CN107930537A - A kind of simulated sea bottom methane leakage causes the reaction unit and method of early diagenesis - Google Patents
A kind of simulated sea bottom methane leakage causes the reaction unit and method of early diagenesis Download PDFInfo
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 235
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 154
- 238000000034 method Methods 0.000 title claims description 13
- 239000007788 liquid Substances 0.000 claims abstract description 161
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 53
- 244000005700 microbiome Species 0.000 claims description 45
- 239000000243 solution Substances 0.000 claims description 45
- 239000012153 distilled water Substances 0.000 claims description 23
- 230000000694 effects Effects 0.000 claims description 12
- 238000002474 experimental method Methods 0.000 claims description 12
- 238000002347 injection Methods 0.000 claims description 10
- 239000007924 injection Substances 0.000 claims description 10
- 239000006004 Quartz sand Substances 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 238000005070 sampling Methods 0.000 claims description 9
- 229910000856 hastalloy Inorganic materials 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 230000000007 visual effect Effects 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
- 238000012800 visualization Methods 0.000 claims description 3
- 238000004088 simulation Methods 0.000 abstract description 6
- 238000004458 analytical method Methods 0.000 abstract description 5
- 239000007789 gas Substances 0.000 description 213
- 239000000523 sample Substances 0.000 description 62
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 18
- 229910052757 nitrogen Inorganic materials 0.000 description 9
- 150000004677 hydrates Chemical class 0.000 description 7
- 230000000813 microbial effect Effects 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 239000013535 sea water Substances 0.000 description 7
- 241000894006 Bacteria Species 0.000 description 6
- 239000011148 porous material Substances 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 238000003860 storage Methods 0.000 description 6
- 229910052594 sapphire Inorganic materials 0.000 description 5
- 239000010980 sapphire Substances 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
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- 239000013049 sediment Substances 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
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- 230000001419 dependent effect Effects 0.000 description 3
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- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
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- 238000012544 monitoring process Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000004659 sterilization and disinfection Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000004846 x-ray emission Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
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- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 238000004378 air conditioning Methods 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
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- 230000005593 dissociations Effects 0.000 description 1
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- 238000011835 investigation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000009533 lab test Methods 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- NMJORVOYSJLJGU-UHFFFAOYSA-N methane clathrate Chemical compound C.C.C.C.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O NMJORVOYSJLJGU-UHFFFAOYSA-N 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
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- 230000001954 sterilising effect Effects 0.000 description 1
- 238000012916 structural analysis Methods 0.000 description 1
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Abstract
The invention discloses the reaction unit that a kind of simulated sea bottom methane leakage causes early diagenesis, including reaction system；The gas pressurizing sub-system and reaction solution feed flow subsystem being connected with reaction system；Further include gas and liquid collecting system, gas and liquid collecting system is connected to the port of export of reaction system, back pressure system is set between gas and liquid collecting system and reaction system, and back pressure system provides pressure difference, the gas and liquid collecting after control reaction between gas and liquid collecting system and reaction system.By early diagenesis caused by unit simulation methane leakage, marine environment and biogeochemical reaction process can be more preferably understood, have important guidance and indicative significance to the specific geochemical analysis in ocean work.
Description
Technical field
The present invention relates to marine oil and gas geochemical exploration technical field, more particularly to simulated sea bottom hydrate preservation area first
The research field of alkane leakage.
Background technology
Gas hydrates are most potential after shale gas, coal bed gas to take over the energy.Gas hydrates conduct
A kind of high-efficiency cleaning energy that is brand-new, having a high potential, it is considered to be the alternative energy source of 21 century.China was in 2007 and 2009
Year successively obtains gas hydrates sample in South China Sea and Qinghai-Tibet Qilian mountains permafrost region, it is predicted that gas water
Compound reserves are petroleum reserves more than two times.Carry out in China at the South Sea within 2017 gas hydrates pilot production and making a breakthrough property into
Work(.
In gas hydrates Favorable Areas, since the decomposition release of hydrate causes the methane of seabed generally existing to leak
(cold spring activity), the methane of leakage can penetrate overlying rock/sedimentary slowly, constantly to seabed surface seep, and
With the isotope of redox-sensitive element such as the sulfate ion in Sediment Pore Water, nitrate ion and iron, manganese in microorganism
Effect is lower to occur redox reaction, wherein a most important reaction is exactly sulfate radical reduction-anaerobic methane oxidation
(AOM), the bicarbonate radical of generation is combined generation northern South China Sea with the calcium and magnesium ion in pore water.Leaked and sent out by methane
Raw serial geochemical process causes deposit, pore water geochemical anomaly, these are exactly that we identify the oil that underlies extremely
The theoretical foundation of gas reservoir/gas hydrates geochemical exploration.Submarine methane leakage represents Deep Oil-gas/hydrate from source
Area or reservoir are migrated to seabed surface, belong to cold spring activity.Therefore, submarine methane leakage process is complicated, and and sea-bottom surface
Serial complex reaction occurs for S ＆ W.Although submarine methane leakage (cold spring activity) generally existing, still lack pair
The serial reaction and its product that the zwitterion of submarine methane seepage Mechanism and methane and pore water occurs under microbial action
With the understanding of early diagenesis, so as to directly influence Geochemical Method Distinguishing and the exploration of marine oil and gas/gas hydrates
Effect.The simulated sea bottom methane leakage early diagenesis reaction system for intending carrying out is the effective technology means for solving this problem
One of.
At present related methane caused by gas hydrate dissociation leak and its and pore water in zwitterion in microorganism
The research of the lower serial geochemical reaction and its product occurred of effect and early diagenesis is at the early-stage, in view of methane leaks
The complexity of (cold spring activity), is carrying out South Sea cold spring behaviour area in the base of pore water and northern South China Sea geochemical investigation
On plinth, it is necessary to be aided with relevant simulating lab test research.It is domestic with submarine methane leakage and its early diagenesis
Experimental system for simulating is few, and existing experimental provision mainly based on simulating hydrate generation decomposition, can not embody submarine sedimentary strata
In methane leakage caused by serial geochemical reaction and early diagenesis, it is difficult to hydrate preservation area methane is leaked and is lived
Early diagenesis carries out qualitative and Quantitative study caused by dynamic.
