CN114577667B - Reaction kettle, device and method for measuring expansion characteristics of porous medium containing hydrate - Google Patents
Reaction kettle, device and method for measuring expansion characteristics of porous medium containing hydrate Download PDFInfo
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 179
- 238000000034 method Methods 0.000 title claims abstract description 76
- 239000007788 liquid Substances 0.000 claims abstract description 173
- 230000008569 process Effects 0.000 claims abstract description 37
- 230000008859 change Effects 0.000 claims abstract description 36
- 238000001179 sorption measurement Methods 0.000 claims abstract description 25
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 15
- 230000006698 induction Effects 0.000 claims abstract description 6
- 238000003860 storage Methods 0.000 claims description 81
- 239000000523 sample Substances 0.000 claims description 72
- 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 claims description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 239000011248 coating agent Substances 0.000 claims description 12
- 238000000576 coating method Methods 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 7
- 239000012295 chemical reaction liquid Substances 0.000 claims description 6
- 238000012545 processing Methods 0.000 claims description 5
- 230000035939 shock Effects 0.000 claims description 5
- 230000006835 compression Effects 0.000 claims description 3
- 238000007906 compression Methods 0.000 claims description 3
- 230000009467 reduction Effects 0.000 claims description 3
- 230000000087 stabilizing effect Effects 0.000 claims description 2
- 239000011148 porous material Substances 0.000 claims 1
- 239000007789 gas Substances 0.000 description 156
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 239000004576 sand Substances 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000013049 sediment Substances 0.000 description 4
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000000903 blocking effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000003345 natural gas Substances 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 1
- 239000006004 Quartz sand Substances 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 230000006399 behavior Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910001919 chlorite Inorganic materials 0.000 description 1
- 229910052619 chlorite group Inorganic materials 0.000 description 1
- QBWCMBCROVPCKQ-UHFFFAOYSA-N chlorous acid Chemical compound OCl=O QBWCMBCROVPCKQ-UHFFFAOYSA-N 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 229910052900 illite Inorganic materials 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- -1 natural gas hydrates Chemical class 0.000 description 1
- VGIBGUSAECPPNB-UHFFFAOYSA-L nonaaluminum;magnesium;tripotassium;1,3-dioxido-2,4,5-trioxa-1,3-disilabicyclo[1.1.1]pentane;iron(2+);oxygen(2-);fluoride;hydroxide Chemical compound [OH-].[O-2].[O-2].[O-2].[O-2].[O-2].[F-].[Mg+2].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[K+].[K+].[K+].[Fe+2].O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2 VGIBGUSAECPPNB-UHFFFAOYSA-L 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N7/00—Analysing materials by measuring the pressure or volume of a gas or vapour
- G01N7/02—Analysing materials by measuring the pressure or volume of a gas or vapour by absorption, adsorption, or combustion of components and measurement of the change in pressure or volume of the remainder
- G01N7/04—Analysing materials by measuring the pressure or volume of a gas or vapour by absorption, adsorption, or combustion of components and measurement of the change in pressure or volume of the remainder by absorption or adsorption alone
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/04—Pressure vessels, e.g. autoclaves
- B01J3/048—Multiwall, strip or filament wound vessels
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Abstract
The invention discloses a reaction kettle, a device and a method for measuring the expansion characteristic change of a porous medium containing hydrate, wherein the reaction kettle is provided with a hollow cavity, and a soft piston is arranged in the hollow cavity so as to divide the hollow cavity into two parts, namely a pressure-covering cavity and a reaction cavity; and a stress induction film is arranged on the wall surface of the reaction cavity. The reaction kettle comprises a pressure-covering cavity and a reaction cavity, is separated by a soft piston, can measure the axial expansion of the porous medium sample containing the hydrate at constant pressure, and the stress-sensing film on the inner wall of the reaction cavity can measure the radial expansion stress of the porous medium sample containing the hydrate at constant pressure. The invention divides the expansion characteristic change process of the porous medium containing the hydrate into a porous medium liquid adsorption process, a porous medium gas adsorption process, a porous medium hydrate generation process and a porous medium hydrate decomposition process, and accurately and detailed analyzes the expansion characteristic change of the porous medium at each stage.
Description
Technical Field
The invention relates to the technical field of natural gas hydrate development, in particular to a reaction kettle, a device and a method for measuring expansion characteristic change of a porous medium containing hydrate.
Background
The natural gas hydrate is regarded as a new energy source in the 21 st century due to the characteristics of rich resources, high quality, cleanness and the like, and is the most powerful alternative energy source for petroleum and natural gas for relieving the energy crisis. Natural gas hydrate sources are mainly deposited in deep sea sedimentary layers and land permanent frozen soil layers, with about 27% land and 90% of the sea bottom considered as potential reservoirs for natural gas hydrates. About 99% of natural gas hydrate resources are allocated in the ocean sediment worldwide, and the estimated natural gas hydrate resources in the south China sea are about half of the total amount of the ascertained oil gas resources in China, so that the research on the natural gas hydrate in the ocean sediment has important significance for the development and utilization of the natural gas hydrate resources.
In 2013, the sea area natural gas hydrate trial exploitation is successfully carried out in the open sea of the well-known triple county for the first time in Japan, and in China, the sea area natural gas hydrate exploratory trial exploitation is realized in 2017 in the south sea god fox sea area, and the trial exploitation is realized in 2020. The sea natural gas hydrate reservoir is mainly a muddy silt deposit, contains porous media such as quartz sand, montmorillonite, illite, chlorite, kaolin and the like, and has the characteristics of high expansibility, high porosity and low permeability. The water absorption expansion characteristic of porous medium particles in a reservoir seriously influences the permeability change of a deposit, meanwhile, the cementation between porous mediums of the deposit is weakened due to the decomposition of hydrate, the porous medium particles shrink and fall off from the deposit to influence multiphase flow of the reservoir, so that the sand production and other problems are caused, and the measurement of the expansion characteristic change of the porous medium containing the hydrate has important significance for deeply analyzing the natural gas hydrate reservoir mechanism and solving the sand production problem in the natural gas hydrate exploitation.
The expansion characteristic of the hydrate reservoir porous medium is ignored in the conventional experiment of generating the hydrate in the porous medium, the water absorption expansion of the porous medium and the generation of the hydrate are simultaneously carried out in the experimental process, the gas diffusion channel is blocked, the generation speed of the hydrate is low, and the generation amount of the hydrate is low. Hydrate decomposition experiments in the porous medium neglect that the hydrate decomposition causes the expansion characteristic of the porous medium to change, so that the particles move and sand production occurs. Thus, the research on the device and the method for measuring the expansion characteristics of the porous medium containing the hydrate is helpful to understand the formation and decomposition behaviors of the natural gas hydrate in the porous sediment in the sea area and control factors. There is no device and method for testing the expansion characteristic change of the porous medium containing hydrate.
