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Operating Regulations for Hydrogen Preparation System

1. General
This hydrogen preparation station is composed by a 5m3/h hydrogen preparation device, a purification device and a storage and filling tank device. The pure hydrogen prepared is used by the electric generator sets. Equipment Specifications: Hydrogen Preparation System Frame I 3000X2000X2450(LXWXH) Material: stainless steel Electrolyzer Hydrogen synthesis tower Oxygen synthesis tower LYE CYC pump LYE filter Pipe coil cooler Dryer Regenesis cooler Frame II (Supply headers) Hydrogen vessel 1844 V=13.9m3 p=32.64kg/cm2 material16MnR Hydrogen drain water seal Frame III (makeup purewater and alkaline solution skid) Water tank Alkali tank Water pump Repetition cooling device Cooling water tank 506 , V=0.219m3 506, V=0.219m3 Q=200L/h CLZ-1002700X1800X1620(LXWXH) V=0.68m3 set set set set set 1 1 1 1 1 108, L=700 1740X1100X1475(LXWXH) set set 1 1 set 3 DQ5/3.2 Q=5Nm3/h set set set set set set set set set 1 1 1 1 1 1 2 2 1 set 1

219, L=1410 219, L=1410 Q=1m3 P=20m 108, L=546 108, L=918 219, L=2000 108, L=918 2180X270X1720(LXWXH)

Cooling pump Heat exchanger (plate type) Gravel for flame arresters Gravel for flame arresters Screen for flame arresters On-line hydrogen leak detector Air tank Nitrogen set

Q=10m3/h p=0.15Mpa(1.53kg/cm2)

set set

2 2 1 1 1 1

DN50 DN15 DN15 MIG219N MIG219N two- transducer p=8kg/cm2 1400 V=3.0m3 V=43~47L 219 p=153kg/cm2 material 37Mn

set set set set

set set

1 8

Rectifier cabinet MCC cabinet Control cabinet

1000X800(LXW) 1000X800(LXW) 1000X800(LXW)

set set set

1 1 1

2. Operating Procedure and Method

2.1 Operation of Hydrogen Preparation Device
2.1.1 Device Cleaning a. The makeup pump shall be started manually at the very beginning. b. Close all valves, add little water into the raw water tank, and then add CC14 for cleaning grease and dirt inside the tank; thereafter, discharge the sewage from the blow down valve. Clean the tank body for 2 to 3 times by raw water with sewage discharged from the blow down valve. Finally fill the water tank with raw water until its full. c. Start the alkali solution pump, and switch the raw water to the hydrogen preparation device; when the liquid level reaches the middle part of the separating section of the hydrogen-oxygen separation scrubber, stop the alkaline solution pump. d. Open the circulating valve, then start the alkaline solution pump and achieve the maximum flow. Stop the pump after 2 to 3 hours circulation cleaning of the system, and open the blow down valve for blowdown unit sewages have been drained away. e. Repeat above steps c and d for 2 to 3 times until the discharged liquid can meet requirements for purity of raw water. f. 2.1.2 Gas Tightness Test g. Close all external linked valves of the hydrogen preparation device (namely valves connecting the frame I with the water tank, the alkali tank and the makeup pump), and open all valves in the device. h. Charge nitrogen gas above the technical pure level into the system through the nitrogen inlet valve (pay attention to the liquid level balance in the nitrogen changing process), boost the pressure to 2.0 Mpa after being confirmed of no leakage point, check gas tightness, then boost the

