CN107930537A - A kind of simulated sea bottom methane leakage causes the reaction unit and method of early diagenesis - Google Patents

Abstract

The invention discloses a reaction device for simulating early diagenesis caused by seabed methane seepage, including a reaction system; a gas pressurization subsystem connected to the reaction system and a reaction solution liquid supply subsystem; a gas-liquid collection system, a gas-liquid The collection system is connected to the outlet of the reaction system. A back pressure system is set between the gas-liquid collection system and the reaction system. The back pressure system provides a pressure difference between the gas-liquid collection system and the reaction system to control the gas-liquid collection after the reaction. By simulating the early diagenesis caused by methane leakage through this device, we can better understand the marine environment and biogeochemical reaction process, which has important guiding and indicating significance for the specific geochemical analysis of the ocean.

Description

A reaction device and method for simulating early diagenesis caused by seabed methane seepage

technical field

The invention relates to the technical field of marine oil and gas geochemical exploration, in particular to the research field of simulating methane seepage in seabed hydrate storage areas.

Background technique

Natural gas hydrate is the most potential alternative energy after shale gas and coalbed methane. Natural gas hydrate, as a brand-new, high-efficiency and clean energy with great potential, is considered as an alternative energy in the 21st century. In 2007 and 2009, China obtained natural gas hydrate physical samples in the South China Sea and the Qilian Mountains permafrost on the Qinghai-Tibet Plateau. It is predicted that the reserves of natural gas hydrates are more than twice that of oil reserves. In 2017, the trial production of natural gas hydrate in the South China Sea was carried out in my country and a breakthrough was achieved.

In the favorable area of natural gas hydrate, due to the decomposition and release of hydrate, the methane seepage (cold seep activity) is ubiquitous on the seabed, and the seeping methane can penetrate the overlying rock layer/sedimentary layer and slowly and continuously seep to the seabed surface , and react with sulfate ions, nitrate ions, and redox-sensitive elements such as iron and manganese in the sediment pore water under the action of microorganisms, and the most important reaction is sulfate reduction-methane anaerobic oxidation (AOM), the generated bicarbonate combines with calcium and magnesium ions in the pore water to form authigenic carbonate rock. A series of geochemical processes through methane seepage lead to sediment and pore water geochemical anomalies, which are the theoretical basis for us to identify underlying oil and gas reservoirs/gas hydrate geochemical exploration. Submarine methane seepage represents the migration of deep oil gas/hydrate from the source area or reservoir to the seabed surface, which belongs to cold seep activity. Therefore, the seepage process of seabed methane is complicated, and a series of complex reactions occur with shallow seabed sediments and water. Although seabed methane seepage (cold seep activity) is ubiquitous, there is still a lack of understanding of the mechanism of seabed methane seepage and the series of reactions between methane and anions and cations in pore water under the action of microorganisms, their products and early diagenesis, which directly affect Geochemical identification and exploration effects of marine oil and gas/gas hydrate. The proposed reaction system for simulating the early diagenesis of seabed methane seepage is one of the effective technical means to solve this problem.

At present, the research on the methane seepage caused by the decomposition of natural gas hydrate and its series of geochemical reactions with anions and cations in pore water under the action of microorganisms and its products and early diagenesis has just started. In view of the complexity of methane seepage (cold seep activity) Therefore, it is necessary to conduct research on pore water and authigenic carbonate rock geochemistry in the cold seep active area of the South China Sea, supplemented by relevant indoor simulation experiments. There are not many simulation experiment systems for seabed methane seepage and its early diagenesis in China, and the existing experimental devices mainly simulate the formation and decomposition of hydrates, which cannot reflect the series of geochemical reactions caused by methane seepage in seabed sediments and the early diagenesis. It is difficult to qualitatively and quantitatively study the early diagenesis caused by methane seepage in the hydrate occurrence area.

Invention patent content

Aiming at the above problems, the present invention proposes an experimental device and method capable of simulating the cold seep environment of seabed methane seepage, and for studying early diagenesis of methane seepage.

In order to achieve the above object, the present invention provides the following technical solutions:

A reaction device for simulating early diagenesis caused by seabed methane seepage, including a reaction system;

Connected with the reaction system to provide a pressure-regulated gas pressurization subsystem for the reaction system;

A reaction solution liquid supply subsystem that is connected to the reaction system and provides a reaction solution supply for the reaction system;

It also includes a gas-liquid collection system, the gas-liquid collection system is connected to the outlet end of the reaction system, a back pressure system is set between the gas-liquid collection system and the reaction system, and the back pressure system is a gas-liquid collection system A pressure difference is provided between the system and the reaction system to control gas-liquid collection after the reaction.

The gas pressurization subsystem includes a methane gas source, an air compressor, a booster pump, and a gas storage tank. The methane gas source, booster pump, and gas storage tank are connected in sequence through a pipeline with a control valve. The air The compressor is connected to the booster pump through a pipeline with a pressure regulating valve and a control valve, and the gas storage tank is connected to the reaction system through a pipeline with a pressure regulating valve, a one-way valve and several control valves. A gas mass flow controller is arranged between the gas storage tank and the reaction system.

The reaction solution liquid supply subsystem includes a liquid container with a piston and a microbial container with a piston. Both of the liquid container with a piston and the microbial container with a piston are connected to a constant-speed constant-pressure pump through a pipeline with a control valve at one end. One end is connected to the reaction system through a pipeline with a control valve, and the constant speed and constant pressure pump is connected to a liquid container filled with distilled water for providing pump liquid to the constant speed and constant pressure pump.

The reaction system includes a reaction kettle placed in a high-low temperature constant temperature box. The reaction kettle is provided with visual windows that are symmetrical to each other up and down, the top of the reaction kettle is provided with a gas sampling port, and the side of the reaction kettle is provided with A number of liquid sampling ports, the liquid sampling ports are distributed at different heights, a thermometer and a number of conductivity sensors are also arranged on the side of the reaction kettle, and the gas pressurization subsystem and the reaction solution liquid supply subsystem respectively pass through A pipeline with a control valve connects the upper and lower ends of the reactor.

The top of the reaction kettle is also provided with a safety valve and a gas storage tank. One end of the gas storage tank is connected to the top of the reaction kettle through a pipeline with a control valve, and the other end is connected to the gas pressurization subsystem through a pipeline with a valve.

The reactor is a visible Hastelloy reactor.

The collection system includes a gas-liquid separator, the top of the gas-liquid separator is connected to a gas flow meter through a pipeline with a control valve, and the bottom of the gas-liquid separator is connected to a production fluid metering system through a pipeline with a control valve.

