Z9 Experimental Procedure

for 3.0L reactor F = 6.6 MPa

D = 4.0 MPa Liner dP/dt fast
Gasfilling (10s) - Formation (20s) –Depressurization (10s) – Thermal stimulation (10s)

This run was done after new volume probe which shows that

a. Reactor volume = 3270 mL

b. Pore volume in reactor = 1438.8 mL
c. Porosity of reactor = 43.0%
d. Criteria for injection: 10kPa/hr drop in gas pressure
e. The plan is to form 40% hydrate, 58% water and 2% gas. As in planning file in H5,
the input will be:
a. Control final reactor pressure at 6600 kPag
b. Vw = mL
c. Conversion is assumed at 95.00%
d. Sand Fill Target = 4937 g Water injection target = 1317.2 mL.
Assuming 99.0 % of gas can be converted into hydrate, and 40% hydrate saturation is
targeted

Gas Filling:

1. Check all venting closed after venting! (one for reactor one for gas storage vessel)
2. Chiller Temperature is set at 15 degrees
3. According to calculation (volume probe), a total of 4930.0g of sand is required to fill up
3270 ml reactor. Sand need to be reduced.
1st fill 2nd fill 3rd fill 4rd fill 5rd fill Final Mass
1540.1 g 1475.0 g 1725.1 g 201.0 40.5 4981.7

4. Reactor dismantling and washing – refilling of gas.

5. Connecting reactor to lines (Torque = 35 ft-lb or 80 N.m)
6. Check all three released values are closed properly. (two at reactor side and one at gas
receiver side).
7. Gas filling data file started at 10s interval. The reactor is first purged (Check valves from
bottom-up) to ~1 MPa (10bar) thrice methane gas to remove any residual air. (V2 to fill,
V7 to purge)
 8. Reactor is pressurized to 6612kPag (corresponding to X.XXX mol, Ptop=6.682MPa,
Pbot=6686kPa, Ta4=14.86,Tb4=14.50,Tc4=15.08) and allowed to stabilize at 15.01 deg
C. V6 was open to maintain consistency in experimental procedures.
9. Perform leak check on the top & bottom fittings (4 key places). Check if external
cylinder is closed.
Water Injection:
10. In Formation file t = 60 s, 1st Injection at 30 ml/min at 15 deg C from V8 was done:

Duration time Start volume Rate*time (ml/min*min) End Pressure

14’30’’ 495.47 mL 435.00 9.088MPa
flowrate End volume Δ Volume (mL)
30 mL/min 60.79 mL 434.68

Time 3:04 pm
Total Water Injection at first time 435.0 mL
To start a new file with name “hydrate formation
11. 2nd water injection when Ptop = 3478 MPa Pbot = 3482 MPa, at 30ml/min.

Duration time Start volume Rate*time (ml/min*min) End Pressure

14min30s 494.87 mL 435 5.923 MPa
flowrate End volume Δ Volume (mL)
30 mL/min 60.30 mL 434.57

Duration time Start volume Rate*time (ml/min*min) End Pressure

6min50s 260.58 mL 205 8.980 MPa
flowrate End volume Δ Volume (mL)
30 mL/min 56.13 mL 204.45
Total Water Injection at second time = 435+205=640.0ml
Total Water Injection at first time 435.0 + 640 = 1075mL

12. 3rd water injection when Ptop = 3.336 MPa, Pbot=6.543MPa, at 30ml/min.
Duration time Start volume Rate*time (ml/min*min) End Pressure
X min XX s 237.06 mL 178.5 ml 9.058 MPa
flowrate End volume Δ Volume (mL) Stable Pressure
30 mL/min 68.02ml 169.04 Top=4.414MPa,
Bot=5.116MPa

Total: 1075+169.04 = 1244.04 g

13. Increase T from 1 C to 5 C to 6 C and stabilize at Ptop = 7370 kPa Pbot = 7379 kPa.
Depressurization
Final Pressure: Ptop = 3036.33 kPa Pbot = 2995.7 kPa PGR = 2054.47 kPa Water mass = 355.9 g

Purge Step:

Learning: Gas cylinder pressure is set as 3.5 MPa and this is believed lead to CV open more than
usual, thus the final pressure attained is at 2.0 Mpa and is less than 4.0 Mpa. Thus, the data cannot
be used for production profile. Learning is that we need to control gas cylinder pressure around 1.0
bar (not more than 2,0 bar) to supply air to CV. Otherwise, CV is not controlling at the later part. In
addition, try dissociation during the day instead of night. If anything went wrong, we can still fix it.