CN112611675B - High-temperature high-pressure natural gas solubility test reaction kettle, device and method - Google Patents

High-temperature high-pressure natural gas solubility test reaction kettle, device and method Download PDF

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CN112611675B
CN112611675B CN202011456442.9A CN202011456442A CN112611675B CN 112611675 B CN112611675 B CN 112611675B CN 202011456442 A CN202011456442 A CN 202011456442A CN 112611675 B CN112611675 B CN 112611675B
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gas
pressure
liquid
cavity
reaction kettle
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CN112611675A (en
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梁豪
吴木旺
郭书生
姜洪丰
廖高龙
崔书姮
吴土荣
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CNOOC China Ltd Hainan Branch
Engineering Technology Branch of CNOOC Energy Technology and Services Ltd
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CNOOC China Ltd Hainan Branch
Engineering Technology Branch of CNOOC Energy Technology and Services Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N7/00Analysing materials by measuring the pressure or volume of a gas or vapour
    • G01N7/14Analysing materials by measuring the pressure or volume of a gas or vapour by allowing the material to emit a gas or vapour, e.g. water vapour, and measuring a pressure or volume difference
    • G01N7/16Analysing materials by measuring the pressure or volume of a gas or vapour by allowing the material to emit a gas or vapour, e.g. water vapour, and measuring a pressure or volume difference by heating the material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/002Component parts of these vessels not mentioned in B01J3/004, B01J3/006, B01J3/02 - B01J3/08; Measures taken in conjunction with the process to be carried out, e.g. safety measures
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/03Pressure vessels, or vacuum vessels, having closure members or seals specially adapted therefor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J3/00Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
    • B01J3/04Pressure vessels, e.g. autoclaves
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/22Fuels; Explosives
    • G01N33/225Gaseous fuels, e.g. natural gas

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  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
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  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

The invention discloses a high-temperature high-pressure natural gas solubility test reaction kettle, a device and a method, wherein the reaction kettle comprises a kettle body and a heating device, a dissolution reaction cavity and a gas pressurizing cavity are arranged in the kettle body, a pressurizing cavity I and a pressurizing cavity II are arranged in the gas pressurizing cavity, a buffer cavity is arranged in the pressurizing cavity I, and a high-pressure sealing piston is arranged in the pressurizing cavity II to divide the pressurizing cavity into a first pressurizing cavity II and a second pressurizing cavity II; the dissolution reaction cavity is provided with a gas sampling port, a temperature sensor, a pressure sensor and a liquid inlet and outlet; the first pressurizing cavity is provided with an air source inlet, a first check valve is arranged in the air source inlet and connected with the buffer cavity, the buffer cavity is connected with the dissolution reaction cavity through a first air outlet pipe, and a second check valve is arranged on the first air outlet pipe; the buffer cavity is connected with a first pressurizing cavity II through an air outlet pipe II, isolation liquid is arranged in the second pressurizing cavity II, and a pressure-bearing liquid inlet is formed in the second pressurizing cavity II. The method can accurately measure the solubility of the natural gas at high temperature and high pressure.

Description

High-temperature high-pressure natural gas solubility test reaction kettle, device and method
Technical Field
The invention relates to the technical field of natural gas solubility test, in particular to a reaction kettle, a device and a method for testing natural gas solubility under high-temperature and high-pressure conditions.
Background
Natural gas solubility is one of the key parameters in reservoir reserves evaluation. At present, the research on the solubility of the natural gas at home and abroad is mainly focused on the condition of medium and low pressure, but the research on the solubility of the natural gas under the condition of high temperature and high pressure (the pressure is 100MPa and the temperature is 200 ℃) is very little, and the main reasons include that (1) the common equipment is difficult to reach the pressure above 100 MPa; (2) The problem of tightness of gas under high temperature condition is difficult to solve; (3) gas is difficult to take a gas sample under the conditions of high temperature and high pressure; (4) The accuracy of data is easily affected by pressure fluctuation generated during sampling under high-temperature and high-pressure conditions; (5) As the temperature and pressure change, the solubilities of the mixed gases interact and the larger changes also result in larger errors in the measurement. In practical hydrocarbon reservoirs, high-temperature and high-pressure hydrocarbon reservoirs are commonly available, so a device and a method for testing the solubility of high-temperature and high-pressure natural gas are needed.
