Polymerization Experiment


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Polymerization Experiment

  1. 1. Polymerization<br />During INTERNSHIP AT MAHIDOL<br />Done by: Cindy & Jack<br />
  2. 2. Polymerization<br />Is a process of reacting monomer molecules together reacting in a chemical reaction to form 3-D networks or polymer chains.<br />
  3. 3. Monomers & Polymers<br />MONOMERS are atoms or a small molecule that may bind chemically to other to form polymers.<br />Polymers are large molecules composed of repeating structural units.<br />
  4. 4. Atomic Transfer Radical Polymerization<br />ATRP is a type of polymerization that can control the length of a polymer<br />There are 3 components, which includes a monomer, catalyst, and a initiator<br />
  5. 5. In this Experiment...<br />We used Two monomers: <br /><ul><li> Methyl Methacrylate (MMA)
  6. 6. Styrene</li></ul>Two catalysts: <br /> - Copper Bromide (CuBr)<br /> - Liquid TRENFCIM<br />Two initiator: <br /> - 1-Bromoethylrenzene<br /> - Ethyl 2-Bromoisobuthylate(??) <br />
  7. 7. Order of experimentation<br />Polymerization of MMA<br />Polymerization of Styrene<br />Polymerization of MMA and Styrene at the same time<br />Copolymerization of MMA + Styrene<br />Copolymerization of Styrene + MMA<br />- First two were to let us be familiarized with polymerization<br />
  8. 8. Purpose<br />Check whether the theory and the experiment matches or not.<br />To find out which monomer the catalyst suits more.<br />To study properties of polymer products and copolymer products<br />
  9. 9. Hypothesis<br />We could have hypothesized, however, we knew nothing about polymerization, so we had no idea what would happen. Therefore, we could not hypothesize.<br />
  10. 10. Materials Used<br />High vacuum <br />grease<br />Trap<br />Parafilm (30)<br />Argon Gas<br />Argon (g)<br />Medium size towel (2)<br />Stand<br />Vacuum pump<br />Thermostat container<br />Styrene (l)<br />Ethyl-2-bromoisobuthyl (l)<br />CuBr (s)<br />Ligand TRFNFclm (s)<br />Mask<br />Aluminum Oxide (s)<br />Stopper<br />Column<br />Cotton<br />THF<br />Plastic Spoon<br />Spatula<br />short Eyedropper<br />Long eyedropper <br />Square Dry Ice (10)<br />Acetone (l)<br />Hammer<br />MMA (l)<br />Goggles<br />Weighing papers<br />Gloves<br />Magnetic bar<br />Funnel<br />Anti-bump<br />Stirrer<br />Magnetic stirrer<br />
  11. 11. Procedure<br />The step by steps in the experiment weren’t complicated but it just took a lot of time and had us ending up like this..<br />
  12. 12. Setting Trap<br />Apply grease to the cap of the trap <br />Put the trap on the stand<br />Connect the 2 tubes from the vacuum to the trap<br />Use parafilm to wrap around the tubes to prevent leakage<br />Turn on the vacuum machine<br />Open the argon gas tank<br />Wait for 30 minutes<br />Put the trap in a thermostat container<br />Get dry ice and put it in the container<br />Once its full, pour acetone in the container slowly<br />Cover the top with a rag<br />
  13. 13. Setting Side-Arm flask<br />Get a side-arm flask from the oven<br />Quickly set it on the stand<br />Adjust the stopper cock onto the flask<br />Stick the rubber stopper on the opening<br />Vacuum it for 5 minutes<br />Change it to argon gas for 20 seconds<br />Repeat the last two steps 2 more times<br />
  14. 14. Weighing Catalyst<br />Get the catalyst needed from the desiccator<br />Put the weighing paper in the weighing scale and zero it<br />Using a spatula get the amount of catalyst needed<br />Do it again using a different spatula and weighing paper if there are more catalysts<br />Quickly open the rubber stopper and put the catalysts needed<br />Vacuum it 3 times<br />
  15. 15. Injecting the monomer <br />Bring out the monomer from the fridge<br />Store it at room temperature<br />Get a needle from the oven and stick it on a plastic syringe<br />Using the needle pump the argon out 3 times<br />Using the needle with the syringe take 2mL out of the monomer<br />Using tissue, adjust the amount of monomer needle by flipping the needle backwards<br />Inject it in the flask<br />Get a glass stopper from the oven<br />Apply grease on it<br />Quickly replace it with the rubber stopper<br />