Disclosure of Invention
In order to solve at least one technical problem existing in the prior art, the invention provides a device and a method for measuring the expansion characteristic change of a porous medium containing hydrate.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
in a first aspect, the present invention provides a reaction kettle, the reaction kettle has a hollow cavity, in which a soft piston is disposed to divide the hollow cavity into two parts, namely a pressure-covering cavity and a reaction cavity; and a stress induction film is arranged on the wall surface of the reaction cavity.
Further, the stress sensing film is connected with a radial stress sensor.
Further, a temperature probe is arranged in the reaction cavity and connected with a temperature sensor, and a pressure probe is arranged in the reaction cavity and connected with a pressure sensor.
Further, the upper end of the pressure covering cavity is closed and provided with a liquid inlet and outlet of the pressure covering cavity; the upper part of the reaction cavity is provided with a reaction liquid inlet, and the bottom is provided with a gas inlet and a gas-producing water-producing outlet.
In a second aspect, the present invention provides a device for measuring expansion characteristics of a porous medium containing hydrate, comprising a gas supply unit, a liquid supply unit, a reaction unit, a pressure-covering control unit, a yield control unit and an environment control unit;
the reaction unit comprises the reaction kettle;
the gas supply unit is connected with a gas inlet of the reaction cavity;
the liquid supply unit is connected with a reaction liquid inlet of the reaction cavity;
the pressure control unit is connected with a pressure cavity liquid inlet and outlet of the pressure cavity;
the output control unit is connected with a gas-producing and water-producing outlet of the reaction cavity;
the environment control unit is used for controlling the reaction environment temperature in the measuring process;
the sensors for sensing the working states of the units are respectively arranged on the units and are electrically connected to the data control unit so as to control the covering pressure control unit and the stable liquid supply unit through the data control unit and further control the covering pressure and the pressure in the reaction kettle.
Further, the gas supply unit comprises a gas input pipeline connected with a gas inlet of the reaction cavity, and a gas cylinder, a gas booster pump, a buffer container, a gas storage tank and a control valve which are arranged on the gas input pipeline and are sequentially connected, wherein a sensor of the gas supply unit is a sensor with a pressure sensor and a control valve on a pipeline, the pressure sensor is electrically connected to the data control unit for carrying out data processing of injection pressure, and the control valve is electrically connected to the data control unit for controlling the opening of the control valve by the sensor; one end of the gas storage tank is connected with the buffer container, pressurized gas in the buffer container enters the gas storage tank, the other end of the buffer container is connected with the reaction kettle through a tee joint, one end of the tee joint is connected with the reaction kettle, the other end of the tee joint is connected with the control valve, and gas in the gas storage tank directly enters the reaction kettle or is controlled by the control valve to enter the reaction kettle;
the output control unit comprises a gas-liquid separator, a liquid container and an electronic balance, wherein the gas-liquid separator is a cavity, the middle part of the gas-liquid separator is provided with an output inlet and is connected with the reaction unit through a pipeline, the upper part of the gas-liquid separator is provided with a gas outlet and is connected with a gas storage tank and a control valve of the gas supply unit through pipelines, the lower part of the gas-liquid separator is provided with a liquid outlet which is directly connected with the liquid container, the liquid container is placed on the electronic balance, and the electronic balance is electrically connected with the data control unit through a sensor to analyze the output liquid.
Further, the pressure-covering control unit comprises a shaft pressure pump and a liquid flowmeter, the other end of the liquid flowmeter is connected with a pressure-covering cavity liquid inlet and outlet of the reaction kettle, a liquid cavity is arranged in the shaft pressure pump, and liquid in the liquid cavity is injected into the pressure-covering cavity of the reaction kettle through a pipeline by the liquid flowmeter; the pressure sensor of the pressure-covering control unit is an axial pressure pump, a liquid flowmeter and a pressure sensor of the pressure-covering cavity, the pressure sensor of the pressure-covering cavity is electrically connected to the data control unit for pressure data processing of the pressure-covering cavity, the axial pressure pump is electrically connected to the data control unit by the sensor for pressure control of the pressure in the pressure-covering cavity, the liquid quantity is injected or withdrawn into the pressure-covering cavity according to the pressure data of the pressure-covering cavity, and the liquid flowmeter is electrically connected to the data control unit by the sensor for recording the injected or withdrawn liquid quantity.
Further, the liquid supply unit comprises a liquid input pipeline connected with the reaction liquid inlet, a advection pump, a piston container and a liquid flowmeter which are sequentially connected with the liquid input pipeline; the sensor of the liquid supply unit is a liquid flowmeter, and the liquid flowmeter inputs the measured liquid flow to the data control unit for data processing of the injected liquid.
Further, the environmental control unit comprises a controllable constant temperature water bath; the reaction unit, the gas storage tank of the gas supply unit and the pipeline for connecting the reaction unit and the gas storage tank are all arranged in a controllable constant-temperature water bath.