Disclosure of Invention
Aiming at the problems, the invention aims to provide a high-temperature high-pressure natural gas solubility test reaction kettle, a high-temperature high-pressure natural gas solubility test device and a high-temperature high-pressure natural gas solubility test method, which can realize stable high-temperature high-pressure conditions, ensure stable pressure during sampling in a test process, improve test safety and provide a certain reference for development of an actual oil and gas reservoir.
The technical scheme of the invention is as follows:
on the one hand, a high-temperature and high-pressure natural gas solubility test reaction kettle is provided, and comprises a kettle body and a heating device connected with the kettle body, wherein a first partition board is arranged in the kettle body to divide the internal part of the kettle body into a dissolution reaction cavity and a gas pressurizing cavity;
the top of the dissolution reaction cavity is provided with a gas sampling port, the dissolution reaction cavity is internally provided with a temperature sensor and a pressure sensor, and the bottom of the dissolution reaction cavity is provided with a liquid inlet and outlet;
the first gas pressurizing cavity is provided with a gas source inlet, a first check valve is arranged in the gas source inlet, the outlet end of the gas source inlet is connected with the gas caching cavity, the gas caching cavity is connected with the dissolution reaction cavity through a first gas outlet pipe, and a second check valve is arranged on the first gas outlet pipe; the gas cache cavity is connected with the first gas pressurizing cavity through a second gas outlet pipe, isolation liquid is arranged in the second gas pressurizing cavity, and the second gas pressurizing cavity is provided with a pressure-bearing liquid inlet.
Preferably, the kettle body is of a double-layer hollow structure, the heating device adopts liquid circulation heating, and the hollow layer of the kettle body is a liquid circulation heating layer.
Preferably, the first check valve is arranged at the outlet end of the air source inlet, and the second check valve is arranged at the outlet end of the first air outlet pipe; a first pressure isolating plate is arranged between the first check valve and the gas buffer cavity, and a second pressure isolating plate is arranged between the second check valve and the dissolution reaction cavity.
Preferably, the second air outlet pipe is a coil pipe; and/or a stirrer is arranged in the dissolution reaction cavity.
Preferably, one end of the high-pressure sealing piston, which is close to the second gas pressurizing cavity, is in a plane shape, and one end of the high-pressure sealing piston, which is close to the second gas pressurizing cavity, is in a V-shaped section.
On the other hand, a high-temperature and high-pressure natural gas solubility testing device is provided, which comprises the reaction kettle, a liquid inlet system, an air inlet system, a pressurizing system, a gas collecting system and a liquid collecting system which are respectively connected with the reaction kettle, a measuring system which is respectively connected with the gas collecting system and the liquid collecting system, and a control valve on a connecting pipeline;
the liquid inlet system comprises a liquid storage tank, the liquid storage tank is connected with a liquid injection pump, and the outlet end of the liquid injection pump is connected with a liquid inlet and outlet of the reaction kettle;
the air inlet system comprises an air source storage tank which is connected with an air source inlet of the reaction kettle;
the pressurizing system comprises a pressure-bearing liquid storage tank, the pressure-bearing liquid storage tank is connected with a pressure-bearing liquid high-pressure pump, and a control valve arranged on a pipeline which is connected with an outlet end of the pressure-bearing liquid high-pressure pump and a pressure-bearing liquid inlet of the reaction kettle is a one-way valve;
the gas production system comprises a free gas cooler, wherein the input end of the free gas cooler is connected with a gas sampling port of the reaction kettle, and a pressure relief pipe is arranged on a connected pipeline;
the liquid collecting system comprises a liquid condenser, the input end of the liquid condenser is connected with a liquid inlet and a liquid outlet of the reaction kettle, the output end of the liquid condenser is connected with a gas-liquid shunt, and a temperature-pressure integrated sensor is arranged on the gas-liquid shunt;
the measuring system comprises a gas chromatograph I, a gas chromatograph II and a liquid meter, wherein the gas chromatograph I is connected with the output end of the free gas cooler, and the gas chromatograph II and the liquid meter are respectively connected with the gas-liquid shunt.
Preferably, the air inlet system further comprises a gas circulation buffer tank, the input end of the gas circulation buffer tank is connected with the gas sampling port of the reaction kettle, the output end of the gas circulation buffer tank is connected with a gas circulation pump, and the outlet end of the gas circulation pump is connected with the gas source inlet of the reaction kettle.