The back pressure system includes a back pressure valve, a back pressure container, a hand pump and a back pressure liquid container connected in sequence through pipelines, and a pressure gauge is set on the pressurized container.

At the same time, a corresponding method for simulating the reaction of seabed methane seepage leading to early diagenesis is provided, including the following steps:

Step 1: Check whether the reaction device is normal, whether there is air leakage in each pipeline and each valve;

Step 2: Add solid sediment/quartz sand sample to the reactor;

Step 3: Open the reaction solution supply subsystem, and adjust the pressure through the constant speed and constant pressure pump

Function, inject the reaction solution in the liquid container with piston into the reaction kettle;

Step 4: Through the pressure regulation of the constant speed and constant pressure pump, the microbial container with piston

Microorganisms are injected into the reactor;

Step 5: Start the high and low temperature thermostat to make the temperature in the reactor reach the set temperature value;

Step 6: Set the experimental pressure value and the pressure value of the back pressure system;

Step 7: Turn on the gas pressurization subsystem to make the methane gas input in the gas storage tank reach the set value.

fixed pressure value;

Step 8: The reaction substance reacts in the reactor, and the pressure in the reactor is controlled in real time within the set range;

Step 9: Collect water samples and gas samples by adjusting the pressure difference every 0.5-12 hours until the reaction ends.

The gas-liquid flow rate during the reaction process can be controlled by the pressure difference between the gas pressurization subsystem, the reactor and the back pressure system, and the methane consumption and liquid discharge can be measured by the metering system.

The beneficial effects of the present invention are:

Through the reaction device simulating the early diagenesis mechanism of seabed methane seepage to simulate the early diagenesis caused by methane seepage, we can better understand the marine environment, understand the global carbon cycle, understand early diagenesis and biogeochemical reaction process, indoor simulation Under the action of microorganisms, methane undergoes a series of geochemical reaction processes with anions and cations in the water body and its products have important guiding and indicating significance for the specific geochemical analysis of the ocean.

Description of drawings

Fig. 1 is a schematic diagram of a reaction device for simulating early diagenesis of seabed methane seepage according to the present invention.

Each reference mark in the figure is:

1. 1-methane gas source, 2-air compressor, 3-gas booster pump, 4-gas storage tank, 5-gas mass flow controller, 6-check valve, 7-high and low temperature thermostat, 8- Reactor, 9-liquid container with piston, 10-microbial container with piston, 11-constant speed constant pressure pump, 12-liquid container, 13-safety valve, 14-methane alarm, 15-vacuum pump, 16-buffer tank, 17-back pressure container, 18-hand pump, 19-back pressure liquid container, 20-gas-liquid separator, 21-gas flow meter, 22-production liquid metering system, 23-vent valve, 24-back pressure valve , 25-sapphire window, 26-temperature sensor, 27-conductivity sensor, 28-sampling port, 29-air intake port, 30-inlet pressure controller, 31-first pressure regulating valve, 32-second pressure regulating valve;

2. Pressure gauge P1-P6;

3. Control valve Z1-Z38.

Detailed ways

The content of the present invention will be described in further detail below in conjunction with the accompanying drawings and specific embodiments.

Example 1: (5°C, 10MPa)

As shown in Figure 1, a reaction device for simulating early diagenesis caused by seabed methane seepage includes a gas pressurization subsystem, a reaction solution liquid supply subsystem, a reaction system, a back pressure system, and a gas-liquid collection system.

The gas pressurization subsystem includes: methane gas source 1, 4 pressure gauges (P1, P2, P3 and P4), 4 control valves (gas cylinder high-pressure inlet valve Z25, driving gas inlet valve Z26, high-pressure gas outlet valve Z27 and Pressure reducing valve outlet valve Z24), 2 pressure regulating valves (31 and 32). (Cylinder pressure: pressure gauge range 16MPa, precision 1.6 (1.6% of full scale); control the pressure of the driving gas (ie compressed air): pressure gauge range 1.6MPa, precision 1.6; outlet pressure is the outlet of the booster pump (that is, the pressure of the gas storage tank): the pressure gauge range is 60MPa, and the accuracy is 1.6; the pressure regulating pressure is the outlet pressure of the pressure regulating valve: the pressure gauge range is 60MPa, and the accuracy is 1.6; the conversion relationship between the driving gas and the final pressure gas is: 60 x driving air pressure = final pressure.)

The specific operation of the pressurization process: turn on the power of the air compressor 2, start the air compressor 2, the first pressure regulating valve 31, and adjust the output pressure of the air compressor 2 to the predetermined driving pressure (0.1MPa) through the pressure gauge P2. After reaching the predetermined driving pressure, the air compressor 2 is automatically closed; the valve Z25 of the methane gas source 1 is opened, and the value displayed by the pressure gauge P1 is the pressure value of the methane source 1. Open the valve Z24 at the end of the air compressor 2, the booster pump 3 starts to work under the driving pressure, and starts to pressurize the methane gas source. Open the valve Z26, the pressurized gas will be delivered to the gas storage tank 4, and the pressure gauge P3 displays the pressure in the gas storage tank 4. After a certain period of time, the pressure in the gas storage tank 4 rises to a predetermined pressure (1-30 MPa). After the pressurization is completed, turn off the methane gas source valve Z25, turn off the air compressor output valve Z24, turn off the air compressor 2, and close the valve Z26.

Reaction solution liquid supply subsystem: prepare the reaction solution (simulated seawater solution) in advance for use. Reset the piston of the liquid container 9 with piston to the bottom of the container, that is, use the high-pressure gas in the gas storage tank 4 to reset the piston of the liquid container 9 with piston, the specific operation is: open the valves Z27, Z21, Z7, Z13, Z14, Z10 And vent valve Z6, slowly adjust the second pressure regulating valve 32, control its outlet pressure at several atmospheres, then under the action of air pressure, the middle piston can be pushed to the bottom of the liquid container 9 with piston, then all valves are closed, and the The second pressure regulating valve 32 is reset. Open the liquid container 9 with a piston, pour in a sufficient amount of reaction solution, and cover the liquid container 9 with a piston. Add about 500ml of distilled water to the liquid container 12 as the pump liquid at the liquid inlet end of the constant pressure constant speed pump 11 . Turn on the constant pressure and constant speed pump 11, set the pumping pressure of 0.5MPa, start the constant pressure and constant speed pump 11, and start to suck the pump liquid from the liquid container 12; Pressure constant speed pump 11 suspends work. At this time, the control valves Z4, Z10, Z14 and Z18 are opened, and the reaction solution in the liquid container 9 with a piston can be input into the reaction kettle 8.