In a third aspect, the present invention provides a method of measuring a change in expansion characteristics of a porous hydrated dielectric, using an apparatus for measuring a change in expansion characteristics of a porous hydrated dielectric as defined in any one of the preceding claims, comprising the steps of:
s1, porous medium liquid adsorption process: setting the experimental environment temperature T i And setting the pressure P of the reaction chamber Kettle 0 Control the pressure P of the pressure-covering cavity Cover 0 ＞P Kettle 0 Injecting liquid into the reaction cavity by adopting a stable liquid supply unit, adsorbing the liquid into the dried porous medium sample, and recording the adsorbed liquid amount n by a liquid flowmeter Liquid and its preparation method ；
S2, gas adsorption in a porous medium: injecting experimental gas into a reaction cavity of a reaction kettle by adopting a gas supply unit, wherein the experimental pressure is P Kettle suction The experimental gas is adsorbed into the porous medium sample which is completely adsorbed with the liquid in the step S1, and the constant pressure adsorption is adopted, so that the pressure of the reaction cavity is controlled to be constant to be the experimental pressure P Kettle 0 ＝P Kettle suction Control of pressure data P of a pressure-covering chamber Cover 0 ＞P Kettle 0 Wherein the pressure P of the gas storage tank is ensured before the gas is adsorbed Store 0 >P Kettle 0 The porous medium sample completes gas adsorption, and the gas storage tank has pressure P Storage i The gas variation n of the gas storage tank can be calculated and obtained according to the method 1 i I.e. the gas adsorption quantity n of the porous medium sample entering the reaction cavity i ＝n Air flow ：
In the formula DeltaP Storage device Is the pressure difference delta P in the air storage tank Storage device ＝|P Store 0 -P Storage i |，V Storage device Is the volume of the air storage tank, Z i For the compression factor, T, of the experimental gas under the conditions of ambient temperature and pressure at the moment i i For the ambient temperature at reaction i, R is the gas constant 8.3145 J.mol -1 ·K -1 ；
S3, generating a hydrate in the porous medium: the porous medium sample which completely absorbs the gas in the step S2 is adopted, and the environment temperature is reduced to be the gas hydrate generation experimental temperature T Raw materials Generating gas hydrate by a constant pressure method, and controlling the pressure of a reaction cavity to be constant at experimental pressure P Kettle 0 ＝P Kettle life Control of pressure data P of a pressure-covering chamber Cover 0 ＞P Kettle 0 Wherein the pressure P of the gas storage tank is ensured before the hydrate is generated Store 0 >P Kettle 0 After the gas hydrate in the porous medium sample is completely generated, the gas variation n of the gas storage tank is obtained by calculating in the formula 1 in the step S2 i I.e. the gas consumption n of the porous medium sample to generate hydrate Raw materials ；
S4, decomposing the hydrate in the porous medium: decomposing gas hydrate by adopting a constant-pressure heat shock method or a constant-pressure depressurization method; constant pressure heat shock method, setting experimental environment temperature T i Is T Dividing into Hydrate in the gas hydrate-containing porous medium sample is decomposed, and the pressure of the reaction cavity is controlled to be constant to be experimental pressure P Kettle 0 ＝P Kettle life Controlling the pressure P of the pressure-covering cavity Cover 0 ＞P Kettle 0 Wherein the pressure P of the gas storage tank is ensured before the hydrate is decomposed Store 0 <P Kettle 0 After the gas hydrate in the porous medium sample is completely decomposed, the gas variation n of the gas storage tank can be obtained by calculating in the formula 1 in the step S2 i I.e. the gas yield n of decomposing the hydrate in the porous medium sample Dividing into The method comprises the steps of carrying out a first treatment on the surface of the Constant pressure depressurization method for maintaining experimental environment temperature T i Is T Raw materials Reducing the pressure P of the reaction chamber Kettle i The control valve is controlled to release free gas to the gas storage tank to ensure the pressure P of the gas storage tank Store 0 <P Kettle 0 When the pressure of the reaction cavity is constant P Kettle 0 ＝P Kettle separator When the gas change amount n of the gas storage tank is obtained by calculating the formula 1 in the step S2 i I.e. the free gas amount n released by the hydrate in the sample of the porous medium by pressure reduction and decomposition Self-supporting Hydrate starts to decompose, and the pressure of the reaction cavity is controlled to be constant to be experimental pressure P Kettle 0 ＝P Kettle separator Controlling the pressure P of the pressure-covering cavity Cover 0 ＞P Kettle 0 The gas hydrate in the porous medium sample is completely decomposed, and the gas consumption n of the gas storage tank is obtained by calculating in the step S2 in the formula 1 i I.e. the gas yield n of decomposing the hydrate in the porous medium sample Dividing into 。
Further, the pressure of the covering pressure cavity is set to be larger than the pressure P in the reaction cavity Coating 0＝P Kettle The porous medium sample in the reaction cavity is compacted by the covering pressure at 0+0.1mpa, the bearing capacity of the porous medium sample plus the pressure in the reaction cavity and the pressure in the covering pressure cavity form force balance, and when the pressure in the reaction cavity and the pressure in the covering pressure cavity are controlled to be constant, the soft piston between the covering pressure cavity and the reaction cavity does not move; according to the change of the bearing capacity of the porous medium sample, the soft piston between the pressure-covering cavity and the reaction cavity moves, the volume in the pressure-covering cavity changes, the liquid quantity in the pressure-covering cavity changes, the liquid flow meter of the pressure-covering control unit records the liquid inlet or outlet Mi, and simultaneously, according to the stress induction film on the inner wall of the reaction cavity of the reaction kettle, the radial expansion stress of the porous medium sample is measured, and according to the injected liquid quantity n Liquid and its preparation method Adsorbed gas amount n Air flow Hydrate forming gas consumption n of porous media sample Raw materials Gas production n of decomposing hydrate in porous Medium sample Dividing into Porous media axial direction combined with measurementThe expansion amount and radial expansion stress are used for obtaining the expansion characteristic change of the porous medium containing the hydrate under different experimental conditions.
Further, reaction chamber pressure P Kettle i Collected by a data control unit through a pressure sensor and according to the collected P Kettle i Data for controlling the on-off of the control valve of the gas supply unit and stably controlling the pressure in the reaction chamber to be P Kettle 0 The method comprises the following specific steps:
when P Kettle i <P Kettle 0 When the control valve is opened, gas in the gas storage tank is injected into the reaction cavity through the control valve, and the pressure P in the reaction cavity Kettle i ＝P Kettle 0 Closing the control valve;
when P Kettle i >P Kettle 0 When the control valve is opened, the gas in the reaction cavity is discharged into the gas storage tank through the control valve, and the pressure P in the reaction cavity Kettle i ＝P Kettle 0 Closing the control valve;
pressure data P of the pressure-coated chamber Covering i By a set of data control units via pressure sensors and according to the collected P Covering i Data, controlling the switch of the axial pump of the pressure covering unit, and stabilizing the pressure P of the pressure covering cavity Cover 0 The method comprises the following specific steps:
when P Covering i <P Cover 0 The axial pressure pump is started, and the liquid in the liquid cavity of the axial pressure pump is injected into the pressure covering cavity until the pressure P of the pressure covering cavity Covering i ＝P Cover 0 Closing the axial pressure pump;
when P Covering i >P Cover 0 The axial pressure pump is started, and the liquid in the pressure coating cavity is withdrawn to the liquid cavity of the axial pressure pump until the pressure P in the pressure coating cavity Covering i ＝P Cover 0 The axial pressure pump is turned off.
