CN113667507B - Device for supercritical water and oxygen collaborative pyrolysis of L-shaped columnar organic rock and use method - Google Patents
Device for supercritical water and oxygen collaborative pyrolysis of L-shaped columnar organic rock and use method Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
- C10G1/002—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal in combination with oil conversion- or refining processes
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- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
- C10G1/008—Controlling or regulating of liquefaction processes
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Abstract
The invention relates to a device for supercritical water and oxygen collaborative pyrolysis of L-shaped columnar organic rock and a using method thereof, belonging to the technical field of deep unconventional or conventional resource special exploitation; the technical scheme comprises a parallel L-shaped reaction kettle, a supercritical water generating system, an axial pressure transmission rod, a pore pressure applying system, an oxygen injection system, a drainage (salt) system and an oil-gas condensation and collection system; the reaction device can fully simulate the process of fracturing a fractured reservoir by supercritical water in-situ pyrolysis, explores the mechanism and the reaction characteristics of the supercritical water and oxygen in cooperation with pyrolysis of the columnar fractured organic rock, can ensure that the pyrolysis environment of the fractured rock is the supercritical environment, can heat in sections, can realize the supercritical water-oxygen pyrolysis reaction of the organic rock in different areas, can realize the real-time high-efficiency separation of oil, gas and water, injects oxygen into a sample after pyrolysis through the oxygen injection system, and ensures that the oxygen slowly flows in the horizontal section to fully react with the organic rock, thereby greatly reducing the explosion risk.
Description
Technical Field
The invention belongs to the technical field of deep unconventional or conventional resource special exploitation, and particularly relates to a supercritical water and oxygen collaborative pyrolysis device for L-shaped columnar organic rock and a using method thereof.
Background
China is rich in organic rock (coal, oil shale, etc.) reserves. The national condition of China is that the oil is poor and the gas is little, and the organic rock is pyrolyzed to form an oil gas product, which has important significance for relieving the current situation of oil shortage in China. The resource reserves of different burial depths are different, and for ore beds with shallow burial depths of 500m, the mining can be carried out by well construction or in-situ mining, high-temperature fluid (550 ℃) is directly injected into a heat injection well in the in-situ mining, and after the organic matter is fully pyrolyzed, the fluid product can be discharged and mined from a production well. However, for a deeply buried ore bed, the difficulty of underground mining is very high, and the potential safety hazard problem is serious, while in-situ mining has very serious heat dissipation because high-temperature fluid is transmitted in a long-distance shaft, and a scheme of injecting normal-pressure or low-pressure high-temperature fluid is not feasible. The supercritical water has the advantages of both liquid and gas, has good mass transfer and heat transfer properties, and is often used as an excellent reaction medium due to the characteristics, the supercritical water is called as the supercritical water when the water is in a high-temperature and high-pressure state with critical points (374.3 ℃ and 22.05 MPa), the rock covering stress on a deep-buried mineral layer is very high, a high-pressure fluid environment is created, the critical temperature (374.3 ℃) is far lower than the fluid temperature (550 ℃) required by pyrolysis of a shallow-buried mineral layer, and the influence of the heat dissipation of a shaft on the effective pyrolysis of the mineral layer is very small, so that the supercritical water in-situ pyrolysis deep-buried mineral layer is a particularly feasible scheme.
The patent in this field has CN 112299546A, CN 112680246A etc. now, but current supercritical water reation kettle all is cylindrical thick wall tubular structure, and single structure, its major defect is as follows:
1. stress loading cannot be carried out on a sample, and supercritical water pyrolysis reaction under the original rock stress condition cannot be realized;
2. graded heating cannot be realized;
3. oil, gas and water are completely mixed and cannot be synchronously separated in real time;
4. after oxygen is input into the reactor, the oxygen rapidly and vertically rises to be mixed with pyrolysis gas generated at the top of the cylindrical reaction reactor, so that explosion risk is generated.
Disclosure of Invention
The invention overcomes the defects of the prior art, provides a device for the supercritical water and oxygen collaborative pyrolysis of L-shaped columnar organic rock and a using method thereof, and solves the problems that the supercritical water and oxygen reaction device of the organic rock cannot be loaded, cannot be heated in a grading manner, is easy to explode and the like at present.
In order to achieve the above object, the present invention is achieved by the following technical solutions.