Reaction system: including high and low temperature constant temperature box 7 (working temperature: range -20～100°C, temperature control accuracy: ±0.1°C), visual Hastelloy reaction kettle 8 and reaction kettle 8 set in high and low temperature constant temperature box 7 There are 4 imported sapphire high-pressure visual windows 25, 7 sampling ports Z31-Z37, gas sampling port 29, temperature probe 26, 5 conductivity probes 27, upper sampling port Z17, lower sampling port Z18, upper outlet Sample port Z19, bottom sample port Z20, and drain port Z30.

Reactor temperature control: open the high and low temperature thermostat 7, and set the temperature at -20 to 20°C. When the temperature of the reaction solution in the reactor 8 reaches a stable temperature (about 10 hours), the reactor 8 can be pressurized. The pressurization operation of the reactor is as follows: open the valve Z27, adjust the pressure regulating valve 32, and adjust the outlet pressure of the gas storage tank 4 (such as 1 MPa). Open the valves Z21, Z7, Z13 and Z17 in sequence to transport the high-pressure gas in the gas storage tank 4 to the reactor 8, and the pressure in the reactor quickly reaches the set value. The temperature in the reactor 8 temporarily rises due to the high-pressure gas input. After the high and low temperature thermostat 7 cools down for a period of time, the temperature in the reactor 8 is reduced to the set temperature before pressurization. Slowly adjust the second pressure regulating valve 32 to increase the outlet pressure, so that the pressure in the reactor 8 gradually increases to the predetermined experimental pressure. The gas is repeatedly inflated many times to make its pressure and temperature reach the predetermined pressure and temperature conditions.

The gas-liquid collection system includes a gas-liquid separator, the top of the gas-liquid separator is connected to the gas flowmeter through a pipeline with a control valve, and the bottom of the gas-liquid separator is connected to the production liquid metering system through a pipeline with a control valve.

The back pressure system includes a back pressure valve, a back pressure container, a hand pump and a back pressure liquid container connected sequentially through pipelines, and a pressure gauge is set on the pressurized container.

Microbial injection: open the control valve Z28 at the top and bottom of the microorganism container with piston 10, and manually reset the piston in the microorganism container with piston 10 to the bottom of the piston (or, when the reactor 8 was in high pressure state, open the valve at the bottom of the microorganism container with piston 10). Control valve Z28, then slightly and slowly open microbial valve Z29, using high pressure gas to push the piston to its bottom). After the piston is pushed to the bottom of the microbial container 10 with the piston, connect the pipeline at the bottom of the microbial container 10 with the piston, and then close the microbial valve Z29 and the control valve Z28. Prepare a nitrogen cylinder equipped with a pressure reducing valve, and connect it with a temporary pipeline to the top of the microbial container. Slowly adjust the pressure regulating valve to control the outlet pressure of nitrogen gas, so that the gas can be output gently. Use 75% alcohol solution to wipe the operator's hand, and carry out disinfection and sterilization treatment to the microorganism container 10 with piston, to reduce the interference of the microorganisms on the hands of the operator and in the air mixed to the injected microorganisms during the microorganism addition process. Adjust the position of the nitrogen outlet so that it can quickly dry the alcohol disinfectant. After drying, keep the nitrogen blowing out continuously. Prepared microbial solution 50ml is poured into the microorganism container 10 with piston, and in the process of pouring the solution, covering and connecting pipe valve parts, it is necessary to ensure that the nitrogen gas is continuously blown off the microbial container 10 with piston. Next, start the constant pressure and constant speed pump 11, open the control valves Z4, Z29, Z10 and Z14, and first set the pressure of the constant pressure and constant speed pump 11 slightly higher than the predetermined experimental pressure of the reactor 8. When the constant pressure and constant speed pump 11 stops working, it means that the pressure in the pipeline has reached the set pressure. Open the control valve Z17, the pressure of the constant pressure and constant speed pump 11 will be slightly reduced, and the microbial solution in the microbial container 10 with piston will be transported from the top of the reactor 8 to the reactor. When the pressure of the constant pressure and constant speed pump 11 is constant, it means that the piston has reached the top of the microorganism container 10 with the piston, and the injection is completed. Close the control valves Z4, Z29, Z10, Z14 and Z17 in sequence.

Data collection of temperature, pressure, etc. during the experiment:

Turn on the computer, start the data acquisition software on the desktop, open the communication between the software and the data acquisition card, and you can see the collected display results of temperature 26 , pressure, resistivity 27 , etc. in the data acquisition software. Set data saving: In the data saving tab, set the location of data saving, the name of the data file, and the data saving interval (s). After clicking start saving, an excel data file will pop up automatically for data saving. After the experiment is over, click to stop saving, and the software will automatically save the data and close the excel file automatically. The data is saved.

Collection and testing of gas and liquid samples during experiments:

Gas sampling: The gas sampling work in the experiment can be completed at the gas sampling port 29 at the top of the reactor 8, specifically: connect the gas sampling bag, slowly open the gas sampling port 29 valve Z38, and close it when the required volume of gas is obtained. The control valve Z38 of the air intake port 29. Remove the gas sampling bag for testing.

Liquid sample: during the experiment, the water sample was sampled at the sampling port 28 on one side of the reaction kettle 8 . The specific operation is: take some clean small conical flasks, hold the small conical flasks in the left hand, and slowly open the seven outlet valves Z31-Z37 of the sampling port 28 to take samples in sequence with the right hand, and close the valves Z31-Z37 in sequence when the predetermined volume is reached. Sampling at different positions on the side wall of the reaction kettle 8 can monitor the change of the chemical composition of the solution at different depths of the reaction kettle 8 in real time, and react to simulate the geochemical process in the seabed methane seepage environment.

The collection and chemical composition test of the effluent in the production liquid metering system 22 under the flow test conditions, and the test of the gas composition collection from the gas flow meter 21 .

After the experiment, solid samples of the sediment (quartz sand) at different depths in the reactor 8 were taken for component and microstructure analysis to study the early diagenesis process in the methane seepage environment.

Reactor 8 gas pressure relief at the end of the reaction: connect the movable exhaust pipe to the outlet of the gas flow meter 21, and move one end of the movable exhaust pipe to the window; open the valve Z19, adjust the hand pump 18 of the back pressure system, and turn the hand pump The pressure gauge P6 slowly decreases in stages, and the high-pressure gas in the reactor 8 is eliminated in stages. Open the valves Z11 and Z22, and the discharged gas will be discharged after gas-liquid separation. Quick pressure relief: connect the movable exhaust pipe to the vent valve Z12 of the reactor, and move one end of the movable exhaust pipe out of the window; open the valve Z19, adjust the hand pump of the back pressure system, and slowly set the pressure of the hand pump instrument in stages Reduce, and remove the high-pressure gas in the reactor in stages.

