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Anodic oxidation of paraquat herbicide on BDD electrode - comparative evaluation of variable effects and degradation mechanisms

MetadataDetails
Publication Date2025-01-01
JournalRSC Advances
AuthorsNejmeddine Rabaaoui, Naoufel Ben Hamadi, Mourad Cherif, Ahlem Guesmi, Wesam Abd El‐Fattah
InstitutionsTunis University, Tunis El Manar University
Citations1
AnalysisFull AI Review Included

This study rigorously compared Boron-Doped Diamond (BDD), Lead Dioxide (PbO2), and Platinum (Pt) anodes for the electrochemical degradation of the persistent herbicide paraquat.

  • Superior Performance: BDD anodes demonstrated exceptional efficiency, achieving 99% Chemical Oxygen Demand (COD) removal and 98.6% Total Organic Carbon (TOC) removal within 300 minutes, significantly outperforming PbO2 (88.5%) and Pt (79.5%).
  • Mechanism Confirmation: The high efficiency is attributed to BDD’s capability to generate highly reactive, physisorbed hydroxyl radicals (‘OH), enabling non-selective, deep mineralization.
  • Kinetics and Mineralization: Degradation followed pseudo-first-order kinetics with a high rate constant (k = 1.53 x 10-2 s-1), confirming rapid initial oxidative transformation. Full mineralization into CO2, H2O, and NH4+ was confirmed via intermediate tracking.
  • Operational Optimization: Optimal conditions were identified as acidic pH (pH 3.0) and a current density of 15 mA cm-2, balancing high efficiency with moderate energy consumption.
  • Sustainability and Durability: BDD exhibited negligible corrosion (less than 10-5 g cm-2 h), ensuring long-term structural integrity, a key advantage over the substantially degrading PbO2 anode (0.0335 g cm-2 h).
  • Energy Metrics: Despite high initial Faradaic Efficiency (FE) (70.14% at 220 min), the Cumulative Energy Consumption (CEC) reached 66 kWh m-3, highlighting the need to optimize treatment duration to avoid excessive energy expenditure in low-efficiency phases.
ParameterValueUnitContext
COD Removal (BDD)99%300 min, 15 mA cm-2, pH 3.0
TOC Removal (BDD)98.6%300 min (from 25 mg L-1 to 0.40 mg L-1)
Kinetic Rate Constant (k)1.53 x 10-2s-1Pseudo-first-order degradation
Optimal Current Density15mA cm-2Balance of efficiency and energy input
Optimal pH3.0-Promotes ‘OH radical generation
BDD Corrosion Rate<10-5g cm-2 hNegligible corrosion
PbO2 Corrosion Rate0.0335g cm-2 hSubstantial degradation observed
Initial Paraquat Conc.30mg L-1Electrolysis starting concentration
Electrolyte Conc.50mmol L-1Used Na2SO4, NaCl, or NaNO3
Electrolysis Temperature20°CControlled operating temperature
Anode Effective Area10cm2BDD, PbO2, and Pt anodes (2.5 cm x 4 cm)
Faradaic Efficiency (FE)70.14%Measured at 220 minutes
Cumulative Energy Cons. (CEC)66.00kWh m-3Measured at 220 minutes
BDD Film Thickness~1”mSynthesized via HF-CVD
BDD Resistivity15 (±30%)mΩ cmElectrical property of the diamond film

The study employed galvanostatic electrochemical advanced oxidation processes (EAOPs) using three distinct anode materials.

  1. BDD Electrode Synthesis (Hot Filament Chemical Vapor Deposition - HF-CVD):

    • Substrate: Conductive p-Si (1 mm, Siltronix).
    • Filament Temperature: Maintained between 2440 °C and 2560 °C.
    • Substrate Temperature: Monitored at 830 °C.
    • Reactive Gas: 1% Methane (CH4) in Hydrogen (H2), containing 1-3 ppm of trimethyl boron (dopant).
    • Gas Flow Rate: 5 mL min-1, resulting in a growth rate of 0.24 ”m h-1.
  2. PbO2 Electrode Preparation:

    • Method: Galvanostatic electrochemical anodization.
    • Substrate: Pretreated lead.
    • Electrolyte: Oxalic acid solution (100 g L-1).
    • Conditions: 30 minutes at ambient temperature, 100 mA cm-2 anodic current density.
  3. Electrolysis Setup and Operation:

    • Cell Type: Single-compartment cylindrical cell, thermostated at 20 °C.
    • Anodes: BDD, PbO2, and Pt, each with a 10 cm2 effective geometric surface area.
    • Cathode: Cylindrical graphite rod (0.8 cm diameter, 4.0 cm immersed length).
    • Electrolyte: Various 50 mmol L-1 solutions (Na2SO4, NaCl, NaNO3) were tested.
    • Analysis: Paraquat and intermediates were quantified using HPLC-Thermo Fisher Scientific equipped with a Diode Array Detector (DAD). Mineralization was tracked via COD and TOC analysis.
  4. Mechanistic Analysis:

    • Aromatic and carboxylic acid intermediates (e.g., monopyridone, oxalic acid, formic acid) were identified using HPLC and Mass Spectrometry (MS) to map the multi-stage degradation pathway, confirming ring-opening and final mineralization.

The findings of this research, particularly the robust performance and durability of Boron-Doped Diamond (BDD) electrodes, are highly relevant for industrial sectors dealing with persistent organic pollutants (POPs).

Application AreaRelevance to Technology
Wastewater Treatment (Industrial Effluents)BDD anodes provide deep mineralization capacity, essential for treating refractory organic contaminants (like herbicides, pesticides, and pharmaceuticals) that resist conventional biological or chemical methods.
Pesticide Manufacturing/FormulationDirect application for treating highly concentrated wastewater streams generated during the production of quaternary ammonium herbicides (e.g., paraquat).
Water Reuse and Discharge ComplianceThe ability to achieve near-complete TOC removal and convert toxic intermediates into harmless inorganic end-products (CO2, H2O, NH4+) ensures compliance with strict regulatory standards for water discharge or reuse.
Advanced Oxidation Processes (AOPs)BDD electrodes are a core component in sustainable EAOPs, offering superior oxidative power and operational stability compared to traditional electrode materials (PbO2, Pt).
Electrochemical Sensor TechnologyThe use of BDD substrates, known for their wide potential window and stability, is foundational for developing highly sensitive electrochemical sensors for detecting environmental contaminants.
View Original Abstract

Anodic oxidation of paraquat on BDD electrodes achieves up to 99% COD and 98.6% TOC removal. A detailed mechanistic pathway via aromatic ring cleavage and carboxylic acids confirms efficient mineralization despite increasing energy demand.