User:Klare Lazor/Notebook/Chem-496-001/2013/02/04

Objective

1. Cross‐link films
2. Make more fixant
3. DSC and FTIR after cross-­‐linking.
4. synthesize quaternary ammonium

Description and Data

Cross-linking PVOH+Isopropyl+glutaraldehdye

1. Allow the PVOH film containing glutaraldehyde to dry completely.
2. Prepare a solution of 100 mL H2O, 2 mL concentrated H2SO4, and 20 g Na2SO4 in a 150 mL beaker. (solution is referred to as glutaraldehyde fixant)
3. Place stir bar in beaker and a Buchner funnel top (cap) over the stir bar
4. Heat solution to 70°C (temperature on hotplate should be about 160)
5. Place film in solution for one hour.
6. Prepare 100 mL of a 1% HCl solution in a 150 mL beaker. Place a stir bar and an inverted buchner funnel into beaker.
7. Heat HCl solution to 70°C
8. Remove film from glutaraldehyde fixant and rinse with distilled water.
9. Place film into HCl solution for 30 minutes.
10. Prepare 0.2 M sodium bicarbonate solution. (1.68 g in 100 mL)
11. After 30 minutes, remove the film from the HCl solution and place into the sodium bicarbonate solution (at room temperature) for about 15 minutes.
12. Use tweezers to remove the film from the sodium bicarbonate solution.
13. Rinse film with deionized water and place in a beaker with distilled water until it is used/tested

Synthesis of Ammonium Salt a 2 fold reaction

• Added 4-chloro-1-butanol (Eastman) and Triethylamine in acetonitrile for 72 hours to reflux.
• SN2 reaction
• Added 10mL of Acetonitrile and 1.148mL chlorobutanol and 0.753ml triethylamine in round bottom flask with stir bar
• Attached flask to a redox condense.
• heated with a heating mantle with sand
• set 100v heater to 50 because of evap temp for acetonitrile should occur around that voltage
• Added nitrogen gas to flow through reflux condenser such that the run occurs under nitrogen.
• turned on heating mantle and left the flask to reflux for 72 hours

Image of SN2 reaction

Results of films after cross linking

• Isopropyl evaporate off before we could cross link the film after the weekend. Could tell because films were very water soluble and were falling apart in sodium bicarbonate solution. Except for the glutaraldehyde control.
• phenol or benzyl alcohol soluble in water can be used because will remain in film long enough to cross-link
• Next time films will contain 1 gram of pvoh because prior films were way to thin.

Notes

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