Develop the materials by adapting a simple protocol
Critical learning
Choosing the manufacturing process
Linking material properties to implementation and composition
Understanding the impact of protocol deviations
Identifying recycling possibilities
By adhering to HSE regulations.
By incorporating the possibility of recycling.
By following a specification sheet (CDC).
By adhering to standard norms and protocols.
I. SAE
Elaboration - Caracterisation
HSE rules
This SAE has been subject to HSE regulations:
In terms of hygiene : I had to pay particular attention to any potential contamination caused by the use of products.
In terms of safety : When carrying out the processes, I consider the use of Personal Protective Equipment (PPE) and Collective Protection Equipment (CPE).
PPE stands for Personal Protective Equipment (examples: safety glasses, safety shoes...).
CPE stands for Collective Protection Equipment (examples: guardrails, signage...).
CONTEXT
Group of 3 students, during the Elaboration and Characterisation SAE, I had the task of studying the influence of the composition of Bulk Molding Compound (BMC) on the properties of the materials obtained after hot compression molding.
Topic : My topic involved developing various formulations of BMC premixes intended for hot compression molding and studying the influence of 2 parameters on 2 or 3 properties.
But what is BMC ? It is a set of semi-finished products resulting from the combination of resins, fillers, and reinforcements in the form of chopped fibers, intended for high-volume molding processes.
MY STRATEGY
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Literature review - Report writing + protocol
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Development of different formulations + preparation of molded BMC plates following the NF ISO 1268-8 standard and HSE regulations.
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Selection of material properties to analyse + associated characterisation techniques
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Experimental plan to identify influential parameters
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Preparation of molded BMC plates + characterisations + analysis of results
MY FEELINGS
This project allowed me to adopt an R&D approach to develop the material. The interesting aspect was that I felt able to elabore and charecterise the composite material.
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Difficulties were encountered, such as raw material sourcing and machine availability, but it allowed me to anticipate tasks by creating a Gantt chart, for example.
The group was cohesive, thanks to the bibliographic phase which allowed each team member to find their place in the project.
This SAE allowed me to realize that I enjoy investigating, searching, thinking, and progressing towards a goal. This SAE served as a trigger, and through this project, I discovered that I was passionate about R&D. I am happy to do my apprenticeship at a CNRS research laboratory, in collaboration with Sÿnia company, but I will talk about it later.
01 - Develop while adhering to HSE regulations
In addition to technical skills and knowledge, I must take into consideration the rules applied to my company and my school. A safety data sheet, accompanied by a tutorial video, has been done highlighting the importance of Personal Protective Equipment (PPE).
02 - Linking material properties to its composition
After conducting a literature review, I have selected some components based on their mechanical properties. I could have chosen epoxy resin and carbon fibers, and the development process would have been the same.
My conclusion : The factors I have chosen that may influence the material properties are CaCO3 and fiberglass. My conclusion is:
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If the % of CaCO3 is high, the surface condition is improved, the elastic modulus is also higher, and the impact energy absorption is better.
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The % of fiberglass needs to be optimized as it has an influence on the elastic modulus and maximum stress. Care must be taken regarding the distribution of the fibers.
03 - Understanding the influence of deviations in protocol implementation.
I 've prepared the premix according to the illustrated protocol below. The red markings indicate my recommendations for preparing the mixture to ensure a non-adherent compound to the mold walls.
II. Development of PU resin for doming SYNIA company internship
Context : I completed my second-year internship at SŸNIA, a company specialising in printing. SŸNIA is an European leader in doming (raised adhesive labels).
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What is doming ? Doming is a process that involves applying a transparent polyurethane resin onto an adhesive substrate.
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Internship suject : The goal was to propose improvements in "bio-based" polyurethane formulations for doming, aiming to reduce environmental impacts. This internship concluded with the signing of an apprenticeship contract that I began in January 2023.
kracken - doming machine
kracken - Resin application
Polyurethanes are obtained through the polyaddition of polyols and polyisocyanates. Since my formulations are confidential, I will not give the names of the polyol and isocyanate components used, nor their percentages.
I developed several formulations of bio-based PU resin and characterised them. Through this process, I optimised one of the formulations that met the specifications (CDC) and analyzed the relationship between the composition of the PU resin and its properties.
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The following properties were analyzed (properties selected based on the CDC provided by the R&D manager - confidential):
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Optical: Transparency (Gardner color < 3)
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Rheology: Viscosity and gel time
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Thermal: Glass transition temperature (Tg) and degradation temperature
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Swelling rate and gel time
04 - Develop while respecting the Specification Sheet
Reflective analysis
Elaboration is a skill that I find very interesting because it allows me to be constrained by norms and protocols while also being creative and testing new formulations. For example, I was required to use the one-pot method to simulate the two tanks of the industrial Kracken machine, but in a different context, I could have developed the PU using another process, such as the two-step method, and achieved the same characteristics.