Compared with the prior art, the invention has the beneficial effects that:
1. the reaction kettle in the device comprises a pressure-covering cavity and a reaction cavity, and is separated by a soft piston, so that the axial expansion of a porous medium sample containing hydrate can be measured at constant pressure, and the stress-sensing film on the inner wall of the reaction cavity can measure the radial expansion stress of the porous medium sample containing hydrate at constant pressure;
2. the invention provides a constant pressure method for testing the expansion characteristic change of a porous medium containing hydrate, wherein a control valve and a shaft pressure pump are adopted to respectively control the pressure of a pressure covering cavity and the pressure of a reaction cavity to be constant, so that an accurate measurement method is provided for the axial expansion change of the porous medium;
3. the invention divides the expansion characteristic change process of the porous medium containing the hydrate into a porous medium liquid adsorption process, a porous medium gas adsorption process, a porous medium hydrate generation process and a porous medium hydrate decomposition process, accurately and detailed analyzes the expansion characteristic change of the porous medium at each stage, and provides effective experimental equipment and a testing method for the generation and decomposition research of the hydrate in the submarine sediment with the expansion characteristic.
Drawings
FIG. 1 is a schematic flow chart of an apparatus for measuring the change of expansion characteristics of a porous medium containing hydrate according to the present invention;
FIG. 2 is a schematic diagram of a one-dimensional autoclave in the apparatus of the present invention;
reference numerals: 1. gas cylinder 2, gas booster pump 3, buffer vessel 4, gas storage tank 5, control valve 6, gas-liquid separator 7, liquid vessel 8, electronic balance 9, reactor vessel 10, pressure-sensitive chamber 11, reaction chamber 12, advection pump 13, piston vessel 14, axial pump 15, liquid flowmeter 16, pressure sensor 17, temperature sensor 18, radial stress sensor 19, valve 20, controllable thermostatic water bath 21, data collector 22, data control and storage 23, pressure-sensitive chamber liquid inlet and outlet 24, soft piston 25, stress-sensitive film 26, filter screen 27, gas inlet 28, gas-producing water outlet 29, reactive liquid inlet.
Detailed Description
Examples:
in the description of the present invention, it should be noted that, unless explicitly specified and limited otherwise, the terms "mounted", "connected" and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected or integrally connected; the device can be mechanically connected, electrically connected and signal connected; the two elements may be directly connected or indirectly connected through an intermediate medium, so to speak, the two elements are communicated internally. It will be understood by those of ordinary skill in the art that the terms described above are in the specific sense of the present invention. The technical scheme of the invention is further described below with reference to the accompanying drawings and examples.
As shown in fig. 1, a device for measuring the expansion characteristic change of a porous medium containing hydrate comprises a gas supply unit, a liquid supply unit, a reaction unit, a covering pressure control unit, a production control unit, an environment control unit and a data control unit, wherein the units are respectively provided with a sensor for sensing the working state of each unit, and the sensors are electrically connected to the data control unit.
The gas supply unit comprises a gas cylinder 1, a gas booster pump 2, a buffer container 3, a gas storage tank 4 and a control valve 5 which are arranged on a gas input pipeline and are sequentially connected, the pressure sensor 16 is electrically connected to the data control unit for carrying out data processing of injection pressure, and the control valve 5 is electrically connected to the data control unit by the sensor for controlling the opening of the control valve 5; one end of the gas storage tank 4 is connected with the buffer container 3, pressurized gas in the buffer container 3 enters the gas storage tank 4, the other end of the gas storage tank is connected with the reaction kettle 9 through a tee joint, one end of the tee joint is connected with the control valve 5, and gas in the gas storage tank 4 can directly enter the reaction kettle 9 or can be controlled by the control valve 5 to enter the reaction kettle 9.
The reaction unit is a high-pressure one-dimensional reaction kettle 9, the reaction kettle 9 is a sealed container, 4 interfaces are arranged at the bottom 1 of the reaction kettle 9, a gas inlet is formed by connecting one end of a tee joint with a gas storage tank 4, one end of the tee joint is connected with a control valve 5, 1 interface at the bottom of the reaction kettle 9 is connected with a gas-liquid separator 6 of a production control unit, 1 interface at the upper part of the reaction kettle 9 is connected with a liquid flowmeter 15 of a stable liquid supply unit, and 1 interface at the top of the reaction kettle 9 is connected with a liquid flowmeter 15 of a pressure covering control unit. As shown in fig. 2, the reaction kettle 9 is provided with a hollow cavity, the upper part of the hollow cavity is a pressure-covering cavity 10, the upper end of the pressure-covering cavity 10 is closed and is provided with a pressure-covering cavity liquid inlet and outlet 23, the lower part of the hollow cavity is a reaction cavity 11, the middle of the pressure-covering cavity 10 and the reaction cavity 11 is separated by a soft piston 24, the upper part of the reaction cavity 11 is provided with a reaction liquid inlet 29, the bottom is provided with a gas inlet 27 and a gas-producing water outlet 28 and is paved with a filter screen 26, the middle part of the reaction cavity 11 is provided with a temperature probe connected with a temperature sensor 17, the pressure probe is connected with a pressure sensor 16, and the wall surface of the reaction cavity 11 is provided with a stress-sensing film 25 connected with a radial stress sensor 18. Therefore, the reaction kettle comprises the pressure-covering cavity and the reaction cavity, and is separated by the soft piston, so that the axial expansion of the porous medium sample containing the hydrate can be measured at constant pressure, and the stress-sensing film on the inner wall of the reaction cavity can be used for measuring the radial expansion stress of the porous medium sample containing the hydrate at constant pressure.
The pressure-covering control unit comprises a shaft pressure pump 14 and a liquid flowmeter 15, one end of the liquid flowmeter 15 is connected with the shaft pressure pump 14, and the other end is connected with 1 interface at the top of the reaction kettle 9; the stable liquid supply unit comprises a advection pump 12, a piston container 13, a liquid flowmeter 15 and a liquid flowmeter 15, wherein the advection pump 12, the piston container 13 and the liquid flowmeter 15 are arranged on a liquid input pipeline and are sequentially connected with each other, and the liquid flowmeter 15 is connected with an upper interface of the reaction kettle 9; the output control unit comprises a gas-liquid separator 6, a liquid container 7 and an electronic balance 8, wherein the gas-liquid separator 6 is a cavity, the middle part of the gas-liquid separator is provided with an output inlet, the gas-liquid separator is connected with a gas-producing water-producing outlet at the bottom of a reaction kettle 9 through a pipeline, the upper part of the gas-liquid separator 6 is provided with a gas outlet, one end of the gas-liquid separator is connected with a gas storage tank 4 through a three-way pipeline, the other end of the gas-liquid separator is connected with a control valve 5, the lower part of the gas-liquid separator 6 is provided with a liquid outlet, the liquid container 7 is directly connected with the liquid container 7, the liquid container 7 is placed on the electronic balance 8, and the weight of liquid in the liquid container 7 can be weighed.