Patent of invention content
The present invention is in view of the above-mentioned problems, propose a kind of cold spring environment be capable of simulated sea bottom methane and leaked, and be used for first
The experimental provision and method that alkane leakage studies early diagenesis.
To realize above-mentioned target, the present invention provides following technical solution：
A kind of simulated sea bottom methane leakage causes the reaction unit of early diagenesis, 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
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, the gas
Back pressure system is set between liquid collection system and the reaction system, and the back pressure system is gas and liquid collecting system and the reaction
Pressure difference, the gas and liquid collecting after control reaction are provided between system.
The gas pressurizing sub-system includes methane source of the gas, air compressor, booster pump and gas reservoir, the methane gas
Source, booster pump and gas reservoir are sequentially communicated by the pipeline with control valve, and the air compressor passes through with pressure regulator valve
And the pipeline of control valve connects the booster pump, the gas reservoir passes through with pressure regulator valve, check valve with the reaction system
And the pipeline connection of some control valves, gas mass flow control is provided between the gas reservoir and the reaction system
Device.
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, it is another
End is connected to the reaction system by the pipeline with control valve, and the liquid of the constant speed and constant pressure pump connection equipped with distilled water holds
Device, pump liquid is provided for being pumped to the constant speed and constant pressure.
The reaction system includes the reaction kettle being placed in high/low temperature insulating box, before being provided with up and down on the reaction kettle
Symmetrical visual windows afterwards, the reaction kettle top are equipped with gas sample mouth, and the reaction kettle side is provided with some liquid
Body sample tap, some liquid sampling mouths are distributed on different height, if the reaction kettle side be additionally provided with thermometer and
Dry conductivity sensor, the gas pressurizing sub-system is with the reaction solution feed flow subsystem respectively by with control valve
Pipeline connects the upper and lower ends of reaction kettle.
Safety valve and gas reservoir are additionally provided with the top of the reaction kettle, described gas reservoir one end passes through with control valve
Pipeline is communicated in the top of the reaction kettle, and the other end connects gas pressurizing sub-system by the pipeline with valve.
The reaction kettle is visualization Hastelloy reaction kettle.
The collection 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.
The back pressure system includes holding by the sequentially connected back-pressure valve of pipeline, back pressure container, hand pump and back pressure liquid
Device, sets pressure gauge on the pressurizing vessel.
At the same time, there is provided a kind of corresponding simulated sea bottom methane leakage causes the reaction method of early diagenesis, including
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 pumped by the constant speed and constant pressure is adjusted
Effect, will inject reaction kettle with the reaction solution in piston liquid container；
Step 4：The pressure adjustment effect pumped by the constant speed and constant pressure, by with piston microorganism container
In microorganism injection 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, which reaches, to be set
Fixed pressure values；
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.
Liquid Flow speed in reaction process can be controlled by the pressure difference of gas pressurizing sub-system, reaction kettle and back pressure system
Rate, the consumption and liquid discharge rate of methane are measured by metering system.
Beneficial effects of the present invention are：
The reaction unit that early diagenesis mechanism is leaked by the simulated sea bottom methane is simulated caused by methane leakage
Early diagenesis, can more preferably understand marine environment, understand global carbon, understand early diagenesis and the biological earth
Serial geochemical reaction occurs under microbial action with the zwitterion in water body for chemical reaction process, indoor simulation methane
Process and its product have important guidance and indicative significance to the specific geochemical analysis in ocean work.
Brief description of the drawings
Fig. 1 is the reaction unit schematic diagram that simulated sea bottom methane of the present invention leaks early diagenesis.
Each reference numeral is in figure：
1st, 1- methane source of the gas, 2- air compressors, 3- gas boostings pump, 4- gas reservoirs, the control of 5- gas mass flows
Device, 6- check valves, 7- high/low temperature insulating boxs, 8- reaction kettles, 9- band piston liquid containers, 10- band piston microorganism containers, 11-
Constant speed and constant pressure pumps, 12- liquid containers, 13- safety valves, 14- methane alarms, 15- vacuum pumps, 16- surge tanks, and 17- back pressure is held
Device, 18- hand pumps, 19- back pressure liquid containers, 20- gas-liquid separators, 21- gas flowmeters, 22- Produced Liquid metering systems,
23- blow valves, 24- back-pressure valves, 25- sapphire forms, 26- temperature sensors, 27- conductivity sensors, 28- sample taps, 29-
Air hatch, 30- inlet pressure controllers, the first pressure regulator valves of 31-, the second pressure regulator valves of 32-；
2nd, pressure gauge P1-P6；
3rd, control valve Z1-Z38.
Embodiment
Present disclosure is described in further details with reference to the accompanying drawings and detailed description.
Embodiment one：(5 DEG C, 10MPa)
As shown in Figure 1, a kind of simulated sea bottom methane leakage causes the reaction unit of early diagenesis, including gas boosting
Subsystem, reaction solution feed flow subsystem, reaction system, back pressure system and gas and liquid collecting system.
Gas pressurizing sub-system includes：1,4 pressure gauge (P1, P2, P3 and P4) of methane source of the gas, 4 control valve (gas cylinders
High-pressure inlet valve Z25, driving gas inlet valve Z26, gases at high pressure outlet valve Z27 and pressure reducing valve outlet valve Z24), 2 pressure regulator valves
(31 and 32).(storage pressure:Pressure gage measuring range 16MPa, 1.6 grades of precision (the 1.6% of full scale)；The pressure of control driving gas
Power (i.e. compressed air):Pressure gage measuring range is 1.6MPa, 1.6 grades of precision；Outlet pressure, that is, booster pump outlet (i.e. gas reservoir pressure
Power):Pressure gage measuring range 60MPa, 1.6 grades of precision；Pressure regulation pressure, that is, pressure regulation valve outlet pressure:Pressure gage measuring range 60MPa, precision
1.6 level；The conversion relation for wherein driving gas of the gas with finally getting pressure is：60 × driving air pressures=finally type it out
Pressure.)