The reaction solution in the reaction kettle 8 is discharged (use the high-pressure gas of the increasing system to press out the water): connect the movable drain pipe to the vent valve Z30 at the bottom of the reaction kettle 8, and empty the beaker at the other end to fill the waste liquid. Open the valve Z27, adjust the second pressure regulating valve 32, adjust the outlet pressure of the gas storage tank to 0.3MPa, open the valves Z21, Z7, Z13 and Z17, and press the water out due to the gas pressure.

Reactor, microbial injection container and pipeline cleaning:

Cleaning of the liquid container 9 with piston: open the valves Z4 and Z8, set the pressure of the constant-speed constant-pressure pump to 0.3 MPa, start the constant-pressure constant-speed pump 11, and discharge the remaining liquid in the liquid container 9 with piston; the liquid container 9 with piston After the liquid in the tank is discharged, close the valve Z8; open the valve Z27, adjust the second pressure regulating valve 32, open the valves Z21, Z7, Z13, Z14, Z10 and Z6, use the pressure in the gas storage tank 4 to turn the liquid container with piston Push the piston in 9 to the bottom, and after the piston reaches the bottom, close the valves Z27, Z21, Z7, Z13, Z14, Z10 and Z6 in sequence; open the liquid container 9 with the piston, pour distilled water into it, and clean the inner wall repeatedly, using the siphon method Suck out the cleaning solution; after three times of cleaning, pour a small amount of distilled water (about 500ml), and cover the reaction solution container. Start the constant pressure and constant speed pump 11, open the valves Z4, Z10, Z14 and Z17, drive distilled water to flow through the pipeline, and clean the pipeline at one end of the valve Z17. After the pipeline at one end of the valve Z17 is cleaned, the valve Z17 is closed, and the valve Z18 is opened to clean the pipeline therein. After the pipeline at one end of the valve Z18 is cleaned, the valve 18 is closed. Open the reaction kettle 8, and use distilled water to repeatedly clean the inner wall of the reaction kettle 8. Use a siphon to suck out the wash solution. Connect other pipelines of the reactor 8, use nitrogen to blow off the pipelines in the reactor to ensure that the containers, pipelines and reactors are dry.

The specific operation of the reaction device for simulating seabed methane seepage leading to early diagenesis is as follows:

Prepare experimental materials, configure simulated seawater solution, prepare methane anaerobic oxidizing bacteria and sulfate radical reducing bacteria solutions, distilled water, South China Sea sediment samples, methane gas source, high-purity nitrogen, etc.

Methane gas source 1, air compressor 2, gas booster pump 3, gas storage tank 4, gas mass flow controller 5, check valve 6, high and low temperature thermostat box 7, visible Hastelloy reactor 8, with Piston liquid container 9, with piston microbial container 10, constant speed and constant pressure pump 11, liquid container 12, safety valve 13, methane alarm 14, vacuum pump 15, buffer tank 16, back pressure container 17, hand pump 18, back pressure Liquid container 19, gas-liquid separator 20, gas flow meter 21, production liquid metering system 22, namely balance, vent valve 23, back pressure valve 24, temperature sensor 26, five conductivity sensors 27, inlet pressure controller 30 , the first pressure regulating valve 31 and the pressure regulating valve 2 are connected with pipelines and valves, all valves are closed, all sensors, probes and instruments are connected to the data collector, and connected to the computer through the data collector.

Turn on the main power switch of the reaction device, check whether the circuits, instruments, valves and sensors are working normally, and check whether the instruments, pipelines and valves are leaking;

Place the pistons of the liquid container 9 with the piston and the microorganism container 10 with the piston at the bottom, and fill the prepared simulated seawater solution and microbial solution;

Open the upper cover of the reaction kettle 8, add about 3/5 of the volume of the sediment/quartz sand sample, then cover the upper cover, and connect the various pipelines connected to the reaction kettle 8.

Open the switches of valves Z3, Z16, Z17, Z18, Z13, Z14, Z10, Z8, Z29, Z21, Z7 and vacuum pump 15 to carry out reaction kettle 8, buffer tank 16, gas storage tank 4, liquid container with piston 9, belt Piston microorganism container 10 and pipeline are evacuated, and the pressure of band pressure gauge P5 is-0.1MPa is to close vacuum pump 15, and closes all valves.

Add about 500ml of distilled water to the liquid container 12 as the pump liquid at the liquid inlet end of the constant pressure constant speed pump 11 . Turn on the constant pressure and constant speed pump 11, set the pumping pressure of 0.5MPa, start the constant pressure and constant speed pump 11 to start working, and suck the pump liquid from the liquid container 12; when the pressure at the outlet end of the constant pressure and constant speed pump 11 reaches 0.5MPa, Constant pressure and constant speed pump 11 suspends work. Now, open the valves Z4, Z10, Z14 and Z18, the reaction solution in the liquid container 9 with the piston can be input into the reactor 8, when the liquid in the reactor 8 is filled with 4/5 volume of the reactor 8, close the constant Pressure constant speed pump 11, close valves Z4, Z10, Z14 and Z18.

Start the constant pressure and constant speed pump 11, open the valves Z4, Z29, Z10, Z14 and Z17, and transport the microbial solution in the microbial container 10 with the piston to the reactor from the top of the reactor 8. Reactor 8 is filled with liquid, and the injection is complete. Close valves Z4, Z29, Z10, Z14 and Z17 in sequence.

Start the high and low temperature incubator 7 to make the temperature in the reaction kettle 8 reach the set temperature of 5°C.

Utilize the hand pump 18, the back pressure liquid container 19 and the back pressure container 17 to set the pressure value of the pressure gauge P6 of the back pressure system at 10MPa.

Start the air compressor 2, adjust the pressure regulating valve 31, and adjust the driving pressure output by the air compressor 2 to a predetermined driving pressure (20MPa) through the pressure gauge P2. Open the valve Z25 of the methane source 1, open the valve Z24 of the air compressor 2, and start boosting through the booster pump 3. Open the valve Z26, the pressurized gas will be delivered to the gas storage tank 4, and the pressure gauge P3 displays the pressure in the gas storage tank 4. Wait for the pressure in the gas storage tank 4 to rise to a predetermined pressure (20MPa). After the pressurization is completed, turn off the methane gas source valve Z25, turn off the air compressor output valve Z24, and turn off the air compressor 2.