The environment control unit is a controllable constant temperature water bath 20, and the reaction kettle 9, the gas storage tank 4 and the pipelines for connecting the two are all arranged in the controllable constant temperature water bath 20.
The data control unit comprises a data collector 21 and a data control and storage 22, wherein the data collector 21 is electrically connected with the sensors on the reaction unit, the pressure covering control unit, the gas supply unit, the stable liquid supply unit, the output control unit and the environment control unit to collect corresponding data of each sensor, the data control and storage 22 is electrically connected with the data collector 21 to store the data collected by the data collector 21, and the data control and storage 22 controls the opening and closing of the axial pressure pump 14 and the control valve 5 by adopting software.
The working principle of the device is as follows:
the porous medium sample is placed in the reaction cavity of the reaction kettle 9 in a sealing way; the experimental gas is pressurized and injected into the gas storage tank 4 from the gas bottle 1 sequentially through the gas booster pump 2 and the buffer container 3, and high-pressure gas in the gas storage tank 4 can be directly injected into the reaction kettle 9 or the injection pressure is controlled to be injected into the reaction kettle 9 through the control valve 5; the experimental liquid sequentially passes through a horizontal pump 12 and a piston container 13, and a liquid flowmeter 15 is directly injected into the reaction kettle 9; the pressure of the reaction cavity 11 of the reaction kettle 9 is collected and processed by a data control unit, and the data control unit controls the control valve 5 to be opened and closed according to the pressure of the reaction cavity 11, so that the pressure in the reaction cavity 11 is kept constant; the liquid in the pressure-covering cavity 10 is injected into the pressure-covering cavity 10 of the reaction kettle 9 through the axial pressure pump 14 and the liquid flowmeter 15, the pressure in the pressure-covering cavity 10 is collected and processed by the data control unit, and the data control unit controls the on-off of the axial pressure pump 14 according to the pressure in the reaction cavity 10, so that the pressure in the pressure-covering cavity is kept constant; the controllable constant-temperature water bath 20 controls the experimental reaction temperature to be constant; the whole experimental process reaction kettle 9 is constant in pressure, according to experimental requirements, liquid is injected firstly to complete the liquid adsorption process, then gas is injected to complete the gas adsorption process, the temperature is reduced to complete the hydrate generation process, the temperature is increased or the pressure is reduced to complete the hydrate decomposition process, the axial expansion variation of the porous medium is recorded through the liquid flowmeter 15 of the pressure-covering control unit, and the radial expansion stress of the porous medium sample can be measured through the stress induction film 25.
Correspondingly, the embodiment also provides a method for measuring the expansion characteristic change of the porous medium containing the hydrate, which divides the expansion change process into a porous medium liquid adsorption process, a porous medium gas adsorption process, a porous medium hydrate generation process and a porous medium hydrate decomposition process, and accurately and specifically analyzes the expansion characteristic change of the porous medium at each stage. Firstly, placing the dried porous medium into a reaction cavity 11, sealing a reaction kettle 9, and then completing the following steps:
(1) Porous media liquid adsorption process
Setting a controllable constant-temperature water bath to set the water bath 20 temperature T i Is at normal temperature T Suction pipe Setting the pressure P of the reaction chamber 11 Kettle 0 =0.1 MPa, i.e. the reaction chamber 11 is vented to atmosphere, controlling the pressure P in the pressure-applying chamber 10 Cover 0 ＝P Kettle 0 The experimental liquid is injected into the reaction cavity 11 through the advection pump 12 and the piston container 13 and the liquid flowmeter 15, the liquid is absorbed into the dried porous medium sample, and the experimental liquid is controlled by the control unit when being covered with the pressureThe liquid flowmeter 15 detects that no liquid enters or exits for 1 day, the porous medium sample completely absorbs the liquid, and the liquid flowmeter 15 records the absorption liquid amount n Liquid and its preparation method ；
(2) Gas adsorption process in porous media
Setting a controllable constant-temperature water bath to set the water bath 20 temperature T i Is at normal temperature T Suction pipe The experimental gas is injected into the reaction cavity 11 from the gas cylinder 1 through the gas booster pump 2, the buffer container 3 and the gas storage tank 4, and the experimental pressure in the reaction cavity 11 is P Kettle suction The experimental gas is absorbed into the porous medium sample which completely absorbs the liquid, and the pressure P of the reaction cavity 11 is generated due to the gas absorption Kettle i Reducing, adopting constant pressure adsorption in the gas adsorption process, and controlling the pressure of the reaction cavity 11 to be constant at experimental pressure P Kettle 0 ＝P Kettle suction Control of the pressure data P of the pressure-covering chamber 9 Cover 0 ＝P Kettle 0 +0.1MPa, wherein the pressure P of the gas tank 4 is ensured before gas adsorption Store 0 ＝P Storage and suction type And P is Storage and suction type >P Kettle 0 When the pressure P of the air storage tank 4 Storage i After the porous medium sample is kept unchanged for 1 day, the porous medium sample completes gas adsorption, and the gas change amount n of the gas storage tank 4 can be calculated according to the formula 1 i I.e. the gas adsorption quantity n of the porous medium sample entering the reaction chamber 11 i ＝n Air flow ：
In the formula DeltaP Storage device Is the pressure difference delta P in the air storage tank 4 Storage device ＝|P Store 0 -P Storage i |，V Storage device For the volume of the air storage tank 4, Z i For the compression factor, T, of the experimental gas under the conditions of ambient temperature and pressure at the moment i i For the ambient temperature at reaction i, R is the gas constant 8.3145 J.mol -1 ·K -1 ；
(3) Hydrate formation process in porous medium