Pressurization concrete operations：2 power supply of air compressor is connected, starts air compressor 2, the first pressure regulator valve 31, leads to
The pressure that excess pressure table P2 exports air compressor 2 will be adjusted to predetermined driving pressure (0.1MPa).Reach predetermined driving pressure
After power, air compressor 2 is automatically closed；The valve Z25 of methane source of the gas 1 is opened, the value that pressure gauge P1 is shown is the pressure of methane origin 1
Force value.The valve Z24 at 2 end of air compressor is opened, booster pump 3 starts to work under driving pressure, methane source of the gas is started to be pressurized.
Valve Z26 is opened, the gas after supercharging will be transported in gas reservoir 4, and pressure gauge P3 shows the pressure in gas reservoir 4.Through
Certain time, pressure rise in gas reservoir 4 to predetermined pressure (1-30MPa).After supercharging, turn off methane gas source valve
Z25, turns off air compressor output terminal valve Z24, turns off air compressor 2, closes valve Z26.
Reaction solution feed flow subsystem：It is spare to prepare reaction solution (simulated seawater solution) in advance.Will be with piston liquid
The piston reset of container 9 is to container bottom, i.e., using the gases at high pressure in gas reservoir 4 by the piston with piston liquid container 9
Reset, concrete operations are：Valve Z27, Z21, Z7, Z13, Z14, Z10 and blow valve Z6 are opened, slowly adjusts the second pressure regulator valve 32,
Its outlet pressure is controlled in several atmospheric pressure, you can under gas pressure, you can shift intermediate piston onto band piston liquid container 9
Bottom, is then shut off all valves, and the second pressure regulator valve 32 is resetted.Band piston liquid container 9 is opened, it is molten to pour into enough reactions
Liquid, covers band piston liquid container 9.The distilled water of about 500ml is added as 11 liquid feeding end of constant pressure constant speed pump toward liquid container 12
Pump liquid.Constant pressure constant speed pump 11 is opened, sets the pressure that pumps out of 0.5MPa, starts constant pressure constant speed pump 11, starts from liquid container
12 suction pump liquids；When 11 outlet pressures of constant pressure constant speed pump reach 0.5MPa, 11 break-off of constant pressure constant speed pump.At this time, beat
Control valve Z4, Z10, Z14 and Z18 are opened, will can be input to the reaction solution in piston liquid container 9 in reaction kettle 8.
Reaction system：Including 7 (operating temperature of high/low temperature insulating box：Scope -20~100 DEG C, temperature-controlled precision：±0.1℃)、
4 import sapphire highpressures are provided with the visualization Hastelloy reaction kettle 8 that is arranged in high/low temperature insulating box 7, reaction kettle 8
25,7 sample tap Z31-Z37 of visual form, gas sample mouth 29, temp probe 26,5 conductivity probes 27, upper injection ports
Z17, lower injection port Z18, upper outlet Z19, lower outlet Z20, leakage fluid dram Z30.
Reaction kettle temperature control：High/low temperature insulating box 7 is opened, design temperature is -20~20 DEG C of degree, the reaction in reaction kettle 8
Solution temperature reaches stablize after when small (about 10 or so), can pressurize to reaction kettle 8.Reaction kettle pressurized operation is：Open valve
Z27, adjusts pressure regulator valve 32, adjusts the outlet pressure (such as 1MPa) of gas reservoir 4.Valve Z21, Z7, Z13 and Z17 are opened successively, will
Gases at high pressure in gas reservoir 4 are transported in reaction kettle 8, and the pressure in reaction kettle quickly reaches setting value.In reaction kettle 8
Since gases at high pressure input, temperature temporarily raises temperature.After high/low temperature insulating box 7 cools down for a period of time, temperature in reaction kettle 8
The design temperature being reduced to before pressurization.The second pressure regulator valve 32 is slowly adjusted, raises outlet pressure so that the pressure in reaction kettle 8
Progressively increase to predetermined experimental pressure.Repeated multiple times charge air conditioning so that its pressure and temperature reaches predetermined pressure and temperature strip
Part.
Gas and liquid collecting system includes gas-liquid separator, passes through the pipeline connection gas stream with control valve at the top of gas-liquid separator
Gauge, gas-liquid separator bottom connect Produced Liquid metering system by the pipeline with control valve.
Back pressure system includes passing through the sequentially connected back-pressure valve of pipeline, back pressure container, hand pump and back pressure liquid container, adds
Pressure gauge is set on pressure vessel.
Microorganism is injected：The control valve Z28 with 10 top/bottom part of piston microorganism container is opened, manually will be with piston microorganism
Piston in container 10 resets into piston base and (alternatively, when reaction kettle 8 is in high pressure conditions, opens band piston microorganism and hold
The control valve Z28 of 10 bottom of device, it is then slight slowly to open microorganism valve Z29, piston is pushed into its bottom using gases at high pressure
Portion).After piston shifts 10 bottom of band piston microorganism container onto, the pipeline of 10 bottom of connect band piston microorganism container, then
Close microorganism valve Z29 and control valve Z28.The nitrogen cylinder for being equipped with pressure reducing valve is got ready, even interim pipeline, is connected to microorganism container
Top.Pressure regulator valve is slowly adjusted, controls the outlet pressure of nitrogen so that gas can be exported leniently.Use 75% alcoholic solution
Manipulator is wiped, and the sterilization treatment that carries out disinfection to band piston microorganism container 10, microorganism was added with reducing
Operator is on hand in journey and microbes in air is mixed into interference to the microorganism of injection.Nitrogen outlet position is adjusted, can
Alcohol disinfection solution is quickly dried up, after drying, keeps nitrogen persistently to blow out.The microbial solution 50ml that will be got ready, it is living to pour into band
Microorganism container 10 is filled in, during pouring into solution, cover and connecting pipe valve, should ensure that nitrogen, constantly stripping band piston is micro-
Biopack 10.Then, start constant pressure constant speed pump 11, open control valve Z4, Z29, Z10 and Z14, set first to constant pressure constant speed pump
11 pressure is slightly above 8 predetermined experimental pressure of reaction kettle.When constant pressure 11 break-off of constant speed pump, illustrate pressure in pipeline
Reach setting pressure.Control valve Z17 is opened, then the pressure of constant pressure constant speed pump 11 is by slight decrease, band piston microorganism container 10
In microbial solution will be transported to by the top of reaction kettle 8 in reaction kettle.When the pressure of constant pressure constant speed pump 11 is constant, illustrate to live
Plug has reached 10 top of band piston microorganism container, and injection finishes.Closing control valve Z4, Z29, Z10, Z14 and Z17 successively.