The device for supercritical water and oxygen collaborative pyrolysis of the L-shaped columnar organic rock comprises an L-shaped parallel connection reaction kettle, a supercritical water generation system, an axial pressure transmission rod, a pore pressure application system, an oxygen injection system, a water (salt) drainage system and an oil-gas condensation and collection system;
the parallel L-shaped reaction kettle comprises a straight barrel reaction kettle and an L-shaped reaction kettle, a gasket is arranged at the parallel position of the straight barrel reaction kettle and the L-shaped reaction kettle, the area of the straight barrel reaction kettle is a supercritical water oxygen reaction area, a snap ring is arranged at the position, close to the gasket, inside the straight barrel reaction kettle, a porous plate is arranged on the snap ring, a fourth thermocouple, a fifth thermocouple and a sixth thermocouple are connected on the kettle body of the straight barrel reaction kettle, and a heat preservation layer is wrapped on the outer surface of the kettle body,
the axial pressure transmission rod is arranged in the straight-barrel reaction kettle and connected through a first flange, a groove is formed in one end, arranged in the straight-barrel reaction kettle, of the axial pressure transmission rod, a supercritical water-oxygen reaction area is formed by an area between the groove and the porous plate, a pyrolysis sample is filled in the supercritical water-oxygen reaction area, a packing is arranged between the pyrolysis sample and the straight-barrel reaction kettle, a high-temperature oil-water area is formed in an area between the porous plate and the transverse edge kettle body side of the L-shaped reaction kettle, and a low-temperature gas area is formed on the longitudinal edge kettle body side of the L-shaped reaction kettle;
the bottom of the kettle body of the L-shaped reaction kettle in the high-temperature oil-water area is provided with a water (salt) drainage hole and is connected with the water (salt) drainage system, a second thermocouple and a pressure sensor are arranged at the position, close to the perforated plate, of the straight-barrel reaction kettle, and the water (salt) drainage system comprises a second back pressure valve, a second heat exchanger and a water tank;
a supercritical water injection cavity is formed in one side of the axial transmission rod and connected with the supercritical water generation system, an air inlet cavity is formed in the other side of the axial transmission rod and connected with the oxygen injection system, and a water circulation cooling cavity is formed in the axial transmission rod; the supercritical water generation system comprises a water pump, a first one-way valve, a supercritical water generator and a third one-way valve, and is used for injecting water into the pyrolysis sample through the supercritical water injection cavity when the pyrolysis sample is in water shortage; the oxygen injection system comprises an oxygen cylinder and a second one-way valve and is used for injecting oxygen into the pyrolysis sample through the air inlet cavity after the pyrolysis sample starts to generate oil gas products;
a hole is arranged on the L-shaped reaction kettle at the same level with the axis of the straight-barrel reaction kettle and is connected with the pore pressure applying system, a liquid level meter is arranged above the connection position of the pore pressure applying system and the L-shaped reaction kettle, the bottom of the liquid level meter is flush with the corner of the L-shaped reaction kettle, a third thermocouple is arranged at the middle upper part of the L-shaped reaction kettle, a second flange is arranged at the top end of the L-shaped reaction kettle, the second flange is provided with a safety valve, the oil gas condensing and collecting system comprises an air water condensing and collecting device and an oil water condensing and collecting device, the gas-water condensation collecting device comprises a first back pressure valve, a first heat exchanger and a gas-water separation device, the oil-water condensation and collection device comprises a third back pressure valve, a third heat exchanger and an oil groove, a hole is arranged on the second flange, the oil-water condensation and collection device is arranged at the lower part of the kettle body of the L-shaped reaction kettle in the low-temperature gas area; the device comprises a low-temperature gas zone, a low-temperature gas zone and a low-temperature gas zone, wherein a kettle body of the L-shaped reaction kettle in the low-temperature gas zone is provided with a multistage water circulation cooling cavity, and a pore pressure applying system comprises a nitrogen gas cylinder, a pressure gauge and a fourth one-way valve and is used for injecting pore pressure into the L-shaped reaction kettle in a forward and parallel connection manner in a pyrolysis test.
Furthermore, a snap ring is welded in the straight-barrel reaction kettle at a position close to the gasket.
Furthermore, the length of the supercritical water-oxygen reaction zone is 200 mm-500 mm, and the supercritical water-oxygen reaction zone is divided into a zone I, a zone II and a zone III for heating in sections, wherein in the pyrolysis process, the zone I has the highest temperature and is firstly used as a pyrolysis zone, and the zone II and the zone III are used as preheating zones; after oxygen injection, the I area is used as an oxidation heat release area, the II area is used as a pyrolysis area, and the III area is used as a preheating area; and after pyrolysis in the area II is finished, the area II is used as an oxidation heat release area, and the area III is used as a pyrolysis area.
Furthermore, the pyrolysis sample is a columnar organic rock containing cracks, and the outer diameter of the columnar organic rock is smaller than the inner diameter of the kettle body of the straight-tube reaction kettle.
Further, the void pressure is greater than 22.05 MPa.
Furthermore, a horizontal pipeline of the third back pressure valve connected with the kettle body of the L-shaped reaction kettle is higher than the bottom end position of the liquid level meter.
Compared with the prior art, the invention has the beneficial effects that.