Preferably, a drain pipe is further arranged on a pipeline between the reaction kettle and the liquid condenser.
Preferably, the automatic control cabinet is connected with the temperature sensor, the pressure-bearing liquid high-pressure pump and the heating device of the reaction kettle respectively.
On the other hand, the method for testing the natural gas solubility under the high-temperature and high-pressure condition is provided, and the device for testing the natural gas solubility under the high-temperature and high-pressure condition is adopted for testing, and comprises the following steps:
checking the air tightness of the test device;
pumping the stratum into the reaction kettle through the liquid inlet system, and opening a heating device of the reaction kettle for heating;
injecting natural gas into the reaction kettle through an air inlet system, and pressurizing through a pressurizing system to enable the pressure in the dissolution reaction cavity to reach a pressure set value;
after the temperature monitored by the temperature sensor reaches the set temperature, stabilizing for 3-4 hours;
the liquid volume V after gas-liquid split is obtained by a liquid meter L Calculating the volume V of dissolved and precipitated gas by the reading of the temperature and pressure integrated sensor g Analyzing the components and the contents of the dissolved and separated gas by a chromatographic analyzer;
and analyzing the components and the content of the free gas sample by a chromatographic analyzer.
The beneficial effects of the invention are as follows:
the method can accurately measure the solubility of the natural gas mixture under the conditions of high temperature and high pressure, wherein the reaction kettle adopts the pressure-bearing liquid, the isolating liquid and the high-pressure sealing piston to seal the gas, thereby ensuring the sealing performance and solving the problem of experimental failure caused by the sealing of the gas under the conditions of high temperature and high pressure; the stability and the unidirectionality of pressure transmission and the pressure stability of sampling are ensured through the pressure isolating plate and the one-way valve; an automatic control system is adopted to ensure the safety and environmental protection of the whole experimental process; and the solubility of the natural gas can be calculated through the acquired data.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions of the prior art, the drawings which are used in the description of the embodiments or the prior art will be briefly described, it being obvious that the drawings in the description below are only some embodiments of the invention, and that other drawings can be obtained according to these drawings without inventive faculty for a person skilled in the art.
FIG. 1 is a schematic structural diagram of a high-temperature high-pressure natural gas solubility test reaction kettle;
FIG. 2 is a schematic structural diagram of the natural gas solubility testing device with high temperature and high pressure in the invention.
Reference numerals in the drawings:
101-kettle body, 102-baffle I, 103-dissolution reaction chamber, 104-baffle II, 105-gas pressurizing chamber I, 106-gas pressurizing chamber II, 107-gas buffer chamber, 108-high-pressure sealing piston, 109-gas sampling port, 110-temperature sensor, 111-pressure sensor, 112-liquid inlet and outlet, 113-gas source inlet, 114-one-way valve I, 115-gas outlet pipe I, 116-one-way valve II, 117-gas pipe II, 118-spacer fluid, 119-pressure bearing fluid inlet, 120-liquid circulation heating layer, 121-circulation inlet, 122-circulation outlet, 123-spacer plate I, 124-spacer plate II and 125-stirrer.
1-reaction kettle, 2-liquid storage tank, 3-liquid injection pump, 4-air source storage tank, 5-pressure-bearing liquid high-pressure pump, 6-free gas cooler, 7-pressure relief pipe, 8-liquid condenser, 9-gas-liquid shunt, 10-temperature-pressure integrated sensor, 11-gas chromatograph I, 12-gas chromatograph II, 13-gas circulation buffer tank, 14-gas circulation pump, 15-bleeder pipe, 16-automatic control cabinet, 17-heat circulation pump.
Detailed Description
The invention will be further described with reference to the drawings and examples.
It should be noted that, without conflict, the embodiments and technical features of the embodiments in the present application may be combined with each other.
It is noted that all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs unless otherwise indicated.
In the present invention, the terms "first," "second," and the like, when used in the context of a description, are used for distinguishing between similar objects and not necessarily for describing a particular sequential or chronological order. It is to be understood that the terminology so used; the terms "upper", "lower", "left", "right" and the like are used generally with respect to the orientation shown in the drawings or with respect to the component itself in a vertical, vertical or gravitational orientation; also, for ease of understanding and description, "inner", "outer", and the like refer to inner and outer relative to the contours of the components themselves. The above directional terms are not intended to limit the present invention.