Formulation is a team effort, and at ICGM, I learn how to communicate in English effectively. I have gained proficiency in sharing ideas, presenting results, and collaborating as part of a team.
01 - Develop while adhering to HSE regulations
During my internship, I had to handle potentially hazardous chemicals by myself. Therefore, I completed an online training program called NEO, and successfully completed three modules related to prevention, chemical risks, and fire risks.
With the training certificate obtained on 21/10/22, I was granted permission to access the laboratories.
02 - Select the manufacturing process
In the company :
Synia works with two-component resins. The machines consist of two tanks (one with an alcohol phase in which additives, including the catalyst, can be added, and another with an isocyanate phase). The doming machine is equipped with a system that pumps the phases from the tanks and then mixes them using a static mixer. At the outlet of the mixer, the multi-nozzle head allows for the resin to be applied onto the substrate.
In the laboratory - ICGM :
I had to choose a manufacturing process that could simulate the role of the two tanks in the company. Therefore, I carried out each PU resin formulation using the One-pot method. This method involves mixing monomers together to react and form a three-dimensional network. The polyurethane resin can then be domed onto an adhesive label and left at room temperature for cross-linking.
The plus...
I developed an optimized formulation of PU resin in which an "olfactory" component was incorporated. An olfactory domed label was created and presented to major perfume groups (Chanel, etc.)
To know more ...
03 - Linking the properties of the resin to its composition
Viscosity
Increasing the XX component of the isocyanate reduces viscosity but increases adhesion.
--> A compromise needs to be made!
Formulations F1 and F2 correspond to the specification sheet.
Gel time
The gel time of formulation F1 meets the specifications, just like that of F2, but its gel time could be extended by reducing the percentage of catalyst XX.
Thermal
Similar temperature profiles are observed among the different formulations. As for the glass transition temperature (Tg), I observed that the use of XX decreases the Tg, which is due to its long structure.
There is a correlation between Tg and material adhesion, where higher Tg indicates greater rigidity and promising adhesive properties.
Swelling/gel rate
My three formulations have lower swelling rates compared to the reference samples, which indicates that :
the use of XX allows for a denser network with tighter mesh structures (due to its higher average functionality (3.1) more functional groups will react)
3. Elaborer les matériaux en adaptant un protocole simple
III. Laboratory
work
Context: In perfumery, esters play a crucial role. Since a perfume is composed of approximately 90% alcohol, it is necessary to be able to mask the odor of ethanol. Esters provide their unique and pleasant fragrance to each perfume. Whether for an organic chemist or a polymer chemist, it is important to master the esterification reaction.
​During a laboratory session at IUT Nîmes, in the course of Synthesis and Purification of Isoamyl Acetate, I independently prepared a solution with a banana-like odor.
Reflective analysis
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I have learned a lot about myself during the various elaboration works, such as patience, precision, and rigor. I feel confident in interpreting experimental data and optimising formulations. In fact, I was able to secure an apprenticeship contract after optimizing a PU resin for scented doming.
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What also motivates me is to explore possibilities for recycling, particularly in the realm of polymers. Currently, I am conducting research on the depolymerization of polylactic acid (PLA) to develop polyurethane resins
Understanding the influence of deviations from protocol application
During the application of the protocol, a reflux setup is used. Why?
it allows for the efficient heating of the reaction mixture to its boiling point, which promotes the desired chemical reactions. The condensed vapors then return to the reaction vessel, preventing the loss of volatile components and ensuring a continuous reaction.
Often, a few grains of pumice stone are added during a reflux setup. What happens if we don't add them?
​Boiling chips help to create a more uniform and even boiling process by promoting the formation of bubbles at specific sites. This helps to prevent bumping, which is the sudden and violent ejection of liquid from the flask, and ensures a more controlled and efficient heat transfer.
If you do not work at a fixed and known temperature, what happens?
emperature plays a crucial role in determining the rate and extent of chemical reactions. Without a controlled temperature, the reaction may proceed too slowly or too quickly, leading to incomplete or undesired reactions.
​Inconsistent or uncontrolled temperatures may result in impurities, lower yields, or variations in product properties.
Why don't we seal the top of the condenser, which would prevent any loss of material?
Some chemical reactions generate gases or volatile substances that can accumulate pressure within the reaction vessel. By leaving the top of the condenser open, any excess pressure can escape, preventing potential hazards or equipment damage.