the total expected sales are expected to grow sharply, the profit generated will reach €5M in 2021, with a Net Present Value (NPV) of €8.4M. This is a high profitability business, estimated with an Internal Rate Return (IRR) of 74%.
• In order to reach these ambitious economic objectives, a global commercial and marketing plan has been designed with the necessary activities to make possible the business. In this sense, this plan has been designed in two phases, the first one will introduce the compound developed from FLHEA into the market and the second one will sell the trays made of the compound from FLHEA for the poultry sector. Specifically, there have been defined three key activities to reach this profitable and sustainable business: Direct sales by means of an own sales force who will be responsible for introducing the solution into the European market. The introduction of the new solution will be made in a gradual way. Once the business has been introduced in Europe, distributors will promote it in the USA. Commercial agreements will be reached with top large companies in the field of interest. The selection will be based on their ability to effectively distribute the product.
• The key strategic partners: to effectively exploit this business model are lead companies of the business value chain (poultry producers, retailers, compounders). There have been already contacted with these potential partners taking advantage of our existing contacts and distributors. These first companies have been expressed their interest and will be the first companies to test the solution and create demand for the poultry trays made of the compound from FLHEA.
Professional Association and Trade fairs: Sales activities will also be supported by dissemination actions such as main trade fairs and/or sectorial conferences in food packaging as exhibitor and/or visitant. Besides, it will include specific website, leaflets, brochures, technical dossiers, samples to present the product, and specific commercial material support: training material for sales people and in-situ demo trials for companies. Some of the main trade fairs and associations to promote the new solution are Interpack, Hispack & BTA, IFE, Emballage and Packnet

List of Websites:
http://www.flhea.eu/

Contact

Viñas Ruiz, Ana (Administration Responsible)
Tel.: +34961820113
E-mail
Record Number: 182269 / Last updated on: 2016-05-13
Information source: SESAM