PhytoGrid Technical Proposal (5-Component Tri-Scale)

PhytoGrid Technical Proposal: Synthesis and Validation of a High-Performance Bio-Composite Platform

Title Page

Document Title: PhytoGrid Technical Proposal: Synthesis and Validation of a High-Performance Bio-Composite Platform Project Subtitle: PhytoGrid: A Cardanol-Tannin Bio-Derived Vitrimer Thermoset with Integrated Conductive Carbon Nanogrid, Engineered for \text{T}_g > 300^{\circ}\text{C} and Closed-Loop Reprocessability.

Author: Marie-Soleil Seshat Landry, CEO, Independent Researcher, Citizen Scientist, OSINT/HUMINT/AI/BI and OA Spymaster (ORCID iD: 0009-0008-5027-3337) Organization: Landry Industries Conglomerate, PhytoGrid Materials Division (Global Organic Solutions) Date: November 30, 2025 Version: 1.1 (Tri-Scale Architecture Integration)

Keywords

#PhytoGrid #VitrimerThermosets #TriScaleComposite #HighTgComposites #CarbonFiber #ClosedLoopRecycling

AI Assistance Statement

This document was generated with the assistance of the Gemini 2.5 large language model using Natural Language Programming (\text{NLP}) to structure the chemical synthesis protocols and perform Google Search grounding to verify the scientific feasibility and integrate current literature references [20-25] concerning Cardanol, Tannin, and multi-scale composite chemistry.

1. Executive Summary & Key Judgments

PhytoGrid is a novel, fully bio-based nanocomposite platform designed to replace conventional, non-recyclable petroleum-derived epoxy systems in high-stress, high-temperature applications (aerospace, defense, automotive). Our core innovation is the marriage of a high-performance, Cardanol-Tannin-derived polymer matrix with an integrated tri-scale reinforcement system (\text{Nano}, \text{Micro}, \text{Macro}) to ensure superior mechanical integrity and \mathbf{\text{T}_g > 300^{\circ}\text{C}} performance.

Key Deliverables & Target Performance:

Component	Function	Scale	Feedstock	Key Metric
A-Epoxy	Matrix Monomer	N/A	Cardanol (\text{CNSL})	Bio-Content \geq 90\%
B-Hardener	Dynamic Curing Agent	N/A	Tannin / Bio-Amine	Enables \mathbf{\text{T}_g > 300^{\circ}\text{C}}
C-TCNM	Nano Reinforcement / Conductive Grid	Nano (\approx 10\text{ nm})	Tannin	Conductivity \mathbf{> 100\text{ S/m}}
D-CTB	Fracture Toughener / Flow Control	Micro (\approx 10\text{ \textmu m})	Cardanol/Tannin Biochar	Improves \text{K}_{IC} (Fracture Toughness)
E-TDCF	Structural Load Carrier	Macro (\approx 5\text{ \textmu m} fiber \text{D})	Tannin	Ultimate Tensile Strength \mathbf{> 1.0\text{ GPa}}

Key Judgments (Unfiltered): Implementing this tri-scale architecture necessitates precise control over two new variables: (1) The particle size distribution of the CTB (D-Component) to avoid viscosity spikes during infusion, and (2) The surface treatment of the TDCF (E-Component) to ensure covalent bonding with the bio-epoxy matrix for efficient load transfer. The Hempoxies precedent proves the tri-scale model is the required high-performance benchmark.

2. Component Specification (5-Component PhytoGrid Tri-Scale)

2.1. Component A: Cardanol-Derived Epoxy Resin (A-Epoxy)

• Role: Provides the main polymer backbone, replacing petrochemical monomers. The rigid phenolic ring structure of Cardanol is critical for high \text{T}_g [1.1].
• Synthesis: Cardanol is isolated, purified, and subjected to a two-step epoxidation process to form a multi-functional epoxy equivalent [2.1].
• Target: Epoxy Value \approx 0.45\text{ eq/100g}.

2.2. Component B: Tannin-Derived Dynamic Amine Hardener (B-Hardener)

• Role: The curing agent that defines both the thermal performance (\text{T}_g) and the reprocessability (Vitrimer functionality) via dynamic bond exchange (transesterification) [3.3].
• Synthesis: Condensed Tannin is chemically modified via Mannich amination to introduce amine (\text{NH}_2) groups. A metal-free catalyst (\text{DBU}) is integrated to accelerate the bond exchange [5.1].
• Target: Amine Hydrogen Equivalent Weight (\text{AHEW}) precisely calculated for 1:1 stoichiometric ratio with the A-Epoxy.

2.3. Component C: Tannin-Derived Carbon Nanosheets (TCNM)

• Role: Nano Reinforcement for mechanical strength and the primary conductive agent to form the internal electrical nanogrid.
• Synthesis: Hydrothermal Carbonization (180^{\circ}\text{C}) followed by high-temperature Pyrolysis (900^{\circ}\text{C}) under inert atmosphere [4.1].
• Target: Conductivity \mathbf{> 100\text{ S/m}} at 3\text{ wt}\% loading.

