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# preparation of ionic liquid modified clays
# preparation of ionic liquid modified clays
## We are going to exchange the sodium in the sodium montmorillonite for an organic cation. The procedures are taken from these two sources ([http://www.scirp.org/journal/PaperInformation.aspx?PaperID=17245#.VA5V9Et5_zY 1], [http://www.clays.org/journal/archive/volume%2010/10-1-153.pdf 2] along with Karlena Brown's thesis. We are working from the starting point that there are 92 miliequivalents (meq) of Na+ per 100g of montmorillonite.  
## We are going to exchange the sodium in the sodium montmorillonite for an organic cation. The procedures are taken from these two sources ([http://www.scirp.org/journal/PaperInformation.aspx?PaperID=17245#.VA5V9Et5_zY 1], [http://www.clays.org/journal/archive/volume%2010/10-1-153.pdf 2] along with Karlena Brown's thesis. We are working from the starting point that there are 92 miliequivalents (meq) of Na+ per 100g of montmorillonite.  
## Add 1.1g of Sodium Montmorillonite (NaMT) to a scintillation vial containing 20mL of 50:50 HPLC grade water:ethanol.
## The original film preparation protocol was followed
## Determine the amount of cation to add if using either [http://www.sigmaaldrich.com/catalog/product/aldrich/276200?lang=en&region=US tributylhexadecylphosphonium bromide]] to exchange 100% of the Na from the clay.
## Began organic cation exchange following [[User:Matt_Hartings/Notebook/AU_Biomaterials_Design_Lab/2014/09/10| Dr. Harting's procedure]]
## Add this amount of phosphonium ion to the clay solution.
### 1.1046 g of Sodium Montmorillonite was added to a vial
## Cap the vial
### Assuming 92 meq of Na per 100 g, the total eq was 10.16232E-04
## Stir for 1 week.
### Added 0.5251 g tributylhexadecylphosphonium bromide (MW=507.65) to the vial
## Vacuum filter using 0.2uM nylon filter paper
### Added 10 mL of HPLC water and 10 mL ethanol
## Dry in oven at 90C overnight
### capped the vial and set to stir for one week
## Grind with a mortar and pestle.  
## Finished compiling and sorting through data (UV-VIS, FTIR) from last week
## Store in a dessicator
## There was not enough time to retrieve the DSC data, so this will be completed on Friday
 
#Prepared Film Samples for Powder X-Ray Diffraction
==Data==
## Incised a PVA-clay film with the size of the scintillating vial lid.  
* Add
## The film was suspended in 10 mL of 2ppm MG solution contained in a scintillating vial. The MG solution for this sample was prepared from the stock solution prepared on [[User:James C. Schwabacher/Notebook/CHEM-571/2014/08/29|August 29, 2014.]]
* The sample will be analyzed for the following lab meeting on September 12, 2014.


==Notes==
==Notes==

Revision as of 08:00, 24 September 2014

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Objective

  • Continued the synthesis of polymer and polymer-clay films.
  • Begin the preparation of ionic liquid modified clays.

Description

  1. Completing the Synthesis
    1. the procedure for completing the synthesis of films may be viewed here.
  2. preparation of ionic liquid modified clays
    1. We are going to exchange the sodium in the sodium montmorillonite for an organic cation. The procedures are taken from these two sources (1, 2 along with Karlena Brown's thesis. We are working from the starting point that there are 92 miliequivalents (meq) of Na+ per 100g of montmorillonite.
    2. The original film preparation protocol was followed
    3. Began organic cation exchange following Dr. Harting's procedure
      1. 1.1046 g of Sodium Montmorillonite was added to a vial
      2. Assuming 92 meq of Na per 100 g, the total eq was 10.16232E-04
      3. Added 0.5251 g tributylhexadecylphosphonium bromide (MW=507.65) to the vial
      4. Added 10 mL of HPLC water and 10 mL ethanol
      5. capped the vial and set to stir for one week
    4. Finished compiling and sorting through data (UV-VIS, FTIR) from last week
    5. There was not enough time to retrieve the DSC data, so this will be completed on Friday
  3. Prepared Film Samples for Powder X-Ray Diffraction
    1. Incised a PVA-clay film with the size of the scintillating vial lid.
    2. The film was suspended in 10 mL of 2ppm MG solution contained in a scintillating vial. The MG solution for this sample was prepared from the stock solution prepared on August 29, 2014.
  • The sample will be analyzed for the following lab meeting on September 12, 2014.

Notes




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