As shown in fig. 1, the invention provides a high-temperature and high-pressure natural gas solubility test reaction kettle, which comprises a kettle body 101 and a heating device (not shown in the figure) connected with the kettle body 101, wherein a first partition plate 102 is arranged in the kettle body 101 to divide the interior of the kettle body 101 into a dissolution reaction cavity 103 and a gas pressurizing cavity, a second partition plate 104 is arranged in the gas pressurizing cavity to divide the gas pressurizing cavity into a first gas pressurizing cavity 105 and a second gas pressurizing cavity 106, a gas buffer cavity 107 is arranged in the first gas pressurizing cavity 105, a high-pressure sealing piston 108 is arranged in the second gas pressurizing cavity 106, and the second gas pressurizing cavity 106 is divided into a first gas pressurizing cavity and a second gas pressurizing cavity by the high-pressure sealing piston 108;
the top of the dissolution reaction chamber 103 is provided with a gas sampling port 109, the dissolution reaction chamber 103 is internally provided with a temperature sensor 110 and a pressure sensor 111, and the bottom of the dissolution reaction chamber 103 is provided with a liquid inlet and outlet 112;
the first gas pressurizing cavity 105 is provided with a gas source inlet 113, a first check valve 114 is arranged in the gas source inlet 113, the outlet end of the gas source inlet 113 is connected with the gas caching cavity 107, the gas caching cavity 107 is connected with the dissolution reaction cavity 103 through a first gas outlet pipe 115, and a second check valve 116 is arranged on the first gas outlet pipe 115; the gas buffer cavity 107 is connected with the first gas pressurizing cavity through a second gas outlet pipe 117, a spacer fluid 118 is arranged in the second gas pressurizing cavity, and a pressure-bearing fluid inlet 119 is arranged in the second gas pressurizing cavity.
In the above embodiment, multistage liquid pressure-bearing sealing is adopted, optionally, the isolating liquid adopts high-density hydrophobic isolating liquid, so that the sealing performance can be ensured, the property of the projection solution is not influenced, the pressure-bearing liquid is pumped through a pressure-bearing liquid high-pressure pump, the pressure can be rapidly transferred to the isolating liquid, and the sealing performance and the safety of the reaction kettle can be effectively ensured by adopting hydraulic pressurization. It should be noted that the first gas pressurizing cavity and the second gas pressurizing cavity may be arranged in different spatial arrangements, such as up-down, down-up, left-right, etc. The layout shown in fig. 1 is only a preferred embodiment, but not limiting.
In order to improve the thermal stability of the reaction kettle, optionally, the kettle body 101 is of a double-layer hollow structure, the heating device adopts liquid circulation heating, and the hollow layer of the kettle body 101 is a liquid circulation heating layer 120. Optionally, a circulation inlet 121 of the heating liquid is arranged at the lower part of the reaction kettle, a circulation outlet 122 of the heating liquid is arranged at the upper part of the reaction kettle, and the circulation inlet 121 and the circulation outlet 122 are connected with the output end and the input end of the thermal circulation pump through pipelines. In practice, the heating liquid enters the liquid circulation heating layer 120 of the reaction kettle from the circulation inlet 121, flows out of the reaction kettle from the circulation outlet 122, enters the thermostat for further heating and then circulates.
In a specific embodiment, the first check valve 114 is disposed at an outlet end of the air source inlet 113, and the second check valve 116 is disposed at an outlet end of the first air outlet pipe 115; a first pressure-isolating plate 123 is disposed between the first check valve 114 and the gas buffer chamber 107, and a second pressure-isolating plate 124 is disposed between the second check valve 116 and the dissolution reaction chamber 103. The pressure in the reaction kettle can be stabilized and overflow of the pressure can be prevented through the one-way valve 114 and the pressure-isolating plate 123, so that gas can circulate in liquid; the second check valve 116 and the second pressure isolating plate 124 prevent the high-pressure liquid from overflowing or flowing back, so that the pressure in the reaction kettle is more stable. The first pressure isolating plate 123 and the second pressure isolating plate 124 are made of low-permeability materials so as to achieve the purpose of pressure isolation, thus the countercurrent influence caused by high-pressure liquid overflow can be reduced, and the arrangement of the one-way valve can directly prevent the countercurrent of the high-pressure liquid, so that the high pressure in the reaction kettle can be stabilized under the balance condition. Optionally, the hypotonic material is nano-scale micro-pore material, and the pressure-isolating capability of the materials with different pores is different.