The data acquisition of temperature, pressure etc. in experimentation：
Computer is opened, starts the data acquisition software of desktop, the communication of software and data collecting card is opened, with regard to that can see
The display result in data acquisition software such as the temperature 26 of collection, pressure, resistivity 27.Data are set to preserve：Deposited in data
In disk tabs, the position of data preservation is set, the title and data of data file preserve interval (s).Click starts to preserve
Afterwards, one excel data file of automatic spring is to carry out data preservation.After experiment, click on and stop preserving, software will be automatic
Data are preserved, and excel files are automatically closed.Data are preserved and finished.
The collection and test of gas and fluid sample in experimentation：
Gas sample：Gas sample work in experiment, can complete in the air hatch 29 on 8 top of reaction kettle, be specially：
Gas sampling bag is connected, gently opens 29 valve Z38 of air hatch, when getting required volumes of gas, closes the control of air hatch 29
Valve Z38 processed.It is to be measured to remove gas sampling bag.
Liquid-like：Water sample sampling work is sampled in 8 side sample tap 28 of reaction kettle in experimentation.Concrete operations are：Take
Clean fine taper bottle is some, and left hand holds fine taper bottle, and 7 outlet valve Z31-Z37 that the right hand slowly opens sample tap 28 take successively
Sample, during predetermined to be achieved, closes valve Z31-Z37 successively.Sample, can monitor in real time in 8 side wall diverse location of reaction kettle
Solution chemistry composition transfer on 8 different depth of reaction kettle, reaction simulation submarine methane leak the geochemical process in environment.
The collection of the efflux in Produced Liquid metering system 22 under the conditions of flowing experiment and chemical constituent test, gas stream
The test for the gas component collection that gauge 21 comes out.
After experiment, deposit (quartz sand) solid sample of different depth in reaction kettle 8 is taken to carry out component and microcosmic
Structural analysis, research methane leak the early diagenesis process in environment.
Reaction reaction was completed 8 pressure relief of gas of kettle：Movable exhaust pipe is connected to 21 port of export of gas flowmeter, activity exhaust
Pipe one end moves to outside window；Valve Z19 is opened, adjusts the hand pump 18 of back pressure system, by the pressure gauge P6 of hand pump slowly stage by stage
Reduce, exclude the gases at high pressure in reaction kettle 8 stage by stage.Valve Z11 and Z22 are opened, the gas of discharge is discharged after gas-liquid separation.
Fast pressure relief：Movable exhaust pipe is connected to the blow valve Z12 of reaction kettle, movable exhaust pipe one end moves to outside window；Open valve
Z19, adjusts the hand pump of back pressure system, and the pressure of hand pump instrument is slowly reduced stage by stage, excludes stage by stage in reaction kettle
Gases at high pressure.
Reaction solution discharge (being gone out hydraulic pressure using the gases at high pressure for increasing system) in reaction kettle 8：Movable drain pipe is connected
It is connected to the blow valve Z30 of 8 bottom of reaction kettle, other end emptying beaker dress waste liquid.Valve Z27 is opened, adjusts the second pressure regulator valve 32, is adjusted
The outlet pressure of throttle body storage tank is 0.3MPa, opens valve Z21, Z7, Z13 and Z17, and since gas pressure acts on, hydraulic pressure is gone out.
Reaction kettle, microorganism injection container and pipeline flush：
Band piston liquid container 9 cleans：Valve Z4 and Z8 are opened, sets constant speed and constant pressure pump pressure as 0.3MPa, starts constant pressure
Constant speed pump 11, will discharge with the remaining liq in piston liquid container 9；After with the liquid discharge in piston liquid container 9,
Close valve Z8；Valve Z27 is opened, adjusts the second pressure regulator valve 32, valve Z21, Z7, Z13, Z14, Z10 and Z6 is opened, uses gas reservoir
Pressure in 4 will shift bottom onto with the piston in piston liquid container 9, after piston reaches bottom, close successively valve Z27, Z21,
Z7, Z13, Z14, Z10 and Z6；Band piston liquid container 9 is opened, distilled water is poured into wherein, cleans inner wall repeatedly, uses siphonage
Suction out cleaning solution；After cleaning three times, a small amount of distilled water (about 500ml) is poured into, covers reaction liquid container.Start constant pressure constant speed
Pump 11, opens valve Z4, Z10, Z14 and Z17, and driving distilled water flows through pipeline, the pipeline of valve Z17 one end is cleaned.Valve Z17
After the pipeline flush of one end, valve Z17 is closed, valve Z18 is opened and cleans pipeline therein.After the pipeline flush of valve Z18 one end,
Close valve 18.Reaction kettle 8 is opened, cleans 8 inner wall of reaction kettle repeatedly using distilled water.Washing lotion is suctioned out with siphonage.Unicom is reacted
Other pipelines of kettle 8, using nitrogen to the pipeline and stripping in reaction kettle, ensure container, pipeline, reaction kettle drying.
Simulated sea bottom methane leakage causes the concrete operations of early diagenesis reaction unit as follows：
Preparing experiment material, configures simulated seawater solution, prepares dependent anaerobic methane oxidation bacteria and sulfate radical reducing bacteria solution, steams
Distilled water, South China Sea sediments sample, methane source of the gas, high pure nitrogen etc..
Methane source of the gas 1, air compressor 2, gas boosting pump 3, gas reservoir 4, gas mass flow controller 5 is single
It is permanent to valve 6, high/low temperature insulating box 7, visual Hastelloy reaction kettle 8, band piston liquid container 9, band piston microorganism container 10
Fast constant pressure pump 11, liquid container 12, safety valve 13, methane alarm 14, vacuum pump 15, surge tank 16, back pressure container 17 are hand
Pump 18, back pressure liquid container 19, gas-liquid separator 20, gas flowmeter 21, Produced Liquid metering system 22, i.e. balance, blow valve
23, back-pressure valve 24,26,5 conductivity sensors 27 of temperature sensor, inlet pressure controller 30, the first pressure regulator valve 31, pressure regulation
Valve 2 is connected with pipeline and valve, closes all valves, all the sensors, probe, instrument are connected on data collector, pass through data
Collector is connected to computer.