According to the invention, the reaction device for supercritical water and oxygen collaborative pyrolysis of the L-shaped columnar organic rock can be designed to fully simulate the process of supercritical water in-situ pyrolysis fracturing of a fractured reservoir, and the mechanism and reaction characteristics of supercritical water and oxygen collaborative pyrolysis of the columnar fractured organic rock are explored, so that a theoretical basis is provided for field practice. Has the following advantages:
1. the pyrolysis environment of the fractured rock can be ensured to be a supercritical environment;
2. the device can be heated in sections, and can realize supercritical water-oxygen pyrolysis reaction of organic rocks in different areas;
3. oxygen is injected into the pyrolyzed sample through an oxygen injection system, a supercritical water reaction area is horizontally placed, and the oxygen slowly flows in a horizontal section, so that the oxygen is ensured to fully react with organic rocks, and the explosion risk is greatly reduced;
4. oil, gas and water can be efficiently separated in real time.
Drawings
The invention is further described below with reference to the accompanying drawings:
FIG. 1 is a schematic view of the structure of a reaction apparatus according to the present invention;
FIG. 2 is a schematic view of a partitioned schematic structure of a reaction apparatus according to the present invention;
FIG. 3 is an elevation view of the axial pressure transfer rod;
FIG. 4 is a side view of the axial pressure rod;
in the figure: 1-a water pump; 2-a first one-way valve; 3-axial pressure transmission rod; 4, a gasket; 5-a second one-way valve; 6-oxygen cylinder; 7-water circulation cooling cavity; 8-a first flange; 9-packing; 10-insulating layer; 11-a second thermocouple; 12-a pressure sensor; 13-supercritical water generator; 14-a snap ring; 15-a perforated plate; 16-third thermocouple; 17-a safety valve; 18-a first heat exchanger; 19-gas-water separation device; 20-a liquid level meter; 21 — a second flange; 22-a second heat exchanger; 23-a water tank; 24-a fourth thermocouple; 25-fifth thermocouple; 26-sixth thermocouple; 27-supercritical water injection cavity; 28-an air inlet cavity; 29 — first back pressure valve; 30-second back pressure valve; 31-pyrolyzing the sample; 32-a valve; 33-a third one-way valve; 34-a straight-barrel reaction kettle; 35-L type reaction kettle; 36-a fourth one-way valve; 37-pressure gauge; 38-nitrogen gas cylinder; 39-a groove; 40-third backpressure valve; 41-third heat exchanger; 42-oil sump; 43-multistage water circulation cooling cavity; 44-supercritical water oxygen reaction zone; 45-high temperature oil-water area; 46-low temperature gas zone; 47-gas-water interface; 48-region I; region 49-II; 50-III.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail with reference to the embodiments and the accompanying drawings. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. The technical solution of the present invention is described in detail below with reference to the embodiments and the drawings, but the scope of protection is not limited thereto.
The device for the supercritical water and oxygen collaborative pyrolysis of the L-shaped columnar organic rock comprises an L-shaped reaction kettle, a supercritical water generating system, an axial pressure transmission rod 3, a pore pressure applying system, an oxygen injection system, a water (salt) drainage system and an oil-gas condensation and collection system which are connected in parallel;
the parallel L-shaped reaction kettle comprises a straight barrel reaction kettle 34 and an L-shaped reaction kettle 35 which are arranged in parallel, a gasket 4 is arranged at the parallel position of the straight barrel reaction kettle 34, the area of the straight barrel reaction kettle 34 is a supercritical water oxygen reaction area 44, a clamping ring 14 is arranged at the position, close to the gasket 4, inside the straight barrel reaction kettle 34, a porous plate 15 is arranged on the clamping ring 14, a fourth thermocouple 24, a fifth thermocouple 25 and a sixth thermocouple 26 are connected on the kettle body of the straight barrel reaction kettle 34, and the outer surface of the straight barrel reaction kettle is wrapped by a heat insulation layer 10,
the axial pressure transmission rod 3 is arranged in the straight-barrel reaction kettle 34 and connected with the straight-barrel reaction kettle through a first flange 8, a groove 39 is arranged at one end of the axial pressure transmission rod 3 arranged in the straight-barrel reaction kettle 34, a supercritical water oxygen reaction area 44 is formed in the area between the groove 39 and the porous plate 15, a pyrolysis sample 31 is filled in the supercritical water oxygen reaction area 44, a packing 9 is arranged between the pyrolysis sample 31 and the straight-barrel reaction kettle 34, a high-temperature oil-water area 45 is arranged in the area between the porous plate 15 and the transverse side kettle body side of the L-shaped reaction kettle 35, and a low-temperature gas area 46 is arranged on the longitudinal side of the L-shaped reaction kettle 35;