Adopting porous medium sample with adsorbed gas, generating gas hydrate by constant pressure method, reducing environmental temperature, and setting controllable constant temperature water bath 20 temperature T i Experimental temperature for gas hydrate formationT Raw materials Gas hydrate in the porous medium sample is generated, free gas in the reaction cavity 11 is consumed, and the pressure P is Kettle i Reducing and controlling the pressure of the reaction cavity 11 to be constant as the experimental pressure P Kettle 0 ＝P Kettle life Controlling the pressure P of the pressure-covering chamber 10 Cover 0 ＝P Kettle 0 +0.1MPa, wherein the pressure P of the gas tank 4 is ensured before hydrate formation Store 0 ＝P Chu Sheng And P is Chu Sheng >P Kettle 0 When the pressure P of the air storage tank 4 Storage i The gas hydrate in the porous medium sample is completely generated after the gas is kept unchanged for 1 day, and the gas variation n of the gas storage tank 4 is obtained by calculating the formula 1 i I.e. the gas consumption n of the porous medium sample to generate hydrate Raw materials The method comprises the steps of carrying out a first treatment on the surface of the (4) Hydrate decomposition process in porous medium
And decomposing the gas hydrate by adopting a constant-pressure heat shock method or a constant-pressure depressurization method. Constant pressure heat shock method: setting a controllable constant-temperature water bath 20 temperature T i Is T Dividing into Hydrate in the gas hydrate-containing porous medium sample is decomposed, free gas in the reaction cavity 11 is increased, and the pressure P is increased Kettle i The pressure of the reaction chamber 11 is controlled to be constant to be the experimental pressure P Kettle 0 ＝P Kettle life Controlling the pressure P of the pressure-covering chamber 10 Cover 0 ＝P Kettle 0 In +0.1Mpa, because sand production occurs in the decomposition process, in order to prevent sand from blocking a pipeline and damaging a control valve 5, decomposed gas firstly flows out of a reaction kettle 9 and passes through a gas-liquid separator 6, gas is separated from gas and then flows into a gas storage tank 4 from a gas outlet at the upper part of the gas-liquid separator 6 through the control valve 5, liquid directly enters a liquid container 7 from a liquid outlet at the lower part of the gas-liquid separator 6, and the weight of the produced liquid is weighed by an electronic balance 8; ensuring the pressure P of the gas-liquid separator 6 before decomposing the hydrate Separation 0 ＝P Kettle 0 Pressure P of the air tank 4 Store 0 ＝P Store and divide And P is Store and divide <P Kettle 0 When the pressure P of the air storage tank 4 Storage i The gas hydrate in the porous medium sample is completely decomposed after the gas is kept unchanged for 1 day, and the gas change amount n of the gas storage tank 4 can be calculated according to the formula 1 i I.e. the gas yield n of decomposing the hydrate in the porous medium sample Dividing into The method comprises the steps of carrying out a first treatment on the surface of the Constant pressure depressurization: maintaining the temperature T of the controllable constant-temperature water bath 20 i Is T Raw materials Reducing the pressure P of the reaction chamber 11 Kettle i The free gas is released to the gas storage tank 4 through the control valve 5, sand is produced in the decomposition process, in order to prevent sand from blocking a pipeline and damaging the control valve 5, the decomposed gas firstly flows out of the reaction kettle 9 and passes through the gas-liquid separator 6, the gas is separated from the gas outlet at the upper part of the gas-liquid separator 6 and passes through the control valve 5 before entering the gas storage tank 4, the liquid directly enters the liquid container 7 from the liquid outlet at the lower part of the gas-liquid separator 6, and the weight of the produced liquid is weighed by the electronic balance 8; ensuring the pressure P of the gas-liquid separator 6 before decomposing the hydrate Separation 0 ＝P Kettle 0 Pressure P of the air tank 4 Store 0 ＝P Stored self And P is Stored self <P Kettle 0 When the pressure of the reaction chamber 11 is constant P Kettle 0 ＝P Kettle separator At the time, the air storage tank 4 pressure P Storage i ＝P Store and divide Can calculate and obtain the gas variation n of the gas storage tank i I.e. the free gas amount n released by the hydrate in the sample of the porous medium by pressure reduction and decomposition Self-supporting Hydrate starts to decompose, free gas in the reaction chamber 11 increases, and the pressure P Kettle i The pressure of the reaction chamber 11 is controlled to be constant to be the experimental pressure P Kettle 0 ＝P Kettle separator Controlling the pressure P of the pressure-covering chamber 10 Cover 0 ＝P Kettle 0 +0.1MPa, when the pressure P of the air storage tank 4 is Storage i The gas hydrate in the porous medium sample is completely decomposed after the gas is kept unchanged for 1 day, and the gas consumption n of the gas storage tank can be calculated according to the formula 1 i I.e. the gas yield n of decomposing the hydrate in the porous medium sample Dividing into ；
(5) Measurement of changes in expansion characteristics of porous hydrate-containing Medium
Setting the pressure P of the pressure-covering chamber 10 Cover 0 ，P Cover 0 ＝P Kettle 0 The porous medium sample in the reaction cavity 11 is compacted by the coating pressure of +0.1Mpa, the bearing capacity of the porous medium sample plus the pressure in the reaction cavity 11 and the pressure in the coating pressure cavity 10 form force balance, when the pressure in the reaction cavity 11 and the pressure in the coating pressure cavity 10 are controlled to be constant, the soft piston 24 between the coating pressure cavity 10 and the reaction cavity 11 does not move, the expansion characteristics of the porous medium sample are changed in the 4 processes, namely, the bearing capacity of the porous medium sample is changed, the soft piston 24 between the coating pressure cavity 10 and the reaction cavity 11 moves,the volume in the pressure-covering cavity 10 changes, and the constant pressure control is performed in the pressure-covering cavity 10, so that the liquid volume in the pressure-covering cavity 10 changes, the liquid enters or exits from the pressure-covering cavity liquid inlet and outlet 23, passes through the liquid flowmeter 15, enters or exits to the liquid cavity of the axial pressure pump 14, and the liquid flowmeter 15 records the liquid entering or exiting volume V Liquid and its preparation method Namely, the volume in the pressure-covering cavity 10 changes, so that the axial expansion change of the porous medium sample in the process is obtained, and meanwhile, the stress-sensing film 25 on the inner wall of the reaction cavity 11 can measure the radial expansion change stress of the porous medium sample in the process; injected liquid amount n combining the above 4 processes Liquid and its preparation method Adsorbed gas amount n Air flow Gas consumption n of hydrate formation Raw materials Gas production amount n of decomposed hydrate Dividing into The expansion characteristic change of the porous medium containing the hydrate under different experimental conditions can be obtained.