Reaction unit total power switch is opened, checks whether circuit, instrument and meter, valve and sensor work normally, is checked
Instrument, pipeline and valve whether gas leakage；
Piston with piston liquid container 9 and with piston microorganism container 10 is placed in bottom, and loads the simulation of preparation
Sea water solution and microbial solution；
The upper cover of reaction kettle 8 is opened, deposit/quartz sand sample of about 3/5 volume is added, then covers upper cover, is connected
The each pipeline being connected with reaction kettle 8.
The switch of valve Z3, Z16, Z17, Z18, Z13, Z14, Z10, Z8, Z29, Z21, Z7 and vacuum pump 15 is opened, is carried out
Reaction kettle 8, surge tank 16, gas reservoir 4, band piston liquid container 9, band piston microorganism container 10 and pipeline vacuumize, band
The pressure of pressure gauge P5 is to close vacuum pump 15 for -0.1MPa, closes all valves.
Pump liquid of the distilled water of about 500ml as 11 liquid feeding end of constant pressure constant speed pump is added toward liquid container 12.Open constant pressure
Constant speed pump 11, sets the pressure that pumps out of 0.5MPa, and starts constant pressure constant speed pump 11 and starts to work, and pump liquid is sucked from liquid container 12；
When 11 outlet pressures of constant pressure constant speed pump reach 0.5MPa, 11 break-off of constant pressure constant speed pump.At this time, open valve Z4, Z10,
Z14 and Z18, will can be input in reaction kettle 8 with the reaction solution in piston liquid container 9, and liquid full reacts in reaction kettle 8
During 4/5 volume of kettle 8, constant pressure constant speed pump 11 is closed, closes valve Z4, Z10, Z14 and Z18.
Start constant pressure constant speed pump 11, valve Z4, Z29, Z10, Z14 and Z17 are opened, by with micro- in piston microorganism container 10
Biological solution is transported in reaction kettle by the top of reaction kettle 8.Liquid full in reaction kettle 8, injection finish.Close successively valve Z4,
Z29, Z10, Z14 and Z17.
Start high/low temperature insulating box 7, the temperature in reaction kettle 8 is reached 5 DEG C of the temperature of setting.
Using hand pump 18, back pressure liquid container 19 and back pressure container 17, the pressure value of the pressure gauge P6 of back pressure system
It is set in 10MPa.
Start air compressor 2, pressure regulator valve 31, the driving pressure for air compressor 2 being exported by pressure gauge P2 will be adjusted
Whole to predetermined driving pressure (20MPa).The valve Z25 of methane origin 1 is opened, the valve Z24 at 2 end of air compressor is opened, leads to
Booster pump 3 is crossed to start to be pressurized.Valve Z26 is opened, the gas after supercharging will be transported in gas reservoir 4, and pressure gauge P3 shows gas
Pressure in body storage tank 4.Treat pressure rise in gas reservoir 4 to predetermined pressure (20MPa).After supercharging, turn off methane
Gas source valve Z25, turns off air compressor output terminal valve Z24, turns off air compressor 2.
Experimental pressure is set as 10MPa by the second pressure regulator valve 32, opens valve Z27, adjusts the second pressure regulator valve 32, opens valve
Z21, Z5, Z9, Z13, Z18, gas mass flow controller 5 and check valve 6, gas will be transported in reaction kettle 8, to reaction
Pressure in kettle 8 reaches predetermined value (10MPa), closes valve Z27, Z21, Z5, Z9, Z13, Z18.
Again by the pressure boost in gas reservoir 4 to 20MPa, valve Z27 is opened, the pressure value for adjusting pressure regulator valve 32 is
10.2MPa, opens valve Z21, Z5, Z27 and Z18, and gas will be transported in reaction kettle 8.Toward the back pressure of back pressure system liquid feeding end
The distilled water of addition about 100ml, slowly shakes hand pump 18, pressure in back pressure system is adjusted in liquid container 19
10MPa (pressure gauge P6 readings).Valve Z19 is opened, waits 8 pressure of reaction kettle to be slightly larger than back-pressure valve pressure gauge P6 numerical value (10MPa), instead
Answer the gas in kettle 8 or gas-liquid to flow out, flow at gas-liquid separator 20.Gas flowmeter 21 measures eluting gas amount, metering
After, safety dumping to outdoor；Liquid will be flowed out in water container, Produced Liquid metering system 22 (balance) measurable outflow
Liquid quality.Slight adjustment pressure regulator valve 32, can control the outlet pressure of gas reservoir 4, you can control under corresponding pressure difference, methane by
The speed that 8 bottom of reaction kettle flows up.
During constant speed rate, the experimental implementation (establishing the upward migration process of methane) under methane flox condition：
Check whether the pressure in gas reservoir 4 is advisable higher than pressure in reaction kettle 8, at least high more than 1MPa.If gas
4 insufficient pressure of storage tank, is pressurized by gas pressurization system to gas reservoir 4.Valve Z27 is opened, the second pressure regulator valve 32, gas is stored up
4 outlet pressure adjusted value of tank opens valve Z21, Z5, Z9, Z13 and Z18 than high 0.2MPa or so in reaction kettle.Pass through gaseous mass
The setting of controller 5 inputs predetermined gas flow, and gas will be transported in reaction kettle 8 in a manner of given pace (has about 10
The delay of or so second), after about 10 seconds, valve Z18 is opened, gas will be transported in reaction kettle 8, and can be seen in sapphire form 25
Little by little migrate upwards to gas.The distilled water of addition about 100ml, delays in toward the back pressure liquid container 19 of back pressure system liquid feeding end
Hand pump 18 is slowly shaken, the pressure gauge P6 readings in back pressure system is paid close attention to, is adjusted to experimental pressure.Open valve
Z19,8 pressure of reaction kettle are more than back-pressure valve pressure gauge P6 numerical value, then the gas in reaction kettle 8 or gas-liquid will flow out, and flow to gas-liquid
At separator 20.Gas flowmeter 21 measures eluting gas amount, after metering, safety dumping to outdoor；Liquid will flow out to
In water container, the measurable trickle quality of Produced Liquid metering system 22 (balance).Set by gaseous mass controller 5 defeated
Enter predetermined gas flow, be the gas flow that methane is flowed up by 8 bottom of reaction kettle.
