User:Sarah Burkhard/Notebook/CHEM 481 Polymers/2016/09/16

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Tasklist

Making of 20 percent clay solution

Friday: 20 percent clay mass of whole solution 20 percent clay in PVOH. 2.5 g PVOH = 80 percent 2.5/.8 = total mass = 3.125 g multiply by 0.2 (20 %) to get mass of clay in g : 0.625 g . divide by 0.03 to get solution: 0.625 g / 0.03 g/ml = 20.83 ml bentonite solution 3 g / 100 ml solution = 0.03 g/ml attention: the HCl will be diluted by the water added with the clay solution. Report the new concentration. Through adding 20.83 ml bentonite solution (97 ml H20/ 100 ml bentonite solution) we effectively added 20.2 ml H20. This will dilute our 30 ml 10% HCL by 2/3 , so to 3.33 % HCl.we would need 30 ml of 30 % HCL solution

8.1 ml 37% concentrated HCl + 20.8 ml water from solution + 1 ml H20 ~ 30 ml 10% Hcl

Beads

Large Scale Synthesis Create a solution of 2.5 g PVA, 0.275 g NaMT, and 30 mL 10% HCl. Place this solution on a hot plate and heat/stir until everything has dissolved. Add 10 mL of this solution to a 50 mL solution of ethyl acetate stirring at 240 rpm in a dropwise manner. Add 1 mL of glutaraldehyde and stir at 260 rpm for 3 minutes. After 3 minutes, add 1 mL of glutaraldehyde and stir at 300 rpm for 2 minutes. After 7 minutes, add 7 mL of sodium bicarbonate and stir for 30 seconds. Remove the solution, put it into 2 50 mL Falcon tubes. Centrifuge the solutions for 1 minute at 3000 rpm.

replaced clay with carbon

DSC

tablet weigh . want 42 mg +/- 0.2 mg open pan . ideal sample : 3-5 mg , 15 for heat capacity\

DSC data

Data

PVOH neat.jpg PVOH x-link.jpg PVOH x-link 10clay.jpg PVOH x-link 10clay Beads.jpg

DSC Data
Glass Transition (°C) Melting Point (°C) Heat of Melting (J/g)
PVOH 70.25 191.13 35.66
PVOH x-link 80.07 179.67 0.6426
PVOH x-link 10% clay 82.19 168.08 0.5314
  • no glass transition, melting point, or heat of melting determined for PVOH 10% Beads

Percent of PVOH not cross-linked:

  • PVOH x-linked film without clay:
0.6426J/g / 35.66J/g *100% = 1.8%
  • PVOH x-linked film with 10% clay:
0.5314J/g / 35.66J/g *100% = 1.49%

Notes

Activated carbon difficult to dissolve in PVOH. Formed clumps, so took additional heat and stirring time. Black dots in transparent solution indicate beads formation.

beads in oven 105 degrees , 30 minutes means acid left next time, measure ph. if low, keep washing .