pressure to 3.2 Mpa, and check for leakage with leak point eliminated. The system pressure shall be maintained for 12 hours and it will be better if the leakage quantity doesnt exceed 6%. Otherwise, the leakage point shall be found out and eliminated until its qualified. i. Start the alkaline solution pump, cycle for 1 to 2 hours, and then stop the pump. j. Open the blow down valve, and release the pressure slowly. The nitrogen pressure shall be utilized for blowdown and pressure relief. k. 2.1.3 Alkaline Solution Preparation l. Close all valves of the alkali tank, inject little water into the alkali tank through the water inlet valve, add CC14 and other substances for alkali tank cleaning, and then wash the tank body by raw water for 2 to 3 times with sewage discharged from the blow down valve. m. 35 kg analytically pure or chemical pure KOH crystalline solid shall be added in for preparing 15% KOH solution. In the preparation process, firstly fill the alkali tank with appropriate amount of raw water, and then slowly add in KOH solid until the KOH has dissolved completely. Slowly open the blow down valve, take the alkali sample by the measuring cylinder, and measure the specific weight until the temperature drops to about 30 .Only when the specific weight reaches 1.18, the KOH solution can be qualified. n. According to steps stipulated in 2.1.1c, switch the 15% KOH solution to the hydrogen preparation device, and stop the alkali circulating pump when the liquid level reaches the middle part of the separating section of the separating scrubber. 2.1.4 For automatic control and rectification operation, please refer to Electrical and Automatic Control Operating Maintenance Manual. 2.1.5 Pre-startup Inspection a. Perform detailed inspection to the outer appearance and surrounding environment of the electrolytic tank, no metal sundries which may lead to short-circuit is allowed to be scattered, and the trough body shall be kept clean and dry. The rectifier cable (or copper bar) shall be in good connection. The process pipeline shall be clean and firm. The blowdown shall be unobstructed and no rainwater leakage shall occur on the building. b. The process pipeline shall be installed and connected correctly in accordance with the flow. And the cooling water pressure shall be able to satisfy the process requirements. c. Inspection to the electrical grounding, the lightning protection device and the gas source shall be performed in accordance with the requirements of the specifications and the instructions. d. Empty it to keep it smooth and guarantee no occurrence of freezing phenomenon. 2.1.6 Diluted Alkali Commissioning a. Connect the power supply and the gas source in accordance with requirements of the Electrical and Automatic Control Operating Maintenance Manual, and set the working pressure at 0.4 Mpa. Turn the startup switch of the makeup pump to the manual shift, set the liquid level interlocking changeover switch at the releasing interlocking gear, and maintain the control system at normal operating status. b. Set the rectifier device at standby state in accordance with the Rectifier System Instructions. c. All valves shall be in the same state as in the gas tightness test, open the nitrogen charging valve, charge nitrogen into the system until the pressure reaches 0.3 Mpa, and then close the

nitrogen charging valve. d. Start the alkaline solution pump and control the circulation quantity at about 0.6 m3/h. e. Set the rectifier cabinet in the steady flow grade, start the rectifier cabinet, and maintain the DC total voltage at 50C (please refer to the Rectifier Cabinet Instructions for operating method). If the trough voltage doesnt exceeding 50V, the DC current shall rise to the set value of 500 A with increasing of the trough temperature. Place the interlocking changeover switch of the upper and lower limit at the interlocking gear. Set the makeup pump at automatic water-feeding shift, and ensure that the water inlet valve and the water tank discharge valve are in the startup sate. f. When the trough temperature reaches 60 , open the cooling water inlet valve and adjust the temperature control; when the trough temperature reaches 80 , the changing trend of the trough temperature shall be observed with the set value of the circulation quantity of the circulating alkali liquid rectified to maintain the trough temperature at about 85 . Under the premise of keeping the trough voltage not exceeding 50 V, the current can be higher, approximately close to the rated current of 500 A. g. 1 hour later after commissioning, when the working pressure is stabilized at 1.0 Mpa and the temperature is at above 50 , the analysis sampling valve can be opened for analyzing concentration of the hydrogen and the oxygen. Please refer to the Analyzer Instructions for operation details. h. Operate for 3 to 4 hours at the operating temperature of above 50 , increase the set value of the working pressure gradually to 3.0 Mpa, and carry out dilute alkali commissioning for over 48 hours. The filter shall be considered to be cleaned when the circulation quantity decreases automatically, and then the operation shall continue. i. Stop operation after dilute alkali operation (refer to section of Normal Stoppage). Discharge the alkali solution from the blow down valve after stoppage. Fill the hydrogen preparation device with raw water, perform circulation cleaning for 2 to 3 times, and then discharge the sewage. j. Clean the alkaline solution filter, and open the valve for blowdown. 2.1.7 Normal Operation a. 70 kg KOH solid with crystal water content lower than or equal to 20% shall be needed for preparing KOH solution with weight concentration of 30%. The specific weight is 1.281 at the temperature of 30 . Meanwhile, 0.5 kg V205 with purity above the additive agent chemical purity needs to be added in. b. The operation steps in this section can take steps in the section of Dilute Alkali Operation as reference. Please note that the total DC current under rated status is 500 A, the operating temperature shall not exceed 90, and the working pressure shall be 3.2 Mpa. c. The operator shall make operating record once every 2 hours, and measure the voltage in the power distribution room once every week. 2.1.8 Normal Stoppage a. Place the manual switch of the makeup pump at manual shift. b. Cut off power supply of the analyzer, and adjust the flow of the analytic gas sample to zero. c. Slowly adjust the total current setting of the rectifier cabinet to zero. d. Keep the liquid levels of the hydrogen-oxygen separation scrubber at basically balanced level. e. Adjust setting of the alkaline solution circulating temperature to