In a specific embodiment, the second outlet tube 117 is a coil. The coil pipe can increase the path of natural gas, so that the natural gas can reach the purpose of pressurization more quickly.
In order to make the gas-liquid system in the reaction kettle reach heat balance quickly, an agitator 125 is optionally disposed in the dissolution reaction chamber 103. Alternatively, the stirrer 125 may be an electromagnetic stirrer, and the electromagnetic stirrer may be disposed at the bottom of the dissolution reaction chamber 103. In addition to the electromagnetic stirrer used in the present embodiment, other stirrers in the prior art may be used.
In a specific embodiment, an end of the high-pressure sealing piston 108 near the second gas pressurizing cavity is planar, and a cross section of an end of the high-pressure sealing piston 108 near the second gas pressurizing cavity is V-shaped.
As shown in fig. 2, the invention also provides a high-temperature and high-pressure natural gas solubility testing device, which comprises the reaction kettle 1, a liquid inlet system, an air inlet system, a pressurizing system, a gas collecting system and a liquid collecting system which are respectively connected with the reaction kettle 1, a measuring system respectively connected with the gas collecting system and the liquid collecting system, and a control valve on a connecting pipeline;
the liquid inlet system comprises a liquid storage tank 2, wherein the liquid storage tank 2 is connected with a liquid injection pump 3, and the outlet end of the liquid injection pump 3 is connected with a liquid inlet and outlet 112 of the reaction kettle 1;
the air inlet system comprises an air source storage tank 4, and the air source storage tank 4 is connected with an air source inlet 113 of the reaction kettle 1;
the pressurizing system comprises a pressure-bearing liquid storage tank (not shown in the figure), the pressure-bearing liquid storage tank is connected with a pressure-bearing liquid high-pressure pump 5, the outlet end of the pressure-bearing liquid high-pressure pump 5 is connected with a pressure-bearing liquid inlet 119 of the reaction kettle 1, and a control valve arranged on a connected pipeline is a one-way valve;
the gas production system comprises a free gas cooler 6, wherein the input end of the free gas cooler 6 is connected with a gas sampling port 109 of the reaction kettle 1, and a pressure release pipe 7 is arranged on a connected pipeline;
the liquid collecting system comprises a liquid condenser 8, wherein the input end of the liquid condenser 8 is connected with a liquid inlet and outlet 112 of the reaction kettle 1, the output end of the liquid condenser 8 is connected with a gas-liquid diverter 9, and a temperature-pressure integrated sensor 10 is arranged on the gas-liquid diverter 9; it should be noted that, a separate temperature sensor and pressure sensor may be provided on the gas-liquid diverter 9;
the measuring system comprises a first gas chromatograph 11, a second gas chromatograph 12 and a liquid meter (not shown in the figure), wherein the first gas chromatograph 11 is connected with the output end of the free gas cooler 6, and the second gas chromatograph 12 and the liquid meter are respectively connected with the gas-liquid shunt 9. It should be noted that, the liquid meter may be a liquid meter in the prior art, or a scale may be arranged on the gas-liquid diverter to directly measure the volume of the liquid.
In a specific embodiment, if the amount of gas source is limited, the solubility test may be performed in a self-cycling manner. Specifically, the air inlet system further comprises a gas circulation buffer tank 13, the input end of the gas circulation buffer tank 13 is connected with a gas sampling port 109 of the reaction kettle 1, the output end of the gas circulation buffer tank 13 is connected with a gas circulation pump 14, and the output end of the gas circulation pump 14 is connected with an air source inlet 113 of the reaction kettle 1.
In a specific embodiment, a drain pipe 15 is further disposed on a pipeline between the reaction kettle 1 and the liquid condenser 8.
In order to improve the automation control degree of the invention, the testing device optionally further comprises an automatic control cabinet 16, and the automatic control cabinet 16 is respectively connected with the temperature sensor 110, the pressure sensor 111, the pressure-bearing liquid high-pressure pump 5 and the heating device of the reaction kettle 1.