Set the experimental pressure to 10MPa through the second pressure regulating valve 32, open the valve Z27, adjust the second pressure regulating valve 32, open the valves Z21, Z5, Z9, Z13, Z18, gas mass flow controller 5 and check valve 6, The gas will be delivered to the reactor 8, and the pressure in the reactor 8 reaches a predetermined value (10MPa), and the valves Z27, Z21, Z5, Z9, Z13, Z18 are closed.

Pressurize the pressure in the gas storage tank 4 to 20MPa again, open the valve Z27, adjust the pressure value of the pressure regulating valve 32 to 10.2MPa, open the valves Z21, Z5, Z27 and Z18, and the gas will be delivered to the reactor 8. Add about 100ml of distilled water to the back pressure liquid container 19 at the liquid inlet end of the back pressure system, slowly shake the hand pump 18, and adjust the pressure in the back pressure system to 10MPa (reading of pressure gauge P6). Open the valve Z19, wait for the pressure of the reactor 8 to be slightly greater than the value (10MPa) of the pressure gauge P6 of the back pressure valve, the gas or gas-liquid in the reactor 8 will flow out, and flow to the gas-liquid separator 20. The gas flow meter 21 measures the amount of outflowing gas, and after the measurement is completed, it is safely discharged to the outside; the liquid will flow out into the water container, and the produced liquid metering system 22 (balance) can measure the quality of the outflowing liquid. Slightly adjusting the pressure regulating valve 32 can control the outlet pressure of the gas storage tank 4, and can control the velocity of methane flowing upward from the bottom of the reactor 8 under the corresponding pressure difference.

When the rate is constant, the experimental operation under the condition of methane flow (establishing the upward migration process of methane):

Check whether the pressure in the gas storage tank 4 is higher than the pressure in the reactor 8, preferably at least 1 MPa higher. If the pressure of the gas storage tank 4 is insufficient, pressurize the gas storage tank 4 through the gas pressurization system. Open the valve Z27 and the second pressure regulating valve 32 to adjust the outlet pressure of the gas storage tank 4 to be about 0.2 MPa higher than that in the reactor, and open the valves Z21, Z5, Z9, Z13 and Z18. Set and input the predetermined gas flow through the gas quality controller 5, the gas will be delivered to the reactor 8 at a certain rate (with a delay of about 10 seconds), after about 10 seconds, open the valve Z18, the gas will be Transported to the reactor 8, the gas can be seen in the sapphire window 25 moving upwards gradually. Add about 100ml of distilled water to the back pressure liquid container 19 at the liquid inlet end of the back pressure system, shake the hand pump 18 slowly, pay close attention to the reading of the pressure gauge P6 in the back pressure system, and adjust it to the experimental pressure. Open the valve Z19, the pressure of the reactor 8 is greater than the value of the pressure gauge P6 of the back pressure valve, then the gas or gas-liquid in the reactor 8 will flow out and flow to the gas-liquid separator 20. The gas flow meter 21 measures the amount of outflowing gas, and after the measurement is completed, it is safely discharged to the outside; the liquid will flow out into the water container, and the produced liquid metering system 22 (balance) can measure the quality of the outflowing liquid. A predetermined gas flow rate is set and input by the gas quality controller 5 , which is the gas flow rate at which methane flows upward from the bottom of the reactor 8 .

Open the control software and data collector to collect data such as temperature, pressure, flow and resistivity during the experiment, and save the data in the computer in real time.

Water samples and gas samples are collected every 2 hours, through the liquid sampling ports Z31-Z37, the liquid samples obtained by the production liquid metering system 22, the water samples and gas samples collected at the gas sampling port 29 and the gas flow meter 21, and the water samples are detected. The changes of anions and cations and the gas components in the gas sample.

After the reaction is over, the collection of water and gas samples is completed, and all valves are closed. Connect the movable exhaust pipe to the outlet of the gas flow meter 21, and move one end of the movable exhaust pipe out of the window; open the valve Z19, adjust the hand pump 18 of the back pressure system, and slowly reduce the pressure gauge P6 of the hand pump in stages , get rid of the high-pressure gas in the reactor 8 in stages. Open the valves Z11 and Z22, and the discharged gas will be discharged after gas-liquid separation. Quick pressure relief: connect the movable exhaust pipe to the air inlet Z19 of the reactor, and move one end of the movable exhaust pipe out of the window; open the valve Z19, adjust the hand pump of the back pressure system, and slowly set the pressure of the hand pump instrument in stages Reduce, and remove the high-pressure gas in the reactor in stages.

Save the data, close all valves, close the monitoring and control system, and turn off the power switch

Open the upper cover of the reaction kettle 8, and collect sediment/quartz sand solid samples and water samples in layers. Analyze the characteristics of the chemical composition of the water at the end of the experiment, and analyze the characteristics of microorganisms in it; analyze the sample components, mineral composition and microstructure through X-ray diffraction, XRF, ICP-MS, scanning electron microscopy and other means.

Clean the reaction kettle 8, the liquid container 9 with the piston and the microorganism container with the piston with distilled water, clean all connecting pipelines with distilled water, and blow dry to prevent rust.

Implementation example 2: (5°C, 10MPa, with a gas mass flow controller 10scc/min)

Prepare experimental materials, configure simulated seawater solution, prepare methane anaerobic oxidizing bacteria and sulfate radical reducing bacteria solutions, distilled water, South China Sea sediment samples, methane gas source, high-purity nitrogen, etc.;

Methane gas source 1, air compressor 2, gas booster pump 3, gas storage tank 4, gas mass flow controller 5, check valve 6, high and low temperature thermostat box 7, visible Hastelloy reactor 8, with Piston liquid container 9, with piston microbial container 10, constant speed and constant pressure pump 11, liquid container 12, safety valve 13, methane alarm 14, vacuum pump 15, buffer tank 16, back pressure container 17, hand pump 18, back pressure Liquid container 19, gas-liquid separator 20, gas flow meter 21, production fluid metering system (balance) 22, vent valve 23, back pressure valve 24, temperature sensor 26, conductivity sensor (5 pieces) 27, inlet pressure control Device 30, pressure regulating valve 31, and pressure regulating valve 2 are connected with pipelines and valves, all valves are closed, all sensors, probes, and instruments are connected to the data collector, and connected to the computer through the data collector.