valve, and slowly reduce the pressure setting to zero so as to release the system pressure slowly to zero. g. Stop the alkaline solution pump after continuous operation for 1 to 2 hours. h. Cut off the power supply, the gas source and the cooling water, and close all valves with device stoppage accomplished. 2.1.9 Emergency Stoppage a. In case of emergency stoppage without occurrence of other faults, reduce the DC current of the rectifier cabinet to zero immediately, cut off power supply of the makeup pump and the analyzer, adjust the valves to keep the liquid levels at both hydrogen and oxygen sides at basically balanced position, and keep the system under dwelling state. If the power supply is normal in a short time, the air exhaust valve can be opened, and the machine can be operated according to normal operating steps. But the product air shall be emptied until the system is stable. The product air can only be supplied after being tested as qualified. For long-time stoppage with power connected, the adjusting valve shall be opened manually to release pressure under conditions that the liquid levels at both sides are basically balanced. Other operation steps Ibid. b. In case of emergency stoppage with hydrogen and oxygen emissions required, the system doesnt need to be kept under dwelling state as mentioned above. Reduce the pressure setting of the pressure adjustment to zero to release pressure of the system or open the valve directly to exhaust all residual gas, and exhaust the hydrogen to outdoors through the flame arrestor. c. Stoppage record shall be made after the stoppage for subsequent analysis and processing. In case that the emergency stoppage belongs to equipment failure, careful analysis and elimination of the failure will be required, and the hydrogen preparation device shall be readjusted and put into operation after returning to normal conditions.

2.2 Hydrogen Purification Device and Operation

2.2.1 Start-up Preparation Charge steel cylinder nitrogen gas into the hydrogen purification device from the nitrogen blowing off valve for the purpose of purging and leaking detection so as to replace air in the equipment and pipe. In the purging process, boost pressure of the equipment slowly to 3.2 Mpa, and keep the system under the pressure for 24 hours. Only leakage quantity of no more than 0.5% per hour is thought to be qualified. Finally the nitrogen gas shall be emptied. Repeat the above steps for 2 to 3 times. The air can be purged and emptied only if the pressure is boosted to 0.5 Mpa. 2.2.2 Start-up Operation a. Open the instrument air source inlet on the touch screen, adjust the outlet pressure of the air pressure relief filter to 0.14 to 0.18 Mpa, and adjust the setting pressure of the setter to 0.075 to 0.085 Mpa. b. After half an hour operation, open the analyzer sampling valve, and measure the water and oxygen content in the product hydrogen; after the product hydrogen is tested as qualified, open the hydrogen outlet valve, and close the hydrogen emptying valve. 2.2.3 Stoppage

