Na2so4

For LDH-organic molecule synthesis, aluminum chloride hexahydrate (AlCl₃·6H₂O, 99%, Merck, Saint-Quentin-Fallavier, France) and magnesium chloride (MgCl₂·6H₂O, 98%, Merck, Saint-Quentin-Fallavier, France), sodium Hydroxide (NaOH, 98%, Acros, Geel, Belgium), ribloflavin-5′-phosphate (C₁₇H₂₀N₄NaO₉P, 98%, Merck, Saint-Quentin-Fallavier, France), ferrocene-carboxylic acid (C₁₁H₁₀FeO₂, 97%, Merck, Saint-Quentin-Fallavier, France) and ferrocene-dicarboxylic acid (C₁₂H₁₀FeO₄, 96%, Merck, Saint-Quentin-Fallavier, France) were used.
For electrode preparation, carbon black (SG, >99%, Superior Graphite Co., Sundsvall, Sweden) and polytetrafluoroethylene (PTFE, 60 wt% in water, Merck, Saint-Quentin-Fallavier, France) were used.
For electrochemical experiments sodium acetate (CH₃COONa, ≥99%, Merck, Saint-Quentin-Fallavier, France), sodium nitrate (NaNO₃, 99%, Merck, Saint-Quentin-Fallavier, France), sodium perchlorate (NaClO₄, 99%, Merck), lithium perchlorate (LiClO₄, 99%, Merck, Saint-Quentin-Fallavier, France), sodium sulfate (Na₂SO₄, 98%, Merck, Saint-Quentin-Fallavier, France) and lithium sulfate (Li₂SO₄, 99%, Merck, Saint-Quentin-Fallavier, France) were used. Deionized water was employed for all experiments.

4-(Phenylazo)phenol (TCI chemicals, Belgium) (50 mg, 0.252 mmol, 1 eq) was dissolved in previously degassed acetone (3 mL) (Merck Life Science S.r.l., Italy). Potassium carbonate (K₂CO₃) (Thermo Fisher Scientific Inc., Germany) (174 mg, 1.26 mmol, 5 eq) was added to the organic solution and the reaction mixture was stirred at r.t. under inert atmosphere for 90 min. Then, propargyl bromide (TCI chemicals, Belgium) (150 mg, 1.26 mmol, 5 eq) was added, and the reaction mixture was refluxed overnight, under inert atmosphere. Removal of the acetone under vacuum provided the solid crude product. It was then re-dissolved and extracted with EtOAc (Merck Life Science S.r.l., Italy) and the combined organic solution was washed with water and dried over Na₂SO₄ (Merck Life Science S.r.l., Italy). Removal of the solvent under vacuum was employed to yield the alkyne as an orange powder (56.5 mg, 0.239 mmol, 95%).
¹H NMR (CDCl₃, 400 MHz, δH, ppm): 7.94 (m, 2H, H-2), 7.89 (dt, 2H, H-2’), 7.54–7.42 (m, 3H, H-3’, H-4’), 7.12 (m, 2H, H-3), 4.78 (d, 2H, CH₂), 2.57 (t, 1H, triple bond C–H). FTIR-ATR: ν (cm⁻¹): 3266, 3076, 2927, 2129, 1600, 1584, 1489, 1237, 1144, 1016.
The above ¹H NMR and FTIR-ATR analytical data agreed with those reported in the literature^{39 (link)}.

PVC with a grade of 57, dimensions of ≤ 85 µM and a pore volume of 0.05–0.2 mL/g was supplied by Abadan Petrochemical Company, Iran. TTC with a purity of 99% was provided by Sinadaro Company, Iran. Other chemicals such as CaCO₃, MgSO₄, NaHCO₃, Na₂SO₄, C₈H₅KO₄, NaCl, HCl, and NaOH were purchased from Merck Company, Germany. Distilled water was used in all stages of this experiment.

Chloroauric acid trihydrate (HAuCl₄∙3H₂O), Silver nitrate (AgNO₃), L-ascorbic acid (AA), Sodium hydroxide (NaOH), anion salts (Na₂SO₄, NaCl, NaNO₃, Na₂HPO₄, NaHS∙H₂O, NaF, NaBr, NaI and KSCN), cation salts (Al(SO₄)₂∙18H₂O, CuSO₄∙5H₂O, ZnSO₄∙7H₂O, HgCl₂, Pb(NO₃)₂, Fe(NO₃)₃, FeSO₄, CaCO₃, MgSO₄∙7H₂O, NiSO₄∙6H₂O, CrN₃O₉∙9H₂O, CdSO₄, CoSO₄∙7H₂O) were obtained from Merck, Germany. All chemicals used in experiment were analytical reagent (AR grade).

A sodium silicate lump (Na₂O × 3SiO₂) was obtained from CheMondis GmbH (Köln, Germany), while the other reagents (TEOS, ethylene glycol, Bi(NO₃)₃, NaOH, Na₂SO₄, glycerol, polystyrene, 1,2-dichloroethane, HNO₃, KCl, K₃Fe(CN)₆, and K₄Fe(CN)₆) were purchased from Merck (Germany) and used as received.