  16. 16. Freeze Pump Thaw<br />Put the side arm flask in a thermostat container<br />Add dry ice into the container<br />Slowly pour in acetone into the container<br />Wait till the liquid solution freezes<br />Vacuum it for 10 minutes<br />Close the valve on the flask<br />Take the flask out of the container<br />Leave it for it to melt<br />After it turns to liquid, put it back in the container<br />When it freezes, open the valve<br />Vacuum it for 10minutes<br />Repeat steps 6~11 again<br />Close the valve<br />Take the flask out and let it melt<br />Change the glass stopper to a rubber stopper before<br /> it melts<br />
  17. 17. Stirring<br />Get a magnetic stirrer<br />Set the flask on top of it<br />Place a piece of tissue under the flask<br />Set it to 300rpm<br />Stir it for 5minutes<br />
  18. 18. Injecting the Initiator<br />Go to the oven and get needle syringe and a glass bottler(idk how to call)<br />Get the initiator from the desiccator (1-bromoethylrenzene)<br />Pour a little bit initiator into the glass bottle<br />Get the needle and pump the argon out 3 times<br />Put it in the flask<br />Move it to the magnetic stirrer with heat ( temperature depends on the catalyst)<br />Stir it<br />Add THF to stop the reaction<br />
  19. 19. Removing Catalyst<br />Wear a mask<br />Get a column with a stopper and fix it on a stand<br />Put a small piece of cotton in the column enough to block the bottom<br />Get 20 spoons of aluminum oxide in a beaker<br />Pour in THF enough to cover the aluminum oxide<br />Mix it well using <br />Pour it down the column<br />Using THF let most of aluminum oxide go in the column<br />Let all the aluminum oxide on the walls of the column go to the bottom<br />Hit the column with a tube so that it’ll be packed<br />Place a beaker under the column and open the valve<br />
  20. 20. Removing Catalyst<br />When a little bit of THF is left, close the valve<br />Using a dropper drop THF in the column along the walls<br />Repeat the steps until the THF in the column is clear<br />When it gets clear, close the valve<br />Get the solution in the side arm flask <br />Using another magnetic bar, take the magnetic bar inside out<br />Get a long dropper and use it to drop towards the wall of the column<br />When done, using THF rinse the side arm flask and pour it in the column (twice)<br />Use a dropper with THF to rinse the walls of the column too<br />Get a flask and replace it with the beaker under the column<br />Open the valve, and make it a drop per 2 seconds<br />Pour THF in the column if the opening near the stopper cock isn’t transparent<br />
  21. 21. Removing Solvent <br />Pour the solution in the flask using a funnel into a 250mL round bottom flask<br />Open the vacuum machine<br />Set it to 40 degrees <br />Connect the anti-bump to the machine<br />Right next to the anti-bump connect the round bottom flask<br />Close the top(??) to reduce pressure<br />Lock the anti-bump and the round bottom flask using a blue clip<br />Rotate it for 20~30 minutes<br />
  22. 22. Removing Solvent <br />Open the top(??) to increase pressure back<br />Take the blue clip out and take out the round bottom flask<br />Using a dropper drop 2 droppers of dichloromethane into the round bottom flask<br />Pour 50mL of methanol into the round bottom flask <br />Leave it for 5 minutes<br />Pour the methanol in the round bottom flask out into a beaker<br />Using a spatula gather all the precipitate in the flask into a ball<br />Vacuum it for __ hours<br />
  23. 23. Results (MMA)<br />
  24. 24. Results (styrene)<br />
  25. 25. Results (MMA then Styrene)<br />
  26. 26. Results (Styrene then MMA)<br />
  27. 27. Results (random)<br />
  28. 28. Conclusion<br /> To conclude, we had to compare between the theory and the real experiment. We have an answer to this which is that the theory’s expected numbers are not same as the one’s in the real experiment. In the theory, the polydispersity number should be 1 for all, however, we got 1.3 or even higher, 2. Therefore, we could say that those two things are two different things. <br /> It has been concluded that the catalyst we used was more suitable for styrene than mma because in the results the polydispersity of styrene was closer to 1; and others it was more than 1.5 which means the catalyst can’t control the process.<br />
  29. 29. The polydispersity of MMA was about 1.92 and for Styrene was about 1.3 . According to the theory, they both should have approximately 1. These are the properties that is the most important. <br />
  30. 30. A BIG THANKS TO…<br />P’ Dear – for helping us throughout the experiment<br />P’ Man – for taking us to MahidolSalaya campus<br />Dr. Ekasith – for allowing the internship to Mahidol<br />& so many other people for helping…<br />