Thus, the expansion characteristic change of the porous medium at each stage can be accurately and detailedly analyzed through the steps
In this embodiment:
(1) Reaction chamber constant pressure control
Pressure P of reaction chamber 11 Kettle i The data is collected 21 by a data collector of a data control unit through a pressure sensor, and the data control unit data control and memory 22 is used for collecting P Kettle i Data, switch of the control valve 5 is set, pressure in the reaction chamber 11 is stably controlled to be experimental pressure P Kettle 0 The method comprises the following specific steps:
when P Kettle i <P Kettle 0 When the control valve 5 is opened, the gas in the gas storage tank 4 is injected into the reaction chamber 11 through the control valve 5, and the pressure P in the reaction chamber 11 Kettle i ＝P Kettle 0 Closing the control valve 5;
when P Kettle i >P Kettle 0 When the control valve 5 is opened, the gas in the reaction chamber 11 is discharged into the gas storage tank 4 through the control valve 5, and the pressure P in the reaction chamber 11 Kettle i ＝P Kettle 0 Closing the control valve 5;
(2) Constant pressure control of pressure-covered cavity
Pressure data P of the blanket chamber 10 Covering i Controlled by data via pressure sensorsThe data collector of the unit collects 21, the data control unit controls the on-off of the axial pressure pump 14 through data control and the memory 22, and the pressure of the pressure covering cavity 10 is stably controlled to be P Cover 0 The method comprises the following specific steps:
when P Covering i <P Cover 0 The axial pressure pump 14 is turned on, and the liquid in the liquid chamber of the axial pressure pump is injected into the pressure-covering chamber 10 until the pressure P of the pressure-covering chamber 10 Covering i ＝P Cover 0 Closing the axial pressure pump 14;
when P Covering i >P Cover 0 The axial pressure pump 14 is opened, and the liquid in the coating cavity 10 is discharged to the liquid cavity of the axial pressure pump 14 until the pressure P of the coating cavity 10 Covering i ＝P Cover 0 The axial pressure pump 14 is turned off.
The above embodiments are only for illustrating the technical concept and features of the present invention, and are intended to enable those skilled in the art to understand the content of the present invention and implement the same, and not to limit the scope of the present invention. All equivalent changes or modifications made in accordance with the essence of the invention should be covered in the scope of the invention.
Claims (3)
1. A method for measuring the expansion characteristic change of a porous medium containing hydrate by using a device for measuring the expansion characteristic change of the porous medium containing hydrate is characterized in that,
the device for measuring the change of the expansion characteristic of the porous medium containing the hydrate comprises: the device comprises a gas supply unit, a stable liquid supply unit, a reaction unit, a pressure-covering control unit, a yield control unit and an environment control unit;
the reaction unit comprises a reaction kettle, wherein the reaction kettle is provided with a hollow cavity, and a soft piston is arranged in the hollow cavity so as to divide the hollow cavity into two parts, namely a pressure-covered cavity and a reaction cavity; a stress induction film is arranged on the wall surface of the reaction cavity; the stress sensing film is connected with a radial stress sensor; a temperature probe is arranged in the reaction cavity and connected with a temperature sensor, and a pressure probe is arranged in the reaction cavity and connected with a pressure sensor; the upper end of the pressure-covering cavity is closed and provided with a liquid inlet and outlet of the pressure-covering cavity; the upper part of the reaction cavity is provided with a reaction liquid inlet, and the bottom is provided with a gas inlet and a gas-producing water-producing outlet;
the gas supply unit is connected with a gas inlet of the reaction cavity;
the stable liquid supply unit is connected with a reaction liquid inlet of the reaction cavity;
the pressure control unit is connected with a pressure cavity liquid inlet and outlet of the pressure cavity;
the output control unit is connected with a gas-producing and water-producing outlet of the reaction cavity;
the environment control unit is used for controlling the reaction environment temperature in the measuring process;
the sensors are respectively arranged on the units and used for sensing the working states of the units, and the sensors are electrically connected to the data control unit so as to control the operation of the pressure covering control unit and the stable liquid supply unit through the data control unit and further control the pressure covering and the pressure in the reaction kettle;
the pressure-covering control unit comprises a shaft pressure pump and a liquid flowmeter, the other end of the liquid flowmeter is connected with a liquid inlet and outlet of a pressure-covering cavity of the reaction kettle, a liquid cavity is arranged in the shaft pressure pump, and liquid in the liquid cavity is injected into the pressure-covering cavity of the reaction kettle through a pipeline by the liquid passing through the liquid flowmeter; the pressure sensor of the pressure-covering control unit is an axial pressure pump, a liquid flowmeter and a pressure sensor of the pressure-covering cavity, the pressure sensor of the pressure-covering cavity is electrically connected to the data control unit for pressure data processing of the pressure-covering cavity, the axial pressure pump is electrically connected to the data control unit by the sensor for pressure control of the pressure in the pressure-covering cavity, the liquid quantity is injected or withdrawn into the pressure-covering cavity according to the pressure data of the pressure-covering cavity, and the liquid flowmeter is electrically connected to the data control unit by the sensor for recording the injected or withdrawn liquid quantity;
the method comprises the following steps:
s1, porous medium liquid adsorption process: setting the experimental environment temperature T i And setting the pressure P of the reaction chamber Kettle 0 Control the pressure P of the pressure-covering cavity Cover 0 ＞P Kettle 0 Injecting liquid into the reaction cavity by adopting a stable liquid supply unit, adsorbing the liquid into the dried porous medium sample, and recording the adsorbed liquid amount n by a liquid flowmeter Liquid and its preparation method ；
S2, multipleGas adsorption process in pore medium: injecting experimental gas into a reaction cavity of a reaction kettle by adopting a gas supply unit, wherein the experimental pressure is P Kettle suction The experimental gas is adsorbed into the porous medium sample which is completely adsorbed with the liquid in the step S1, and the constant pressure adsorption is adopted, so that the pressure of the reaction cavity is controlled to be constant to be the experimental pressure P Kettle 0 ＝P Kettle suction Control of pressure data P of a pressure-covering chamber Cover 0 ＞P Kettle 0 Wherein the pressure P of the gas storage tank is ensured before the gas is adsorbed Store 0 >P Kettle 0 The porous medium sample completes gas adsorption, and the gas storage tank has pressure P Storage i The gas variation n of the gas storage tank can be calculated and obtained according to the method 1 i I.e. the gas adsorption quantity n of the porous medium sample entering the reaction cavity Air flow ：
In the formula DeltaP Storage device Is the pressure difference delta P in the air storage tank Storage device ＝|P Store 0 -P Storage i |，V Storage device Is the volume of the air storage tank, Z i For the compression factor, T, of the experimental gas under the conditions of ambient temperature and pressure at the moment i i For the ambient temperature at reaction i, R is the gas constant 8.3145 J.mol -1 ·K -1 ；
