NH2-MIL-53(Al) Synthesis

NH2-MIL-53(Al) Synthesis SOP

Standard Operating Procedure (SOP)

Synthesis of NH2-MIL-53(Al) using Aluminium Nitrate + 2-Aminoterephthalic Acid

Hydrothermal / Solvothermal route using DMF + Water

Al-MOF Magnetic Stirrer Digital pH Meter Teflon-lined Autoclave Beginner-Friendly Lab SOP
“SOP”

1. Aim

To synthesize NH2-MIL-53(Al), an amino-functionalized aluminium-based metal-organic framework (Al-MOF), using a mixed solvent system of DMF and water, followed by drying and activation for future characterization and photocatalytic studies.

2. Important Note

Very important: Confirm the exact hydrate form of aluminium nitrate on the bottle label before weighing.

Many procedures use Al(NO3)3·9H2O, but your available bottle may be a different hydrate. The mass must be calculated from the actual molecular weight on the bottle.

3. Chemicals Required

Chemical Role Suggested Quantity Remarks
Aluminium nitrate hydrate Metal source Calculated from actual hydrate form Must be verified from bottle label
2-Aminoterephthalic acid (NH2-BDC) Organic linker 0.453 g (for 2.5 mmol) Main linker for NH2-MIL-53(Al)
DMF (N,N-Dimethylformamide) Main solvent 25 mL Improves crystallization
DI Water Co-solvent 5 mL Used to dissolve aluminium salt
Methanol Washing solvent As required For removing trapped DMF / unreacted linker

4. Batch Basis and Mass Calculation

Use a 2.5 mmol scale for the first trial batch.

Linker mass:
NH2-BDC molar mass ≈ 181.15 g/mol
Required moles = 0.0025 mol
Therefore, required mass = 0.453 g
For aluminium nitrate: Do not blindly use an old value.
Use:
Mass = moles × molar mass of actual hydrate on bottle

Example: if your bottle says a different hydrate than nonahydrate, the required mass will change accordingly.

5. Apparatus Needed

  • Magnetic stirrer with stir bars
  • Digital pH meter
  • Teflon-lined autoclave
  • Analytical balance
  • Beakers / measuring cylinders
  • Filtration setup or centrifuge
  • Drying oven
  • Glass petri dish or vial for drying / storage

6. Safety Precautions

DMF: Toxic solvent. Avoid inhalation and skin contact. Use in a well-ventilated area or fume hood.
Methanol: Toxic and flammable. Keep away from ignition sources.
Autoclave: Never fill above 80% of liner volume. Do not open while hot or pressurized.
Wear gloves, goggles, and lab coat throughout the experiment.

7. Final Improved Synthesis Procedure

1Preparation of Metal Solution

Take a clean beaker. Add 5 mL DI water. Weigh the required mass of aluminium nitrate hydrate based on the verified bottle label. Add it to the water and stir on a magnetic stirrer for about 10 minutes until dissolved.

2Preparation of Linker Solution

In another clean beaker, add 25 mL DMF. Weigh 0.453 g of 2-aminoterephthalic acid and add it slowly. Stir for 20–30 minutes.

If dissolution is slow, mild warming to about 50–60 °C is acceptable. Slight turbidity is not a problem.

3Mixing

Slowly pour the aluminium nitrate solution into the linker solution under continuous stirring. Continue stirring the combined mixture for 30 minutes to obtain a uniform solution/suspension.

4pH Measurement

Measure the pH of the final reaction mixture using a digital pH meter and record it in the lab notebook.

No pH adjustment is required. Do not add NaOH or strong acid unless following a specific literature procedure.

5Autoclave Loading

Transfer the reaction mixture into the Teflon-lined autoclave. Ensure that the fill volume is below 80% of the liner capacity. Clean the rim and seal the autoclave properly.

6Hydrothermal / Solvothermal Reaction

Place the autoclave in the oven/heating unit and heat at:

150 °C for 12–15 hours

For the first trial, 12 hours is acceptable. If crystallinity is poor, try 15 hours in the next run.

7Cooling

After completion of heating, allow the autoclave to cool naturally to room temperature. Do not force-cool and do not open while hot.

8Product Recovery

Open the autoclave carefully after cooling. Collect the solid product by filtration or centrifugation. The product is expected to appear as a yellowish to pale cream powder.

9Washing

Wash the obtained solid thoroughly as follows:

  • DI water: 2–3 times
  • Methanol: 2–3 times

This helps remove residual salts, DMF, and unreacted linker.

10Drying

Dry the washed product at 80 °C overnight.

11Activation

For better porosity and future characterization, activate the dried sample at:

120 °C for 4 hours

Then cool in a desiccator and store in an airtight vial.

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