a. Close the analyzer sampling valve. b. Set the hydrogen preparation outlet valve under emptying state, and close the instrument air source inlet valve. 2.3 Operation of the Injection System 2.3.1 Preparation for Startup a. Purge the hydrogen storage tank and the injection row, and test the leakage quantity (if necessary). 2.3.2 Startup Operation a. Open the product hydrogen outlet valve of the hydrogen purification device to keep the outlet valve under drying status; and the tank filling shall start automatically after the dried hydrogen becomes qualified.

3. Device Maintenance
3.1 Maintenance of Hydrogen Preparation Device
3.1.1 The sealing strip of the electrolytic tank is made of fluoroplastics. Because that under a certain temperature and pressure conditions, the fluoroplastics may become deformed, the sealing strip shall be observed to check whether there is extrusion, distortion or lye leakage phenomenon after a period of operation. In case of poor sealing, the sealing can be kept in good conditions by fastening the tensile screw rod. 3.1.2 The diaphragm of the electrolytic tank adopts asbestos diaphragm. In the operation process, a little of short fibers and impurity particles might drop into the lye, and finally deposit on the filtering screen of the lye filter in the lye circulation process. Therefore, the filtering screen shall be cleaned periodically. The cleaning steps are as follows: a. Open the bypass valve, slowly open the air exhaust valve (pay attention to harms caused by lye splashing), keep the interior pressure of the filter under normal pressure, and close the valve. b. Dismantle the top cover of the filter, take out the filter core, scrub the filtering screen by brush, and then flush it by raw water. c. Open the blow down valve, discharge the foul solution, flush by raw water for 1 or 2 times, discharge the foul solution, and close the valve. d. install the filter core and the top cover, slightly open the air exhaust valve and the alkaline solution inlet valve, close the valve after the lye overflows, open the lye outlet valve, close the bypass valve, and achieve normal lye circulation flow. 3.1.3 After operating for a long period of time, if its found that the heat exchange effect of the heat exchanger becomes poorer, it may be caused by scale formation. Therefore, the device cooling water system shall be treated for scale removal and clearing out. 3.1.4 Please refer to corresponding instructions and materials for electrical, automatic control and

instrument maintenance.

3.2 Maintenance of Hydrogen Purification Device

3.2.1 The gas path system of the device must keep good gas tightness. After being put into operation, the pipe joint and the flange gasket might leak for thermal expansion and cold contraction, therefore shall be inspected regularly.

4. Failure and Elimination

4.1 Hydrogen Preparation Device
Failure Situations 4.1.1 Over a Poor pressure adjustment Re-calibrate the transmitter or Causes Elimination Methods

high trough pressure Failure reach or to rated b Incorrect valve position or blockage of the adjusting valve c Blockage of the gas system d System leakage a Scale formation or blockage of the cooling water system b Incorrect valve position of the

rectify the set value Calibrate the valve position and eliminate blockage Check and eliminate blockage Eliminate leak sources Descale and clear out the cooling water system Calibrate the adjusting valve

pressure 4.1.2 Over

high trough temperature

temperature adjusting valve c Poor adjustment of the temperature adjusting valve d Low cooling water pressure or flow Rectify the set value and examine and repair the transmitter Boost the cooling water pressure and increase the flow e Slightly low alkali circulation quantity 4.1.3 big level difference at both hydrogen and oxygen sides 4.1.4 a Failure of lye pump Too liquid a Poor adjustment of the liquid level regulator b Incorrect valve position of the Increase the circulation quantity Inspect the transmitter and the guide pipe Calibrate the adjusting valve,

adjusting valve, and valve core blockage or leakage at both hydrogen and oxygen sides c Over high trough pressure

eliminate the leakage or exchange the adjusting valve

Inspect in synchronization with steps in 4.1.1 Examine and repair the lye pump

Decrease of lye circulation quantity

b Big filter resistance c Blockage of the alkali circulating system d Gas entry from the suction port of the pump e Over high or low voltage of the power supply f Inaccurate flow indication