Turn on the power switch, check whether the circuits, instruments, valves and sensors are working normally, and check whether the instruments, pipelines and valves are leaking;

Place the pistons of the liquid container 9 with the piston and the microorganism container 10 with the piston at the bottom, and fill the prepared simulated seawater solution and microbial solution;

Open the upper cover of the reaction kettle 8, add about 3/5 of the volume of the sediment/quartz sand sample, then cover the upper cover, and connect the various pipelines connected to the reaction kettle 8.

Open the switches of valves Z3, Z16, Z17, Z18, Z13, Z14, Z10, Z8, Z29, Z21, Z7 and vacuum pump 15 to carry out reaction kettle 8, buffer tank 16, gas storage tank 4, liquid container with piston 9, belt Piston microorganism container 10 and pipeline are evacuated, and the pressure of band pressure gauge P5 is-0.1MPa is to close vacuum pump 15, and closes all valves.

Add about 500ml of distilled water to the liquid container 12 as the pump liquid at the liquid inlet end of the constant pressure constant speed pump 11 . Turn on the constant pressure and constant speed pump 11, set the pumping pressure of 0.5Mpa, start the constant pressure and constant speed pump 11 to start working, and suck the pump liquid from the liquid container 12; when the pressure at the outlet end of the constant pressure and constant speed pump 11 reaches 0.5MPa, Constant pressure and constant speed pump 11 suspends work. Now, open the valves Z4, Z10, Z14 and Z18, the reaction solution in the liquid container 9 with the piston can be input into the reactor 8, when the liquid in the reactor 8 is filled with 4/5 volume of the reactor 8, close the constant Pressure constant speed pump 11, close valves Z4, Z10, Z14 and Z18.

Start the constant pressure and constant speed pump 11, open the valves Z4, Z29, Z10, Z14 and Z17, and transport the microbial solution in the microbial container 10 with the piston to the reactor from the top of the reactor 8. Liquid is filled in reaction kettle 8, has injected. Close valves Z4, Z29, Z10, Z14 and Z17 in sequence.

Start the high and low temperature incubator 7 to make the temperature in the reaction kettle 8 reach the set temperature of 5°C.

Utilize the hand pump 18, the back pressure liquid container 19 and the back pressure container 17 to set the pressure value of the pressure gauge P6 of the back pressure system at 10MPa.

The air compressor 2 is started, and the first pressure regulating valve 31 adjusts the output drive of the air compressor 2 to a predetermined pressure (20MPa) through the pressure gauge P2. Open the valve Z25 of the methane source 1, open the valve Z24 of the air compressor 2, and start boosting through the booster pump 3. Open the valve Z26, the pressurized gas will be delivered to the gas storage tank 4, and the pressure gauge P3 displays the pressure in the gas storage tank 4. Wait for the pressure in the gas storage tank 4 to rise to a predetermined pressure (20MPa). After the pressurization is completed, turn off the methane gas source valve Z25, turn off the air compressor output valve Z24, and turn off the air compressor 2.

Set the test pressure (10MPa) by the inlet pressure controller 30, open the valve Z27, adjust the pressure regulating valve 32, open the valves Z21, Z5, Z9, Z13, Z18, the gas mass flow controller 5 and the one-way valve 6, and the gas will Be transported in the reactor 8, the pressure in the reactor 8 reaches a predetermined value (10MPa), and the valves Z27, Z21, Z5, Z9, Z13, Z18 are closed.

Pressurize the pressure in the gas storage tank 4 to 20MPa again, open the valve Z27, adjust the pressure value of the pressure regulating valve 32 to 10.2MPa, open the valves Z21, Z5, gas mass flow controllers 5, Z9, one-way valve and Z18 , the gas will be delivered to the reactor 8. Set and input a predetermined gas flow rate of 10scc/min through the gas quality controller 5, the gas will be delivered to the reactor 8 at a certain rate (with a delay of about 10 seconds), after about 10 seconds, open the valve Z18, The gas will be transported into the reaction vessel 8, which can be seen in the sapphire window 25 gradually moving upwards. Add about 100ml of distilled water to the back pressure liquid container 19 at the liquid inlet end of the back pressure system, slowly shake the hand pump 18, and adjust the pressure in the back pressure system to 10MPa (reading of pressure gauge P6). Open the valve Z19, wait for the pressure of the reactor 8 to be slightly greater than the value (10MPa) of the pressure gauge P6 of the back pressure valve, the gas or gas-liquid in the reactor 8 will flow out, and flow to the gas-liquid separator 20. The gas flow meter 21 measures the amount of outflowing gas, and after the measurement is completed, it is safely discharged to the outside; the liquid will flow out into the water container, and the produced liquid metering system 22 (balance) can measure the quality of the outflowing liquid. A predetermined gas flow rate of 10 scc/min is set and input by the gas quality controller 5 , which is the gas flow rate of 10 scc/min for methane to flow upward from the bottom of the reactor 8 .

Open the control software and data collector to collect data such as temperature, pressure, flow and resistivity during the experiment, and save the data in the computer in real time.

Water samples and gas samples are collected every 2 hours, through the liquid sampling ports Z31-Z37, the liquid samples obtained by the production liquid metering system 22, the water samples and gas samples collected at the gas sampling port 29 and the gas flow meter 21, and the water samples are detected. The changes of anions and cations and the gas components in the gas sample.

After the reaction is over, the collection of water and gas samples is completed, and all valves are closed. Connect the movable exhaust pipe to the outlet of the gas flow meter 21, and move one end of the movable exhaust pipe out of the window; open the valve Z19, adjust the hand pump 18 of the back pressure system, and slowly reduce the pressure gauge P6 of the hand pump in stages , get rid of the high-pressure gas in the reactor 8 in stages. Open the valves Z11 and Z22, and the discharged gas will be discharged after gas-liquid separation. Quick pressure relief: connect the movable exhaust pipe to the air inlet Z19 of the reactor, and move one end of the movable exhaust pipe out of the window; open the valve Z19, adjust the hand pump of the back pressure system, and slowly set the pressure of the hand pump instrument in stages Reduce, and remove the high-pressure gas in the reactor in stages.

Save the data, close all valves, close the monitoring and control system, and turn off the power switch

Open the upper cover of the reaction kettle 8, and collect sediment/quartz sand solid samples and water samples in layers. Analyze the characteristics of the chemical composition of the water at the end of the experiment, and analyze the characteristics of microorganisms in it; analyze the sample components, mineral composition and microstructure through X-ray diffraction, XRF, ICP-MS, scanning electron microscopy and other means.

Clean the reaction kettle 8, the liquid container 9 with the piston and the microorganism container with the piston with distilled water, clean all connecting pipelines with distilled water, and blow dry to prevent rust.