Control software and data collector are opened, temperature, pressure, flow and resistivity in experimentation etc. is gathered and counts
According to data are stored in computer in real time.
Water sample and gas sample are gathered when 2 is small, by liquid sampling mouth Z31-Z37, Produced Liquid metering system 22 obtains
Liquid-like, the water sample collected at 29 and gas flow meter 21 of air hatch and gas sample, detect zwitterion change in water sample and
Gas component in gas sample.
Reaction terminates, and water sample and gas sample acquisition finish, and closes all valves.Movable exhaust pipe is connected to gas flowmeter
21 ports of export, movable exhaust pipe one end move to outside window；Valve Z19 is opened, the hand pump 18 of back pressure system is adjusted, by the pressure of hand pump
Power table P6 slowly reduces stage by stage, excludes the gases at high pressure in reaction kettle 8 stage by stage.Open valve Z11 and Z22, the gas of discharge
Discharged after gas-liquid separation.Fast pressure relief：Movable exhaust pipe is connected to the air hatch Z19 of reaction kettle, movable exhaust pipe one end
Move to outside window；Valve Z19 is opened, the hand pump of back pressure system is adjusted, the pressure of hand pump instrument is slowly reduced stage by stage, sublevel
Gases at high pressure in section exclusion reaction kettle.
Data are preserved, close whole valves, Monitoring and control system is closed, turns off the power switch
Open the upper cover of reaction kettle 8, layering collection deposit/quartz sand solid sample and water sample.At the end of analysis experiment
Hydrochemical Composition feature, analyzes microorganism feature therein；By means such as X-ray diffraction, XRF, ICP-MS, scanning electron microscope,
Analyze sample component, mineral composition and microstructure.
Reaction kettle 8, band piston liquid container 9 are cleaned with distilled water and with piston microorganism container, are cleaned with distilled water dry
Net all connecting pipelines, dry up to prevent getting rusty.
Embodiment 2：(5 DEG C, 10MPa, with gas mass flow controller 10scc/min)
Preparing experiment material, configures simulated seawater solution, prepares dependent anaerobic methane oxidation bacteria and sulfate radical reducing bacteria solution, steams
Distilled water, South China Sea sediments sample, methane source of the gas, high pure nitrogen etc.；
Methane source of the gas 1, air compressor 2, gas boosting pump 3, gas reservoir 4, gas mass flow controller 5 is single
It is permanent to valve 6, high/low temperature insulating box 7, visual Hastelloy reaction kettle 8, band piston liquid container 9, band piston microorganism container 10
Fast constant pressure pump 11, liquid container 12, safety valve 13, methane alarm 14, vacuum pump 15, surge tank 16, back pressure container 17 are hand
Pump 18, back pressure liquid container 19, gas-liquid separator 20, gas flowmeter 21, Produced Liquid metering system (balance) 22, blow valve
23, back-pressure valve 24, temperature sensor 26, conductivity sensor (5) 27, inlet pressure controller 30, pressure regulator valve 31, pressure regulator valve
2 connect with pipeline and valve, close all valves, all the sensors, probe, instrument are connected on data collector, are adopted by data
Storage is connected to computer.
Turn on the power switch, check whether circuit, instrument and meter, valve and sensor work normally, inspection apparatus, pipeline and
Valve whether gas leakage；
Piston with piston liquid container 9 and with piston microorganism container 10 is placed in bottom, and loads the simulation of preparation
Sea water solution and microbial solution；
The upper cover of reaction kettle 8 is opened, deposit/quartz sand sample of about 3/5 volume is added, then covers upper cover, is connected
The each pipeline being connected with reaction kettle 8.
The switch of valve Z3, Z16, Z17, Z18, Z13, Z14, Z10, Z8, Z29, Z21, Z7 and vacuum pump 15 is opened, is carried out
Reaction kettle 8, surge tank 16, gas reservoir 4, band piston liquid container 9, band piston microorganism container 10 and pipeline vacuumize, band
The pressure of pressure gauge P5 is to close vacuum pump 15 for -0.1MPa, closes all valves.
Pump liquid of the distilled water of about 500ml as 11 liquid feeding end of constant pressure constant speed pump is added toward liquid container 12.Open constant pressure
Constant speed pump 11, sets the pressure that pumps out of 0.5Mpa, and starts constant pressure constant speed pump 11 and starts to work, and pump liquid is sucked from liquid container 12；
When 11 outlet pressures of constant pressure constant speed pump reach 0.5MPa, 11 break-off of constant pressure constant speed pump.At this time, open valve Z4, Z10,
Z14 and Z18, will can be input in reaction kettle 8 with the reaction solution in piston liquid container 9, and liquid full reacts in reaction kettle 8
During 4/5 volume of kettle 8, constant pressure constant speed pump 11 is closed, closes valve Z4, Z10, Z14 and Z18.
Start constant pressure constant speed pump 11, valve Z4, Z29, Z10, Z14 and Z17 are opened, by with micro- in piston microorganism container 10
Biological solution is transported in reaction kettle by the top of reaction kettle 8.Liquid full in reaction kettle 8, injection finish.Close successively valve Z4,
Z29, Z10, Z14 and Z17.
Start high/low temperature insulating box 7, the temperature in reaction kettle 8 is reached 5 DEG C of the temperature of setting.
Using hand pump 18, back pressure liquid container 19 and back pressure container 17, the pressure value of the pressure gauge P6 of back pressure system
It is set in 10MPa.
Start air compressor 2, the first pressure regulator valve 31, the driving for air compressor 2 being exported by pressure gauge P2 will adjust
It is whole to predetermined pressure (20MPa).The valve Z25 of methane origin 1 is opened, the valve Z24 at 2 end of air compressor is opened, passes through increasing
Press pump 3 starts to be pressurized.Valve Z26 is opened, the gas after supercharging will be transported in gas reservoir 4, and pressure gauge P3 shows gas storage
Pressure in tank 4.Treat pressure rise in gas reservoir 4 to predetermined pressure (20MPa).After supercharging, turn off methane source of the gas
Valve Z25, turns off air compressor output terminal valve Z24, turns off air compressor 2.