Clean the filter Inspect the alkali circulating system and eliminate blockage Empty the gas

Resolve the power supply problem

Inspect the flow meter Calibrate the analyzer to make it return to the normal state

4.1.5 gas index

Low purity

a Abnormal analytic system

b Unqualified chemical composition of raw water or lye c Inappropriate circulation quantity of lye d Inappropriate liquid level e Inappropriate alkali concentration f f Poor sealing of electrolytic tank g Interior blockage of the electrolytic tank h Broken diaphragm asbestos fabric

Replace the lye and use qualified raw water Adjust the circulation quantity

Adjust the liquid level Prepare lye Fasten the electrolytic tank

appropriately Clean the electrolytic tank

Overhaul the electrolytic tank Prepare lye of the appropriate concentration Appropriately increase the operating temperature








electricity consumption of the total electrolytic tank voltage 4.1.7 Big

concentration b Slight low operating temperature

c Inappropriate circulation quantity of lye a Big interior resistance of the

Adjust the circulation quantity

Clean the electrolytic tank

left and right current difference of the

electrolytic tank b Poor contact of the transmission cable system Exchange with new cable or replace the burned cable of small cross section

electrolytic tank 4.1.8 High

c Instrument indication errors

Repair the instrument

a Low operating pressure b Poor gas cooling

Increase the system pressure Increase the cooling water pressure Discharge water by the water drainer Improve the operating status

moisture content in

c Too much condensed water of the gas path d Operating pressure and temperature fluctuation

the product gas

5. Safety Considerations
5.1 The hydrogen preparation station shall be designed by strictly conforming to the national fire
prevention specifications, to ensure safe production. The operator is prohibited to perform the fireuse work without authorization and it is forbidden to smoke in the station.

5.2 Inspect the fire fighting facilities in the station from time to time, to make sure that the
facilities are in good condition. The electrical grounding, the static grounding and the lightning protection facilities shall also be checked periodically.

5.3 Good ventilation shall be maintained in the hydrogen preparation workshop. The hydrogen
detection alarm shall be in good condition, and the supplied data shall be correct and without any error.

5.4 It is better to lay the insulating rubber slab in front of the electrolytic tank, the rectifier
cabinet, the control cabinet as well as the microcomputer working table.

5.5 The operator shall take appointment with certificate after examination, strictly abide by the
operating rules, perform the operating record well and can proficiently judge and quickly tackle the device alarm performance.

5.6 Operators shall be cautious, and wear protection gloves and protection glasses when preparing
the electrolyte, and prepare the boric acid solution with the concentration of 2 % for standby in case of burns.

5.7 When the hydrogen preparation device is stopped for a long time (more than 2 months), the
electrolyte shall be discharged, the raw water shall be filled in the system liquid phase and the nitrogen shall be filled in the gas phase space.

5.8 The emission shall be controlled by using the adjusting valve and the control system as far as
possible when the product air is completed emitted. The opening degree shall not be too large when using the bypass valve to emit, so as to maintain the balance of the liquid level of hydrogen

and oxygen at the two sides.

5.9 Tidiness and oil stain-free shall be maintained, and the hardware is strictly prohibited to fall
onto the electrolytic tank when operating the maintenance equipment.

5.10 Oil-free, dust-free and dryness shall be maintained for the gas source, and the contact
position between the instrument and the medium shall be free of oil and stains.

5.11 The hydrogen preparation station shall be equipped with the special-purpose telephone and
the alarm device. If it is required to perform the emergency shut-down due to failures of equipment, the relevant departments and personnel can be notified through the telephone and the alarming, so as to organize relevant treatment matters well.

5.12 Irrelevant personnel is forbidden to enter the site, and the flammable and explosive materials
shall be far away from the hydrogen preparation station.