Implementation Example 3: (0°C, 20MPa, with a gas mass flow controller 10scc/min)

Prepare experimental materials, configure simulated seawater solution, prepare methane anaerobic oxidizing bacteria and sulfate radical reducing bacteria solutions, distilled water, South China Sea sediment samples, methane gas source, high-purity nitrogen, etc.;

Methane gas source 1, air compressor 2, gas booster pump 3, gas storage tank 4, gas mass flow controller 5, check valve 6, high and low temperature thermostat box 7, visible Hastelloy reactor 8, with Piston liquid container 9, with piston microbial container 10, constant speed and constant pressure pump 11, liquid container 12, safety valve 13, methane alarm 14, vacuum pump 15, buffer tank 16, back pressure container 17, hand pump 18, back pressure Liquid container 19, gas-liquid separator 20, gas flow meter 21, production fluid metering system (balance) 22, vent valve 23, back pressure valve 24, temperature sensor 26, five conductivity sensors 27, inlet pressure controller 30 , the pressure regulating valve 31 and the pressure regulating valve 2 are connected with pipelines and valves, all valves are closed, all sensors, probes and instruments are connected to the data collector, and connected to the computer through the data collector.

Turn on the power switch, check whether the circuits, instruments, valves and sensors are working normally, and check whether the instruments, pipelines and valves are leaking;

Place the pistons of the liquid container 9 with the piston and the microorganism container 10 with the piston at the bottom, and fill the prepared simulated seawater solution and microbial solution;

Open the upper cover of the reaction kettle 8, add about 3/5 of the volume of the sediment/quartz sand sample, then cover the upper cover, and connect the various pipelines connected to the reaction kettle 8.

Open the switches of valves Z3, Z16, Z17, Z18, Z13, Z14, Z10, Z8, Z29, Z21, Z7 and vacuum pump 15 to carry out reaction kettle 8, buffer tank 16, gas storage tank 4, liquid container with piston 9, belt Piston microorganism container 10 and pipeline are evacuated, and the pressure of band pressure gauge P5 is-0.1MPa is to close vacuum pump 15, and closes all valves.

Add about 500ml of distilled water to the liquid container 12 as the pump liquid at the liquid inlet end of the constant pressure constant speed pump 11 . Turn on the constant pressure and constant speed pump 11, set the pumping pressure of 0.5Mpa, start the constant pressure and constant speed pump 11 to start working, and suck the pump liquid from the liquid container 12; when the pressure at the outlet end of the constant pressure and constant speed pump 11 reaches 0.5MPa, Constant pressure and constant speed pump 11 suspends work. Now, open the valves Z4, Z10, Z14 and Z18, the reaction solution in the liquid container 9 with the piston can be input into the reactor 8, when the liquid in the reactor 8 is filled with 4/5 volume of the reactor 8, close the constant Pressure constant speed pump 11, close valves Z4, Z10, Z14 and Z18.

Start the constant pressure and constant speed pump 11, open the valves Z4, Z29, Z10, Z14 and Z17, and transport the microbial solution in the microbial container 10 with the piston to the reactor from the top of the reactor 8. Reactor 8 is filled with liquid, and the injection is complete. Close valves Z4, Z29, Z10, Z14 and Z17 in sequence.

Start the high and low temperature incubator 7 to make the temperature in the reactor 8 reach the set temperature of 0°C.

Utilize the hand pump 18, the back pressure liquid container 19 and the back pressure container 17, the pressure value of the pressure gauge P6 of the back pressure system is set at 20MPa.

Start the air compressor 2, the first pressure regulating valve 31, and adjust the drive output of the air compressor 2 to a predetermined pressure (25MPa) through the pressure gauge P2. Open the valve Z25 of the methane source 1, open the valve Z24 of the air compressor 2, and start boosting through the booster pump 3. Open the valve Z26, the pressurized gas will be delivered to the gas storage tank 4, and the pressure gauge P3 displays the pressure in the gas storage tank 4. Wait for the pressure in the gas storage tank 4 to rise to a predetermined pressure (25MPa). After the pressurization is completed, turn off the methane gas source valve Z25, turn off the air compressor output valve Z24, and turn off the air compressor 2.

Set the test pressure (20MPa) by the inlet pressure controller 30, open the valve Z27, adjust the pressure regulating valve 32, open the valves Z21, Z5, Z9, Z13, Z18, the gas mass flow controller 5 and the one-way valve 6, and the gas will Be transported in the reactor 8, the pressure in the reactor 8 reaches a predetermined value (20MPa), and the valves Z27, Z21, Z5, Z9, Z13, Z18 are closed.

Pressurize the pressure in the gas storage tank 4 to 20MPa again, open the valve Z27, adjust the pressure value of the pressure regulating valve 32 to 10.2MPa, open the valves Z21, Z5, gas mass flow controllers 5, Z9, one-way valve and Z18 , the gas will be delivered to the reactor 8. Set and input a predetermined gas flow rate of 10scc/min through the gas quality controller 5, the gas will be delivered to the reactor 8 at a certain rate (with a delay of about 10 seconds), after about 10 seconds, open the valve Z18, The gas will be transported into the reaction vessel 8, which can be seen in the sapphire window 25 gradually moving upwards. Add about 100ml of distilled water to the back pressure liquid container 19 at the liquid inlet end of the back pressure system, shake the hand pump 18 slowly, and adjust the reading of the pressure gauge P6 in the back pressure system to 20MPa. Open valve Z19, wait for reactor 8 pressure to be slightly greater than back pressure valve pressure gauge P6 value (20MPa), the gas or gas-liquid in reactor 8 will flow out, flow to gas-liquid separator 20 places. The gas flow meter 21 measures the amount of outflowing gas, and after the measurement is completed, it is safely discharged to the outside; the liquid will flow out into the water container, and the produced liquid metering system 22 (balance) can measure the quality of the outflowing liquid. A predetermined gas flow rate of 10 scc/min is set and input by the gas quality controller 5 , which is the gas flow rate of 10 scc/min for methane to flow upward from the bottom of the reactor 8 .

Open the control software and data collector to collect data such as temperature, pressure, flow and resistivity during the experiment, and save the data in the computer in real time.

Water samples and gas samples are collected every 2 hours, through the liquid sampling ports Z31-Z37, the liquid samples obtained by the production liquid metering system 22, the water samples and gas samples collected at the gas sampling port 29 and the gas flow meter 21, and the water samples are detected. The changes of anions and cations and the gas components in the gas sample.