S3, generating a hydrate in the porous medium: the porous medium sample which completely absorbs the gas in the step S2 is adopted, and the environment temperature is reduced to be the gas hydrate generation experimental temperature T Raw materials Generating gas hydrate by a constant pressure method, and controlling the pressure of a reaction cavity to be constant at experimental pressure P Kettle 0 ＝P Kettle life Control of pressure data P of a pressure-covering chamber Cover 0 ＞P Kettle 0 Wherein the pressure P of the gas storage tank is ensured before the hydrate is generated Store 0 >P Kettle 0 After the gas hydrate in the porous medium sample is completely generated, the gas variation n of the gas storage tank is obtained by calculating in the formula 1 in the step S2 i I.e. the gas consumption n of the porous medium sample to generate hydrate Raw materials ；
S4, decomposing the hydrate in the porous medium: by constant pressure heat shockOr decomposing gas hydrate by a constant pressure depressurization method; constant pressure heat shock method, setting experimental environment temperature T i Is T Dividing into Hydrate in the gas hydrate-containing porous medium sample is decomposed, and the pressure of the reaction cavity is controlled to be constant to be experimental pressure P Kettle 0 ＝P Kettle life Controlling the pressure P of the pressure-covering cavity Cover 0 ＞P Kettle 0 Wherein the pressure P of the gas storage tank is ensured before the hydrate is decomposed Store 0 <P Kettle 0 After the gas hydrate in the porous medium sample is completely decomposed, the gas variation n of the gas storage tank can be obtained by calculating in the formula 1 in the step S2 i I.e. the gas yield n of decomposing the hydrate in the porous medium sample Dividing into The method comprises the steps of carrying out a first treatment on the surface of the Constant pressure depressurization method for maintaining experimental environment temperature T i Is T Raw materials Reducing the pressure P of the reaction chamber Kettle i The control valve is controlled to release free gas to the gas storage tank to ensure the pressure P of the gas storage tank Store 0 <P Kettle 0 When the pressure of the reaction cavity is constant P Kettle 0 ＝P Kettle separator When the gas change amount n of the gas storage tank is obtained by calculating the formula 1 in the step S2 i I.e. the free gas amount n released by the hydrate in the sample of the porous medium by pressure reduction and decomposition Self-supporting Hydrate starts to decompose, and the pressure of the reaction cavity is controlled to be constant to be experimental pressure P Kettle 0 ＝P Kettle separator Controlling the pressure P of the pressure-covering cavity Cover 0 ＞P Kettle 0 The gas hydrate in the porous medium sample is completely decomposed, and the gas variation n of the gas storage tank is obtained by calculating in the step S2 in the formula 1 i I.e. the gas yield n of decomposing the hydrate in the porous medium sample Dividing into 。
2. The method for measuring the change of the expansion characteristics of a porous medium containing hydrate according to claim 1, wherein the pressure in the blanket pressure chamber is set to be larger than the pressure P in the reaction chamber Cover 0 ＝P Kettle 0 The porous medium sample in the reaction cavity is compacted by the covering pressure at +0.1Mpa, the bearing capacity of the porous medium sample and the pressure in the reaction cavity are balanced with the pressure in the covering pressure cavity, and when the pressure in the reaction cavity and the pressure in the covering pressure cavity are controlled to be constant, the soft piston between the covering pressure cavity and the reaction cavity is not moved; then according to the bearing capacity change of the porous medium sample, the pressure-covering cavity and the reverseThe soft piston in the middle of the stress cavity moves, the volume in the pressure-covering cavity changes, the liquid quantity in the pressure-covering cavity changes, and the pressure-covering control unit liquid flowmeter records the liquid inlet or outlet M i Simultaneously, according to the stress induction film on the inner wall of the reaction cavity of the reaction kettle, measuring the radial expansion stress of the porous medium sample, and according to the adsorbed liquid amount n Liquid and its preparation method Adsorbed gas amount n Air flow Hydrate forming gas consumption n of porous media sample Raw materials Gas production n of decomposing hydrate in porous Medium sample Dividing into And combining the measured axial expansion amount and radial expansion stress of the porous medium to obtain the expansion characteristic change of the porous medium containing the hydrate under different experimental conditions.
3. The method for measuring changes in expansion characteristics of a porous medium containing hydrate according to claim 1, wherein the reaction chamber pressure P Kettle i Collected by a data control unit through a pressure sensor and according to the collected P Kettle i Data for controlling the on-off of the control valve of the gas supply unit and stably controlling the pressure in the reaction chamber to be P Kettle 0 The method comprises the following specific steps:
when P Kettle i <P Kettle 0 When the control valve is opened, gas in the gas storage tank is injected into the reaction cavity through the control valve, and the pressure P in the reaction cavity Kettle i ＝P Kettle 0 Closing the control valve;
when P Kettle i >P Kettle 0 When the control valve is opened, the gas in the reaction cavity is discharged into the gas storage tank through the control valve, and the pressure P in the reaction cavity Kettle i ＝P Kettle 0 Closing the control valve;
pressure data P of the pressure-coated chamber Covering i By a set of data control units via pressure sensors and according to the collected P Covering i Data, controlling the switch of the axial pump of the pressure covering unit, and stabilizing the pressure P of the pressure covering cavity Cover 0 The method comprises the following specific steps:
when P Covering i <P Cover 0 The axial pressure pump is started, and the liquid in the liquid cavity of the axial pressure pump is injected into the pressure covering cavity until the pressure P of the pressure covering cavity Covering i ＝P Cover 0 Closing the axial pressure pump;
when P Covering i >P Cover 0 The axial pressure pump is started, and the liquid in the pressure coating cavity is withdrawn to the liquid cavity of the axial pressure pump until the pressure P in the pressure coating cavity Covering i ＝P Cover 0 The axial pressure pump is turned off.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103513019A (en) * | 2013-09-22 | 2014-01-15 | 西南石油大学 | Gas channeling simulated evaluation instrument for casing cement slurry |
| CN105259003A (en) * | 2015-11-25 | 2016-01-20 | 中国科学院广州能源研究所 | Experiment device and method for synthesizing marine natural gas hydrate sample |
| CN105699247A (en) * | 2016-03-04 | 2016-06-22 | 西南石油大学 | Experimental method for synthesizing and decomposing natural gas hydrate and experiment system |
-
2022
- 2022-02-21 CN CN202210155072.8A patent/CN114577667B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103513019A (en) * | 2013-09-22 | 2014-01-15 | 西南石油大学 | Gas channeling simulated evaluation instrument for casing cement slurry |
| CN105259003A (en) * | 2015-11-25 | 2016-01-20 | 中国科学院广州能源研究所 | Experiment device and method for synthesizing marine natural gas hydrate sample |
| CN105699247A (en) * | 2016-03-04 | 2016-06-22 | 西南石油大学 | Experimental method for synthesizing and decomposing natural gas hydrate and experiment system |
Non-Patent Citations (2)
| Title |
|---|
| 天然气水合物三维成藏物模实验系统的构建与检验;粟科华 等;天然气工业;第33卷(第12期);P173-178 * |
| 水合物降压分解的实验及数值模拟;冯自平 等;化工学报;第58卷(第06期);P1548-1553 * |
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