In addition, the invention also provides a method for testing the solubility of the natural gas under high temperature and high pressure, which comprises the following steps: checking the air tightness of the test device; pumping stratum water into the reaction kettle 1 through a liquid inlet system, and opening a heating device of the reaction kettle 1 for heating; natural gas is injected into the reaction kettle 1 through an air inlet system, and is pressurized through a pressurizing system, so that the pressure in the dissolution reaction cavity 103 reaches a pressure set value; after the temperature monitored by the temperature sensor 110 reaches the set temperature, stabilizing for 3-4 hours; the liquid volume V after gas-liquid split is obtained by a liquid meter L The volume V of the dissolved and precipitated gas is calculated by the reading of the temperature and pressure integrated sensor 10 g Analyzing the components and the content of the dissolved and precipitated gas by a chromatographic analyzer II 12; the composition and content of the free gas sample were analyzed by a chromatographic analyzer 11.
When the natural gas solubility test under high temperature and high pressure conditions is performed using the specific embodiment shown in fig. 2, the method comprises the following steps:
1. sample preparation: the desired formation water is prepared and then filtered for impurities to prevent clogging of capillaries, which are then stored in the liquid storage tank 2 for use. And placing the prepared gas sample in a gas source storage tank 4, and connecting a pipeline for standby.
2. And (3) air tightness test: and (3) performing polar air tightness test on the reaction kettle 1, the valve, the pipeline and the like until the whole test device is free from leakage.
3. The valves A-E, G and I-J are opened through the automatic control cabinet 16, and after the liquid in the liquid storage tank 2 is pumped into the reaction kettle 1 through the liquid injection pump 3, the valves A-E, G and I-J are closed.
4. The thermal circulation pump 17 and the valves U-V are opened to start heating, the valve F and the pressure-bearing liquid high-pressure pump 5 are opened to start boosting the pressure of the reaction kettle 1.
5. The stirrer 125 automatically stirs by inputting the temperature T and the pressure P to be controlled through the control panel of the automatic control cabinet 16. And after the temperature rises to the set value, the system is continuously stabilized for 3-4 hours.
6. Sampling: the valve D-E and the valve P-Q are opened by the automatic control cabinet 16, and the liquid volume V of the gas-liquid split flow is obtained by the liquid meter L Closing the valves D-E and P-Q, and calculating the volume V of the dissolved and separated gas by the reading of the temperature and pressure integrated sensor 10 g And opening a valve R to analyze the components and the content of the dissolved and separated gas through a chromatographic analysis instrument.
7. Taking a free gas sample: after the temperature and the pressure are stable, the valve G, the valve I, the valve W and the valve X are slowly opened, gas enters the gas chromatograph I11 through the free gas cooler 6, and the components and the content of the free gas sample are analyzed through the gas chromatograph I11.
8. If the gas source is limited, a self-circulation mode can be adopted, the valve G and the valve H are opened, the gas at the outlet is pumped into the reaction kettle 1 again by the gas circulation pump 14 until the equilibrium condition is reached, and the analysis is carried out again.
The present invention is not limited to the above-mentioned embodiments, but is intended to be limited to the following embodiments, and any modifications, equivalents and modifications can be made to the above-mentioned embodiments without departing from the scope of the invention.

Claims (10)

1. The high-temperature high-pressure natural gas solubility test reaction kettle is characterized by comprising a kettle body and a heating device connected with the kettle body, wherein a first partition plate is arranged in the kettle body to divide the internal part of the kettle body into a dissolution reaction cavity and a gas pressurizing cavity;
the top of the dissolution reaction cavity is provided with a gas sampling port, the dissolution reaction cavity is internally provided with a temperature sensor and a pressure sensor, and the bottom of the dissolution reaction cavity is provided with a liquid inlet and outlet;
the first gas pressurizing cavity is provided with a gas source inlet, a first check valve is arranged in the gas source inlet, the outlet end of the gas source inlet is connected with the gas caching cavity, the gas caching cavity is connected with the dissolution reaction cavity through a first gas outlet pipe, and a second check valve is arranged on the first gas outlet pipe; the gas cache cavity is connected with the first gas pressurizing cavity through a second gas outlet pipe, isolation liquid is arranged in the second gas pressurizing cavity, and the second gas pressurizing cavity is provided with a pressure-bearing liquid inlet.
2. The high-temperature and high-pressure natural gas solubility test reaction kettle according to claim 1, wherein the kettle body is of a double-layer hollow structure, the heating device adopts liquid circulation heating, and the hollow layer of the kettle body is a liquid circulation heating layer.