After the reaction is over, the collection of water and gas samples is completed, and all valves are closed. Connect the movable exhaust pipe to the outlet of the gas flow meter 21, and move one end of the movable exhaust pipe out of the window; open the valve Z19, adjust the hand pump 18 of the back pressure system, and slowly reduce the pressure gauge P6 of the hand pump in stages , get rid of the high-pressure gas in the reactor 8 in stages. Open the valves Z11 and Z22, and the discharged gas will be discharged after gas-liquid separation. Quick pressure relief: connect the movable exhaust pipe to the air inlet Z19 of the reactor, and move one end of the movable exhaust pipe out of the window; open the valve Z19, adjust the hand pump of the back pressure system, and slowly set the pressure of the hand pump instrument in stages Reduce, and remove the high-pressure gas in the reactor in stages.

Save the data, close all valves, close the monitoring and control system, and turn off the power switch

Open the upper cover of the reaction kettle 8, and collect sediment/quartz sand solid samples and water samples in layers. Analyze the characteristics of the chemical composition of the water at the end of the experiment, and analyze the characteristics of microorganisms in it; analyze the sample components, mineral composition and microstructure through X-ray diffraction, XRF, ICP-MS, scanning electron microscopy and other means.

Clean the reaction kettle 8, the liquid container 9 with the piston and the microorganism container with the piston with distilled water, clean all connecting pipelines with distilled water, and blow dry to prevent rust.

The above detailed description is a specific description of the feasible embodiment of the present invention. This embodiment is not used to limit the patent scope of the present invention. Any equivalent implementation or change that does not deviate from the present invention should be included in the patent scope of this case. middle.

Claims (10)

1. a kind of simulated sea bottom methane leakage causes the reaction unit of early diagenesis, it is characterised in that：Including reaction system；

It is connected with the reaction system, the gas pressurizing sub-system of pressure adjusting is provided for the reaction system；

It is connected with the reaction system, the reaction solution feed flow subsystem of reaction solution supply is provided for the reaction system；

Gas and liquid collecting system is further included, the gas and liquid collecting system is connected to the port of export of the reaction system, and the gas-liquid is received Back pressure system is set between collecting system and the reaction system, and the back pressure system is gas and liquid collecting system and the reaction system Between pressure difference is provided, the gas and liquid collecting after control reaction.

2. simulated sea bottom methane leakage according to claim 1 causes the reaction unit of early diagenesis, its feature exists In：The gas pressurizing sub-system includes methane source of the gas, air compressor, booster pump and gas reservoir, and the methane source of the gas, increase Press pump and gas reservoir are sequentially communicated by the pipeline with control valve, and the air compressor passes through with pressure regulator valve and control The pipeline of valve connects the booster pump, and the gas reservoir passes through with pressure regulator valve, blow valve, check valve with the reaction system And the pipeline connection of some control valves, gas mass flow control is additionally provided between the gas reservoir and the reaction system Device.

3. simulated sea bottom methane leakage according to claim 1 causes the reaction unit of early diagenesis, its feature exists In：The reaction solution feed flow subsystem includes band piston liquid container and with piston microorganism container, the band piston liquid Container with it is described with piston microorganism container, to be one end be connected to constant speed and constant pressure by the pipeline with control valve pumps, the other end leads to Cross the pipeline with control valve and be connected to the reaction system, the liquid container of the constant speed and constant pressure pump connection equipped with distilled water, is used Pump liquid is provided in being pumped to the constant speed and constant pressure.

4. simulated sea bottom methane leakage according to claim 1 causes the reaction unit of early diagenesis, its feature exists In：The reaction system includes the reaction kettle being placed in high/low temperature insulating box, four before and after being provided with up and down on the reaction kettle A visual windows, the reaction kettle top are equipped with gas sample mouth, and the reaction kettle side is provided with some liquid sampling mouths, institute State some liquid sampling mouths to be distributed on different height, the reaction kettle side is additionally provided with thermometer and some conductivity sensors Device, the gas pressurizing sub-system connect reaction by the pipeline with control valve respectively with the reaction solution feed flow subsystem The upper and lower ends of kettle.

5. simulated sea bottom methane leakage according to claim 4 causes the reaction unit of early diagenesis, its feature exists In：Safety valve and gas reservoir are additionally provided with the top of the reaction kettle, described gas reservoir one end passes through the pipeline with control valve The top of the reaction kettle is communicated in, reaction kettle can be vacuumized, the other end connects gas boosting by the pipeline with valve System.

6. the simulated sea bottom methane leakage according to claim 4-5 causes the reaction unit of early diagenesis, its feature It is：The reaction kettle is visualization Hastelloy reaction kettle.

7. simulated sea bottom methane leakage according to claim 1 causes the reaction unit of early diagenesis, its feature exists In：The gas and liquid collecting system includes gas-liquid separator, passes through the pipeline connection gas with control valve at the top of the gas-liquid separator Flowmeter body, the gas-liquid separator bottom connect Produced Liquid metering system by the pipeline with control valve.

8. simulated sea bottom methane leakage according to claim 1 causes the reaction unit of early diagenesis, its feature exists In：The back pressure system includes passing through the sequentially connected back-pressure valve of pipeline, back pressure container, hand pump and back pressure liquid container, institute State and pressure gauge is set on pressurizing vessel.

9. a kind of simulated sea bottom methane leakage causes the reaction method of early diagenesis, it is characterised in that：Comprise the following steps：

Step 1：Check whether reaction unit is normal, and each pipeline and each valve whether there is gas leakage；

Step 2：Solid deposited thing/quartz sand sample is added in a kettle；

Step 3：The reaction solution feed flow subsystem is opened, the pressure adjustment effect pumped by the constant speed and constant pressure will be with work Fill in the reaction solution injection reaction kettle in liquid container；

Step 4：The pressure adjustment effect pumped by the constant speed and constant pressure, will inject with the microorganism in piston microorganism container In reaction kettle；

Step 5：Start high/low temperature insulating box, the temperature in reaction kettle is reached the temperature value of setting；

Step 6：Setting experiment pressure values and back pressure system pressure values；

Step 7：The gas pressurizing sub-system is opened, the methane gas for making to input in gas reservoir reaches the pressure values of setting；

Step 8：Reactive material reacts in a kettle, controls the pressure in reaction kettle in real time in setting range；

Step 9：When 0.5-12 is small, water sample and gas sample are gathered by adjusting pressure difference, until reaction terminates.

10. simulated sea bottom methane leakage according to claim 9 causes the reaction method of early diagenesis, its feature exists In：Liquid Flow speed in reaction process is controlled by the pressure difference of gas pressurizing sub-system, reaction kettle and back pressure system.