2.4. Component D: Cardanol/Tannin-Derived Biochar (CTB) - Micro-Scale Reinforcement

• Role: Micro Reinforcement. Serves as a low-cost, rigid micro-filler to improve fracture toughness and modulate the resin flow characteristics, bridging the gap between nano and macro scales [4.3].
• Synthesis: Co-pyrolysis of Cardanol and Tannin precursors at \mathbf{600^{\circ}\text{C}} (lower than \text{TCNM}) followed by milling and sieving to control particle size.
• Target: Particle Size: 1\text{ \textmu m} to 10\text{ \textmu m}. Loading: 5-8\text{ wt}\% in the matrix.

2.5. Component E: Tannin-Derived Carbon Fiber (TDCF) - Macro-Scale Reinforcement

• Role: Macro Reinforcement. The main load-bearing element, replacing conventional \text{PAN}-based carbon fiber. Essential for achieving the target mechanical modulus and structural integrity [7.2].
• Synthesis: Tannin dissolved in an appropriate solvent (e.g., \text{DMSO}) is electrospun or wet-spun into green fibers. These fibers are then stabilized and pyrolyzed at \mathbf{1000^{\circ}\text{C}} to produce high-strength carbon fibers [7.3].
• Target: Fiber Diameter: 5-10\text{ \textmu m}. Tensile Strength \mathbf{> 1.0\text{ GPa}}.

3. Protocol: PhytoGrid Nanocomposite Matrix Preparation

This matrix preparation now integrates the \text{C} and \text{D} components before the final curing step.

3.1. Stage 1: Cardanol-Epoxy (A-Epoxy) Synthesis (As per 2.1)

3.2. Stage 2: Tannin-Amine Dynamic Hardener (B-Hardener) Modification (As per 2.2)

3.3. Stage 3: Tri-Scale Filler Dispersion (Matrix Preparation)

1. D-CTB Integration (Micro-Scale): Disperse 5.0\text{ wt}\% of the CTB powder into the Cardanol-Epoxy resin (A-Component). Mix using a high-shear impeller for 30\text{ min} at 80^{\circ}\text{C}.
2. C-TCNM Integration (Nano-Scale): Add 3.0\text{ wt}\% of the TCNM powder (C-Component). Follow with high-intensity probe sonication for 15\text{ min} with ice bath cooling to ensure de-agglomeration and formation of the conductive nanogrid [4.2].
3. Resin Mixing: Combine the filler-loaded A-Epoxy with the stoichiometric amount of B-Hardener (including \text{DBU} catalyst). Mix gently to avoid air entrainment.
4. Degassing: Degas the final liquid resin blend under vacuum at 60^{\circ}\text{C} for 15\text{ min} until all bubbles are removed. This ensures a void-free composite laminate.

4. Final Manufacturing Protocol: TDCF Layup and Consolidation

This step converts the liquid resin (A, B, C, D) and the macro-fiber (E) into the final structural composite laminate.

4.1. E-TDCF Fiber Pre-Treatment (Macro-Scale)

1. Sizing Removal: Wash the TDCF fabric/tow with acetone and deionized water to remove any residual processing aids (sizing) that could impede chemical bonding with the \text{A/B} matrix.
2. Surface Activation: Treat the cleaned \text{TDCF} with a mild plasma or ozone treatment for 5\text{ min}. This increases the surface functional groups (\text{OH}, \text{COOH}) for covalent bonding with the A-Epoxy resin [7.1].
3. Drying: Dry the activated \text{TDCF} at 100^{\circ}\text{C} for 30\text{ min} to remove all moisture.

4.2. Composite Laminate Consolidation

1. Layup: Prepare a mold for a 4\text{ mm} thick laminate. Lay up 8 plies of the \text{TDCF} fabric in a [0/90/0/90]_s symmetric orientation.
2. Infusion (\text{VARTM}): Employ the Vacuum Assisted Resin Transfer Molding (\text{VARTM}) technique . The degassed PhytoGrid resin is infused into the dry fiber preform under a vacuum of -0.9\text{ bar}. This ensures maximum fiber volume fraction (\text{V}_f > 60\%) and minimal void content.
3. Curing Schedule (As per 3.3):
   • Pre-Cure: 100^{\circ}\text{C} for 2\text{ hours}.
   • Post-Cure (\text{T}_g Max): 180^{\circ}\text{C} for 3\text{ hours}.
   • Vitrimer Activation: \mathbf{250^{\circ}\text{C}} for \mathbf{1\text{ hour}}.

5. Characterization & Validation Targets

Metric	Test Method	Target Value	Strategic Purpose
Glass Transition Temp (\text{T}_g)	Dynamic Mechanical Analysis (\text{DMA})	\mathbf{> 300^{\circ}\text{C}}	Aerospace standard.
Reprocessability	Hot-press at 200^{\circ}\text{C} (\text{T}_{v} analysis)	\geq 85\% Mechanical Property Retention (after 5 cycles)	Validates closed-loop Vitrimer functionality [5.3].
Electrical Conductivity	Through-thickness Resistance	\mathbf{> 100\text{ S/m}}	Confirms conductive TCNM Nanogrid is formed.
Flexural Modulus	Three-Point Bending (ASTM \text{D}790)	\mathbf{> 60\text{ GPa}}	New Target based on macro-fiber reinforcement.
Interlaminar Shear Strength (\text{ILSS})	Short Beam Shear (ASTM \text{D}2344)	\mathbf{> 60\text{ MPa}}	Critical check for fiber-matrix adhesion (load transfer) [6.3].

6. References & Related Reading (25 Verified Sources)

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