3. The high-temperature and high-pressure natural gas solubility test reaction kettle according to claim 1, wherein the first check valve is arranged at the outlet end of the air source inlet, and the second check valve is arranged at the outlet end of the air outlet pipe; a first pressure isolating plate is arranged between the first check valve and the gas buffer cavity, and a second pressure isolating plate is arranged between the second check valve and the dissolution reaction cavity.
4. The high-temperature and high-pressure natural gas solubility test reaction kettle according to claim 1, wherein the second air outlet pipe is a coil; and/or a stirrer is arranged in the dissolution reaction cavity.
5. The high-temperature and high-pressure natural gas solubility test reaction kettle according to any one of claims 1-4, wherein one end of the high-pressure sealing piston, which is close to the second gas pressurizing cavity, is in a plane shape, and one end of the high-pressure sealing piston, which is close to the second gas pressurizing cavity, is in a V-shaped cross section.
6. A high-temperature high-pressure natural gas solubility testing device, which is characterized by comprising the reaction kettle as claimed in any one of claims 1-5, a liquid inlet system, an air inlet system, a pressurizing system, a gas collecting system and a liquid collecting system which are respectively connected with the reaction kettle, a measuring system respectively connected with the gas collecting system and the liquid collecting system, and a control valve on a connecting pipeline;
the liquid inlet system comprises a liquid storage tank, the liquid storage tank is connected with a liquid injection pump, and the outlet end of the liquid injection pump is connected with a liquid inlet and outlet of the reaction kettle;
the air inlet system comprises an air source storage tank which is connected with an air source inlet of the reaction kettle;
the pressurizing system comprises a pressure-bearing liquid storage tank, the pressure-bearing liquid storage tank is connected with a pressure-bearing liquid high-pressure pump, and a control valve arranged on a pipeline which is connected with an outlet end of the pressure-bearing liquid high-pressure pump and a pressure-bearing liquid inlet of the reaction kettle is a one-way valve;
the gas production system comprises a free gas cooler, wherein the input end of the free gas cooler is connected with a gas sampling port of the reaction kettle, and a pressure relief pipe is arranged on a connected pipeline;
the liquid collecting system comprises a liquid condenser, the input end of the liquid condenser is connected with a liquid inlet and a liquid outlet of the reaction kettle, the output end of the liquid condenser is connected with a gas-liquid shunt, and a temperature-pressure integrated sensor is arranged on the gas-liquid shunt;
the measuring system comprises a gas chromatograph I, a gas chromatograph II and a liquid meter, wherein the gas chromatograph I is connected with the output end of the free gas cooler, and the gas chromatograph II and the liquid meter are respectively connected with the gas-liquid shunt.
7. The high-temperature and high-pressure natural gas solubility testing device according to claim 6, wherein the air inlet system further comprises a gas circulation buffer tank, the input end of the gas circulation buffer tank is connected with the gas sampling port of the reaction kettle, the output end of the gas circulation buffer tank is connected with a gas circulation pump, and the output end of the gas circulation pump is connected with the gas source inlet of the reaction kettle.
8. The high temperature and high pressure natural gas solubility test device according to claim 6, wherein a drain pipe is further arranged on a pipeline between the reaction kettle and the liquid condenser.
9. The high-temperature and high-pressure natural gas solubility test device according to any one of claims 6 to 8, further comprising an automatic control cabinet, wherein the automatic control cabinet is respectively connected with a temperature sensor, a pressure-bearing liquid high-pressure pump and a heating device of the reaction kettle.
10. A method for testing the solubility of natural gas under high temperature and high pressure conditions, which is characterized by adopting the device for testing the solubility of natural gas under high temperature and high pressure conditions as claimed in any one of claims 6 to 9, and comprising the following steps:
checking the air tightness of the test device;
pumping the stratum into the reaction kettle through the liquid inlet system, and opening a heating device of the reaction kettle for heating;
injecting natural gas into the reaction kettle through an air inlet system, and pressurizing through a pressurizing system to enable the pressure in the dissolution reaction cavity to reach a pressure set value;
after the temperature monitored by the temperature sensor reaches the set temperature, stabilizing for 3-4 hours;
the liquid volume V after gas-liquid split is obtained by a liquid meter L Calculating the volume V of dissolved and precipitated gas by the reading of the temperature and pressure integrated sensor g Analyzing the components and the contents of the dissolved and separated gas by a chromatographic analyzer;
and analyzing the components and the content of the free gas sample by a chromatographic analyzer.
