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Life Integrated Process for the Enzymatic Splitting of triglycerides

Periodic Reporting for period 4 - LIPES (Life Integrated Process for the Enzymatic Splitting of triglycerides)

Reporting period: 2021-01-01 to 2021-12-31

The LIPES project was dedicated to reaching the first market replication of an innovative production process leading to greener and healthier fatty acids. The LIPES approach involved an enzymatic process as an environmentally friendly alternative to the current thermal hydrolysis and saponification production routes. Its objectives were to lead to the creation of high purity bio-based intermediates and end products from vegetable oils and fats.

The overall objectives of the LIPES project were :
- To perform the scale-up to pre-industrial level of a new, economically viable and environmentally friendly alternative process leading to higher quality fatty acids and derivatives, therefore widening their range of application
- To optimise resource efficiency with a minimum saving of 45% water consumption, 70% of enzymes and 80% of energetic consumption over traditional processes
- To contribute to reaching the EC goals on waste reduction by elaborating and evaluating new value chains for making use of agricultural co-products

During this reported period, the LIPES project delivered on the operation of the demo unit for the enzymatic hydrolysis process in continuous mode through a series of modifications to the process and installation. Demo trials have led to the hydrolysis of 55 tons of sunflower and high oleic sunflower oil (crude and refined) and 10 tons of rapeseed oil to specifications. Overall, optimisations and adaptations of equipment have led to less failures and for longer periods of time in continuous mode, i.e. to an overall better process control of the demo unit. On castor oil hydrolysis, 95% hydrolysis could finally be reached, but still with a high enzyme consumption and therefore a high cost; this is leading to further investigations. In parallel, OLEON, STC and TUB set the basis for a flagship unit for the enzymatic hydrolysis of high oleic oils (rape, sunflower, linseed, soybean) and the size of the required unit was determined; a basic design of the flagship unit and a first budget have been estimated.

Synthesis and evaluation of esters from enzymatically produced fatty acids was performed. A series of esters: polyglycerol polyricinoleate, glycerol monooleate, trimethylolpropane trioleate were synthesised, characterised and favorably evaluated respectively in food, cosmetic and lubricant applications in comparison with the reference ingredients manufactured from fatty acids obtained through the classical hydrolysis route involving the thermal hydrolysis process. Polymerisation of hydrogenated dimer fatty acid produced from enzymatically hydrolysed fatty acids was attempted but did not reach the targeted melt viscosity. Nevertheless, conditions of the polymerisation process itself could be optimised and in addition to this, efforts have been targeted to improve the process mixing equipment.

Finally, training activities took place during the course of the last period at Maastricht University and although the organisation of dissemination activities has been greatly impacted by the COVID 19 sanitary crisis, a project day event has been organised alongside the BIOKET international conference held in March 2021 to present the outcomes of the LIPES project to a wide audience.
Demonstration of a new sustainable process in mild conditions: the enzymatic hydrolysis of lipids to fatty acids (then derivatization to dimer chemical intermediates, esters and polymer end-products) was performed according to the nature of the raw materials involved, as their different structure greatly influence reaction parameters.

Two main sets of results have therefore been achieved on the enzymatic hydrolysis of vegetable oils :

- enzymatic hydrolysis of sunflower and rapeseed oils: efforts have led to the production at demo scale of 65 tons of fatty acid intermediates (rapeseed and (high oleic)sunflower oils). Data collected during these operations have led to process and equipment modifications to further improve the competitivity of the process that already allows to reach 95%+ conversion. In parallel, ester and dimer fatty acids have been produced at demo scale to further evaluate end product performances.

- enzymatic hydrolysis of castor oil leading to ricinoleic acid: an enzyme leading to the expected conversion yields has been identified and selected. Demo scale runs could not take place as planned during the course of the LIPES project as greater optimization work was required; a first demo scale run is expected during the course of 2022.

A new enzymatic hydrolysis process operating under mild conditions has therefore been developed. This has led to the design and the construction of a new demo plant, which is now operating in continuous mode and modified in line with supporting studies carried out by project partners to develop an economically viable process.

- selection and production of efficient enzymes: specific enzymes have been developed by Biocatalysts for the hydrolysis of different vegetable oils to produce high quality products. Biocatalysts is now ready to produce the enzyme using a large scale production process.

- first market introduction of higher quality and healthier products: achieved work led to the expected environmental benefits as the developed process operates at low temperature compared to the thermal process, LCA shows a significantly reduced carbon footprint.

Additionnally, it led to the expected improved quality as no neo-formed trans fatty acids are generated when fatty acids are enzymatically produced, contrarily to what is observed when the thermal process is run. And finally, efforts showed a positive impact on end-product stability in food and cosmetic formulations when a difference is observed.

The LIPES technology is expected to be industrially exploited by OLEON. An outline of project results is also available on the website and will be disseminated during the course of 2022 to a wide range of stakeholders with an interest in the LIPES technology thanks to the efforts of the IAR (Bioeconomy for change) competitivity cluster.
Progress beyond the state of the art at the end of the project is explained in line with initially stated challenges:

1. Enzyme: Operational stability of the selected enzyme and development of commercially shear stable enzyme achieved

2. Free Fatty Acid enzymatically produced: Demo scale production of zero trans free fatty acids from high oleic oils achieved: 65 tons of oils transformed (semi refined rapeseed oil, crude and refined sunflower oils, refined high oleic sunflower oil)

3. Esters: Synthesis and application testing of esters successfully performed in food, cosmetics, lubricants, with equivalent or superior performance and with improved sustainability scoring

4. Dimers from Fatty Acids : Production of C36/C44 dimer fatty acids at demo scale

5. Polymers: Validation issues with the C36-dimer destined to the production of the polymeric end products prevented from leading to their production and application testing at demo scale. Initial experiments with C44 dimers have been performed but were not conclusive. The equipment for polymerization mixing was optimised through an improved design.

Overall, the LIPES technology leads to a safer process and meets key societal expectations by providing safer food products with zero trans fats and overall through a more sustainable and natural enzymatic approach.
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