Experimental pressure (10MPa) is set by inlet pressure controller 30, opens valve Z27, adjusts pressure regulator valve 32, opens valve
Z21, Z5, Z9, Z13, Z18, gas mass flow controller 5 and check valve 6, gas will be transported in reaction kettle 8, to reaction
Pressure in kettle 8 reaches predetermined value (10MPa), closes valve Z27, Z21, Z5, Z9, Z13, Z18.
Again by the pressure boost in gas reservoir 4 to 20MPa, valve Z27 is opened, the pressure value for adjusting pressure regulator valve 32 is
10.2MPa, reaction kettle 8 will be transported to by opening valve Z21, Z5, gas mass flow controller 5, Z9, check valve and Z18, gas
In.Predetermined gas flow 10scc/min is inputted by the setting of gaseous mass controller 5, gas will be with the side of given pace
Formula is transported in reaction kettle 8 (delay for having about 10 seconds or so), after about 10 seconds, opens valve Z18, gas will be transported to reaction kettle
In 8, it can see that gas is little by little migrated upwards in sapphire form 25.Toward the back pressure liquid container 19 of back pressure system liquid feeding end
The distilled water of interior addition about 100ml, slowly shakes hand pump 18, pressure in back pressure system is adjusted to 10MPa (pressure gauge P6
Reading).Valve Z19 is opened, waits 8 pressure of reaction kettle to be slightly larger than back-pressure valve pressure gauge P6 numerical value (10MPa), the gas in reaction kettle 8
Or gas-liquid will flow out, and flow at gas-liquid separator 20.Gas flowmeter 21 measures eluting gas amount, after metering, safety row
Put to outdoor；Liquid will be flowed out in water container, the measurable trickle quality of Produced Liquid metering system 22 (balance).Pass through
The setting of gaseous mass controller 5 inputs predetermined gas flow 10scc/min, is that methane is flowed up by 8 bottom of reaction kettle
Gas flow 10scc/min.
Control software and data collector are opened, temperature, pressure, flow and resistivity in experimentation etc. is gathered and counts
According to data are stored in computer in real time.
Water sample and gas sample are gathered when 2 is small, by liquid sampling mouth Z31-Z37, Produced Liquid metering system 22 obtains
Liquid-like, the water sample collected at 29 and gas flow meter 21 of air hatch and gas sample, detect zwitterion change in water sample and
Gas component in gas sample.
Reaction terminates, and water sample and gas sample acquisition finish, and closes all valves.Movable exhaust pipe is connected to gas flowmeter
21 ports of export, movable exhaust pipe one end move to outside window；Valve Z19 is opened, the hand pump 18 of back pressure system is adjusted, by the pressure of hand pump
Power table P6 slowly reduces stage by stage, excludes the gases at high pressure in reaction kettle 8 stage by stage.Open valve Z11 and Z22, the gas of discharge
Discharged after gas-liquid separation.Fast pressure relief：Movable exhaust pipe is connected to the air hatch Z19 of reaction kettle, movable exhaust pipe one end
Move to outside window；Valve Z19 is opened, the hand pump of back pressure system is adjusted, the pressure of hand pump instrument is slowly reduced stage by stage, sublevel
Gases at high pressure in section exclusion reaction kettle.
Data are preserved, close whole valves, Monitoring and control system is closed, turns off the power switch
Open the upper cover of reaction kettle 8, layering collection deposit/quartz sand solid sample and water sample.At the end of analysis experiment
Hydrochemical Composition feature, analyzes microorganism feature therein；By means such as X-ray diffraction, XRF, ICP-MS, scanning electron microscope,
Analyze sample component, mineral composition and microstructure.
Reaction kettle 8, band piston liquid container 9 are cleaned with distilled water and with piston microorganism container, are cleaned with distilled water dry
Net all connecting pipelines, dry up to prevent getting rusty.
Embodiment 3：(0 DEG C, 20MPa, with gas mass flow controller 10scc/min)
Preparing experiment material, configures simulated seawater solution, prepares dependent anaerobic methane oxidation bacteria and sulfate radical reducing bacteria solution, steams
Distilled water, South China Sea sediments sample, methane source of the gas, high pure nitrogen etc.；
Methane source of the gas 1, air compressor 2, gas boosting pump 3, gas reservoir 4, gas mass flow controller 5 is single
It is permanent to valve 6, high/low temperature insulating box 7, visual Hastelloy reaction kettle 8, band piston liquid container 9, band piston microorganism container 10
Fast constant pressure pump 11, liquid container 12, safety valve 13, methane alarm 14, vacuum pump 15, surge tank 16, back pressure container 17 are hand
Pump 18, back pressure liquid container 19, gas-liquid separator 20, gas flowmeter 21, Produced Liquid metering system (balance) 22, blow valve
23, back-pressure valve 24,26,5 conductivity sensors 27 of temperature sensor, inlet pressure controller 30, pressure regulator valve 31, pressure regulator valve 2
Connected with pipeline and valve, close all valves, all the sensors, probe, instrument are connected on data collector, pass through data acquisition
Device is connected to computer.
Turn on the power switch, check whether circuit, instrument and meter, valve and sensor work normally, inspection apparatus, pipeline and
Valve whether gas leakage；
Piston with piston liquid container 9 and with piston microorganism container 10 is placed in bottom, and loads the simulation of preparation
Sea water solution and microbial solution；
The upper cover of reaction kettle 8 is opened, deposit/quartz sand sample of about 3/5 volume is added, then covers upper cover, is connected
The each pipeline being connected with reaction kettle 8.
The switch of valve Z3, Z16, Z17, Z18, Z13, Z14, Z10, Z8, Z29, Z21, Z7 and vacuum pump 15 is opened, is carried out
Reaction kettle 8, surge tank 16, gas reservoir 4, band piston liquid container 9, band piston microorganism container 10 and pipeline vacuumize, band
The pressure of pressure gauge P5 is to close vacuum pump 15 for -0.1MPa, closes all valves.