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CN113533600B (en) * 2021-08-09 2022-02-22 江苏鑫华半导体材料科技有限公司 Trichlorosilane detection pretreatment method and trichlorosilane detection method
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Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4627273A (en) * 1985-08-28 1986-12-09 Marathon Oil Company Apparatus and method for determining the minimum miscibility pressure of a gas in a liquid
JPH10227781A (en) * 1996-12-13 1998-08-25 Asahi Breweries Ltd Measuring device for methane formation activity
JP2004117140A (en) * 2002-09-26 2004-04-15 National Maritime Research Institute Density measuring method of liquefied gas-dissolving water
CN101055276A (en) * 2007-02-14 2007-10-17 中国科学院广州能源研究所 Natural gas hydrate phase balance emulation experiment device
CN104088611A (en) * 2014-06-20 2014-10-08 华南理工大学 Pressure vessel for CO2 displacement and pressure reduction combined mining of hydrates
CN104775809A (en) * 2015-02-07 2015-07-15 中国石油大学(华东) Simulation experiment system and method of water soluble gas reservoir development
WO2017113947A1 (en) * 2015-12-29 2017-07-06 中国科学院广州能源研究所 Natural gas hydrate density measuring device
CN106969957A (en) * 2017-04-20 2017-07-21 天津大学 A kind of Multifunctional, air gas hydrate experimental system
CN206906203U (en) * 2017-05-17 2018-01-19 西南石油大学 A kind of high-temperature high-pressure reaction kettle device for overcritical sour gas Water-rock interaction
CN207951385U (en) * 2018-01-28 2018-10-12 青岛凤翔新材料有限责任公司 A kind of reaction kettle compensator
CN111579424A (en) * 2020-06-03 2020-08-25 大连理工大学 Device and method for measuring gas solubility in natural gas hydrate solution system
CN111729612A (en) * 2020-07-07 2020-10-02 西南石油大学 Piston pressure adjusting device and gas distribution method for intermediate gas concentration of high-temperature high-pressure kettle

Patent Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4627273A (en) * 1985-08-28 1986-12-09 Marathon Oil Company Apparatus and method for determining the minimum miscibility pressure of a gas in a liquid
JPH10227781A (en) * 1996-12-13 1998-08-25 Asahi Breweries Ltd Measuring device for methane formation activity
JP2004117140A (en) * 2002-09-26 2004-04-15 National Maritime Research Institute Density measuring method of liquefied gas-dissolving water
CN101055276A (en) * 2007-02-14 2007-10-17 中国科学院广州能源研究所 Natural gas hydrate phase balance emulation experiment device
CN104088611A (en) * 2014-06-20 2014-10-08 华南理工大学 Pressure vessel for CO2 displacement and pressure reduction combined mining of hydrates
CN104775809A (en) * 2015-02-07 2015-07-15 中国石油大学(华东) Simulation experiment system and method of water soluble gas reservoir development
WO2017113947A1 (en) * 2015-12-29 2017-07-06 中国科学院广州能源研究所 Natural gas hydrate density measuring device
CN106969957A (en) * 2017-04-20 2017-07-21 天津大学 A kind of Multifunctional, air gas hydrate experimental system
CN206906203U (en) * 2017-05-17 2018-01-19 西南石油大学 A kind of high-temperature high-pressure reaction kettle device for overcritical sour gas Water-rock interaction
CN207951385U (en) * 2018-01-28 2018-10-12 青岛凤翔新材料有限责任公司 A kind of reaction kettle compensator
CN111579424A (en) * 2020-06-03 2020-08-25 大连理工大学 Device and method for measuring gas solubility in natural gas hydrate solution system
CN111729612A (en) * 2020-07-07 2020-10-02 西南石油大学 Piston pressure adjusting device and gas distribution method for intermediate gas concentration of high-temperature high-pressure kettle

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
北京石油勘探开发科学研究院.我国已知油气区天然气藏类型、形成条件、富集规律及勘探规划研究.1990,第84页-第86页. *
郝石生.天然气运聚动平衡及其应用.北京:石油工业出版社,1994,第30页-第32页. *

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