Reactor Cleaning

1. Disassemble reactor. When removing cooling water hoses, do not get water in reactor. Remove gas outlet (but not the inlet). Remove very bottom screw on outer ring. Loosen all six screws on inner ring, alternating to not put more pressure on one side. Use lift to lift up reactor and pick up outer ring. Remove both halves on inner ring. Shift mixer to one side and pull out thermocouples. Pull out inside of reactor and place on stand.
2. Recover all of the catalyst as is possible and store in used catalyst bottle. Dry it with nitrogen to remove solvent.
3. Clean inside of reactor with cyclohexane. Scrub with green scotch pads gently.
4. Clean catalyst filter with cyclohexane and wash filtering container.
5. Clean all of screws and other parts for reactor by putting in THF in the sonicator for 1 hour.
6. Fill reactor ¼ full with cyclohexane.
7. Pressurize to 100 psi N2 and then depressurize. Repeat 4 times. Pressurize at 100 psi.
8. Turn on cooling water and stirrer to 250 rpm. Set temperature to 60 oC and watch to make sure that temperature controller is working. Press reset button to reset the high temperature limit. Double check to see that thermocouples are in place. (Very Important!!)
9. When finished, turn off heater and stirrer and drain out cyclohexane.

Sample Preparation

1. Dissolve polymer sample in 100 mL cyclohexane for every 1 g polymer. Stir overnight.
2. Directly before hydrogenation, blow N2 on solution for 1 hour while stirring to remove air in solvent.

Reactor Set-Up

1. Put catalyst in oven for 2 hours (or overnight if preparing ahead of time) at 400 oC (ramp 100 oC every hour for 4 hours).
2. Turn off cooling water. Remove the two clear water lines (without spilling water on reactor).
3. Shift stirrer out of the way and remove the thermocouples.
4. Remove the other two cooling water lines (remember to stabilize with a second wrench.)
5. Disconnect the exit gas line (leave entrance line in place) and open the outlet valve to equalize the pressure inside.
6. Undo the bottom screw on the outer ring.
7. Remove the six screws on the inner ring, slowly loosening them in alternating order.
8. Lift up reactor with lift.
9. Remove both halves of inner ring.
10. Lift out inside of reactor and place on stand (be careful not to tip so no water falls in reactor).
11. Wipe inside of reactor until it is dry (to remove excess cyclohexane).
12. Get weighing paper ready on scale and polymer solution near reactor.
13. Remove catalyst from oven.
14. Weight out same weight of catalyst as polymer was used.
15. Pour polymer solution into reactor.
16. Carefully pour catalyst into reactor.
17. Put top back on reactor and immediately open N2 inlet and outlet valves (make sure it is N2 and not H2).
18. Replace the inner ring and all screws. Make sure it is lines up correctly so that all can be accessed.
19. Line up bottom screw with hole and tighten.
20. Turn off N2 inlet. Connect exit gas line.
21. Pressurize to 100 psi N2 and then depressurize. Repeat 4 times.
22. Connect all water lines. Put stirrer into position (make sure black connection is loose) and replace thermocouples (important!)
23. Turn on cooling water (keep checking rate as it will decrease)
24. Turn on motor to 250 rpm. Make sure that it is not making any unusual noises or is obstructed.
25. Pressure with N2 and then depressurize. Repeat 4 times.
26. Pressurize to 100 psi with N2.
27. Heat to 50oC.
28. Hit reset button for high temperature limit.
29. Watch to make sure that temperature control is working and double check to make sure that thermocouples are in.
30. Leave it for approximately one hour.
31. Assemble filtering apparatus in the following order: bottom plate, ringed piece (straight pieces facing down), blue screen, four filters (11, 8, 5, 1) and top piece. Screw it together and heat to 60 oC. (Top filter is largest pore size)

Hydrogenation Reaction – First Day

1. Check to make sure that pressure did not leak.
2. Switch the H2/N2 valve to the off position.
3. Depressurize reactor. Pressurize reactor to remove N2 from line. Depressurize reactor.
4. Check H2/D2 valve and choose desired gas.
5. Make sure that all exit valves are closed on reactor.
6. Open valve on top of H2 (D2) cylinder. Open green valve on line to reactor.
7. Point H2 (D2) /N2 valve to H2 (D2).
8. Pressurize to around 50 psi.
9. Check to see that N2 has at least 500 psi of gas. If not, replace cylinder before proceeding.
10. Open N2 outlet valve to a very high flow rate (need to dilute the H2 (D2) that will be released so that it is below the upper flammability limit)
11. Let H2 out very slowly. When most of it is gone, slowly decrease the N2 rate until all of the gas is removed.
12. Close all outlet valves.
13. Repeat steps 8-11 (only for H2 – do not repeat for D2 to conserve D2).
14. Fill reactor to 500 psi with H2 (use 300 psi for D2).
15. Close valve on H2 tank and green valve on H2 line.
16. Check cooling water rate.
17. Set T to 85oC (want actual temperature to be about 90 oC)
18. After temperature has reached 90oC, check to make sure that pressure has not gone down.
19. Wait at least a half-hour and check pressure, temperature, and cooling water rate.
20. Leave overnight

Second Day

1. Put catalyst in oven at 400 oC (or use catalyst that has already been regenerated).
2. Put filter in oven at 60 oC (can do this the night before if oven is free) (only if filtering a polymer at 60oC)
3. Gradually cool reactor down to 60 oC (or room temperature if not filtering hot).
4. Check to make sure there is at least 500 psi of N2 gas in cylinder.
5. Open N2 exit valve.
6. Purge all H2 out of reactor very slowly
7. Turn N2/H2 valve to off.
8. Fill reactor to remove H2 from line.
9. Turn on N2 exit valve.
10. Purge out H2 from reactor
11. Switch H2/N2 valve to N2
12. Fill to 100 psi with N2
13. Turn on N2 exit valve and purge reactor
14. Fill to 100 psi with N2
15. Purge reactor
16. Pressurize to 50 psi (not more than 100 psi) with N2
17. Turn off heater (if reactor is not at room temperature)
18. Remove bottle and filter from oven (if filtering hot)
19. Filter polymer into bottle
20. Turn off stirrer
21. Repressurize with N2 to 50 psi and filter again.
22. Close sample bottle and remove filter.
23. If IR/NMR (see below) shows peaks for double bonds, repeat steps from "Reactor Set-up" through Day 1.
24. Continue process until all C=C bonds have been saturated. If using D2, switch to H2 after one or two days of saturation (assuming it is around 99% complete at that time.)