Pump liquid of the distilled water of about 500ml as 11 liquid feeding end of constant pressure constant speed pump is added toward liquid container 12.Open constant pressure
Constant speed pump 11, sets the pressure that pumps out of 0.5Mpa, and starts constant pressure constant speed pump 11 and starts to work, and pump liquid is sucked from liquid container 12；
When 11 outlet pressures of constant pressure constant speed pump reach 0.5MPa, 11 break-off of constant pressure constant speed pump.At this time, open valve Z4, Z10,
Z14 and Z18, will can be input in reaction kettle 8 with the reaction solution in piston liquid container 9, and liquid full reacts in reaction kettle 8
During 4/5 volume of kettle 8, constant pressure constant speed pump 11 is closed, closes valve Z4, Z10, Z14 and Z18.
Start constant pressure constant speed pump 11, valve Z4, Z29, Z10, Z14 and Z17 are opened, by with micro- in piston microorganism container 10
Biological solution is transported in reaction kettle by the top of reaction kettle 8.Liquid full in reaction kettle 8, injection finish.Close successively valve Z4,
Z29, Z10, Z14 and Z17.
Start high/low temperature insulating box 7, the temperature in reaction kettle 8 is reached 0 DEG C of the temperature of setting.
Using hand pump 18, back pressure liquid container 19 and back pressure container 17, the pressure value of the pressure gauge P6 of back pressure system
It is set in 20MPa.
Start air compressor 2, the first pressure regulator valve 31, the driving for air compressor 2 being exported by pressure gauge P2 will adjust
It is whole to predetermined pressure (25MPa).The valve Z25 of methane origin 1 is opened, the valve Z24 at 2 end of air compressor is opened, passes through increasing
Press pump 3 starts to be pressurized.Valve Z26 is opened, the gas after supercharging will be transported in gas reservoir 4, and pressure gauge P3 shows gas storage
Pressure in tank 4.Treat pressure rise in gas reservoir 4 to predetermined pressure (25MPa).After supercharging, turn off methane source of the gas
Valve Z25, turns off air compressor output terminal valve Z24, turns off air compressor 2.
Experimental pressure (20MPa) is set by inlet pressure controller 30, opens valve Z27, adjusts pressure regulator valve 32, opens valve
Z21, Z5, Z9, Z13, Z18, gas mass flow controller 5 and check valve 6, gas will be transported in reaction kettle 8, to reaction
Pressure in kettle 8 reaches predetermined value (20MPa), closes valve Z27, Z21, Z5, Z9, Z13, Z18.
Again by the pressure boost in gas reservoir 4 to 20MPa, valve Z27 is opened, the pressure value for adjusting pressure regulator valve 32 is
10.2MPa, reaction kettle 8 will be transported to by opening valve Z21, Z5, gas mass flow controller 5, Z9, check valve and Z18, gas
In.Predetermined gas flow 10scc/min is inputted by the setting of gaseous mass controller 5, gas will be with the side of given pace
Formula is transported in reaction kettle 8 (delay for having about 10 seconds or so), after about 10 seconds, opens valve Z18, gas will be transported to reaction kettle
In 8, it can see that gas is little by little migrated upwards in sapphire form 25.Toward the back pressure liquid container 19 of back pressure system liquid feeding end
The distilled water of interior addition about 100ml, slowly shakes hand pump 18, pressure gauge P6 readings in back pressure system is adjusted to 20MPa.
Valve Z19 is opened, waits 8 pressure of reaction kettle to be slightly larger than back-pressure valve pressure gauge P6 numerical value (20MPa), gas or gas-liquid in reaction kettle 8
It will flow out, flow at gas-liquid separator 20.Gas flowmeter 21 measures eluting gas amount, after metering, safety dumping to room
Outside；Liquid will be flowed out in water container, the measurable trickle quality of Produced Liquid metering system 22 (balance).Pass through gas matter
The setting of amount controller 5 inputs predetermined gas flow 10scc/min, is the gas that methane is flowed up by 8 bottom of reaction kettle
Flow 10scc/min.
Control software and data collector are opened, temperature, pressure, flow and resistivity in experimentation etc. is gathered and counts
According to data are stored in computer in real time.
Water sample and gas sample are gathered when 2 is small, by liquid sampling mouth Z31-Z37, Produced Liquid metering system 22 obtains
Liquid-like, the water sample collected at 29 and gas flow meter 21 of air hatch and gas sample, detect zwitterion change in water sample and
Gas component in gas sample.
Reaction terminates, and water sample and gas sample acquisition finish, and closes all valves.Movable exhaust pipe is connected to gas flowmeter
21 ports of export, movable exhaust pipe one end move to outside window；Valve Z19 is opened, the hand pump 18 of back pressure system is adjusted, by the pressure of hand pump
Power table P6 slowly reduces stage by stage, excludes the gases at high pressure in reaction kettle 8 stage by stage.Open valve Z11 and Z22, the gas of discharge
Discharged after gas-liquid separation.Fast pressure relief：Movable exhaust pipe is connected to the air hatch Z19 of reaction kettle, movable exhaust pipe one end
Move to outside window；Valve Z19 is opened, the hand pump of back pressure system is adjusted, the pressure of hand pump instrument is slowly reduced stage by stage, sublevel
Gases at high pressure in section exclusion reaction kettle.
Data are preserved, close whole valves, Monitoring and control system is closed, turns off the power switch
Open the upper cover of reaction kettle 8, layering collection deposit/quartz sand solid sample and water sample.At the end of analysis experiment
Hydrochemical Composition feature, analyzes microorganism feature therein；By means such as X-ray diffraction, XRF, ICP-MS, scanning electron microscope,
Analyze sample component, mineral composition and microstructure.
Reaction kettle 8, band piston liquid container 9 are cleaned with distilled water and with piston microorganism container, are cleaned with distilled water dry
Net all connecting pipelines, dry up to prevent getting rusty.
Above-listed detailed description is illustrating for possible embodiments of the present invention, which simultaneously is not used to limit this hair
Bright the scope of the claims, all equivalence enforcements or change without departing from carried out by the present invention, are intended to be limited solely by the scope of the claims of this case.
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.
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