a drain (salt) hole is formed in the bottom of the kettle body of the L-shaped reaction kettle 35 of the high-temperature oil-water area 45 and is connected with a drain (salt) system, a second thermocouple 11 and a pressure sensor 12 are arranged at the position, close to the porous plate 15, of the straight-barrel reaction kettle 34, and the drain (salt) system comprises a second back pressure valve 30, a valve 32, a second heat exchanger 22 and a water tank 23;
one side of the axial transmission rod is provided with a supercritical water injection cavity 27 and is connected with a supercritical water generation system, the other side of the axial transmission rod is provided with an air inlet cavity 28 and is connected with an oxygen injection system, and the axial transmission rod 3 is provided with a water circulation cooling cavity 7; the supercritical water generation system comprises a water pump 1, a first one-way valve 2, a supercritical water generator 13 and a third one-way valve 33, and is used for injecting water into the pyrolysis sample 31 through the supercritical water injection cavity 27 when the pyrolysis sample 31 is in water shortage; the oxygen injection system comprises an oxygen cylinder 6 and a second one-way valve 5, and is used for injecting oxygen into the pyrolysis sample 31 through the air inlet cavity 28 after the pyrolysis sample 31 starts to generate oil gas products;
a hole is arranged on the L-shaped reaction kettle 35 at the same level with the axis of the straight-barrel reaction kettle 34 and is connected with a pore pressure applying system, a liquid level meter 20 is arranged above the connecting position of the pore pressure applying system and the L-shaped reaction kettle 35, the bottom of the liquid level meter 20 is flush with the corner position of the L-shaped reaction kettle 35, a third thermocouple 16 is arranged at the middle upper part of the L-shaped reaction kettle 35, a second flange 21 is arranged at the top end of the L-shaped reaction kettle, a safety valve 17 is arranged on the second flange 21, the oil-gas condensation and collection system comprises an air-water condensation collection device and an oil-water condensation collection device, the air-water condensation collection device comprises a first back pressure valve 29, a first heat exchanger 18 and an air-water separation device 19, the oil-water condensation collection device comprises a third back pressure valve 40, a third heat exchanger 41 and an oil groove 42, holes are arranged on the second flange 21, and is communicated with a gas-water condensation collecting device which is arranged at the lower part of the L-shaped reaction kettle 35 of the low-temperature gas area 46; the multistage water circulation cooling cavity 437 is arranged on the kettle body of the L-shaped reaction kettle 35 of the low-temperature gas zone 46, and the pore pressure applying system comprises a nitrogen gas bottle 38, a pressure gauge 37 and a fourth one-way valve 36, and is used for injecting pore pressure into the parallel connection L-shaped reaction kettle 35 before the pyrolysis test is carried out.
Furthermore, a snap ring 14 is welded inside the straight-tube reaction kettle 34 at a position close to the gasket 4.
Furthermore, the length of the supercritical water-oxygen reaction zone 44 is 200 mm-500 mm, and the supercritical water-oxygen reaction zone is divided into a zone I48, a zone II 4948 and a zone III 504948 for heating in a segmented manner, wherein in the pyrolysis process, the zone I48 is at the highest temperature and is firstly used as a pyrolysis zone, and the zone II 4948 and the zone III 504948 are used as preheating zones; after oxygen injection, the I area 48 is used as an oxidation heat release area, the II area 4948 is used as a pyrolysis area, and the III area 504948 is used as a preheating area; zone II 4948 serves as the oxidative exothermic zone after pyrolysis is complete, and zone III 504948 serves as the pyrolysis zone.
Further, the pyrolysis sample 31 is a columnar organic rock containing cracks, and the outer diameter is smaller than the inner diameter of the kettle body of the straight-tube reaction kettle 34.
Further, the void pressure is greater than 22.05 MPa.
Further, a horizontal pipeline of the third back pressure valve 40 connected with the kettle body of the L-shaped reaction kettle 35 is higher than the bottom end position of the liquid level meter 20.
Example 1
When the buried depth of the ore bed is 900m and the heat injection temperature is 400 ℃, the reaction device comprises the following specific operation steps:
1. placing a porous plate 15 on a snap ring 14 of a straight-barrel reaction kettle 34, filling and placing columnar crack-containing organic rock, and simultaneously tightly filling a high-temperature-resistant packing 9 in a gap between a pyrolysis sample 31 and the straight-barrel reaction kettle 34;
2. fixing a high-temperature high-pressure first flange 8, extruding a packing (9) through a groove 39 at the bottom of the axial transmission rod 3, and applying 23.4MPa pressure to the blocky sample;
3. connecting a straight barrel reaction kettle 34, an L-shaped reaction kettle 35, a drainage (salt) system and an oil gas condensation and collection system, setting the pressure of a first backpressure valve 29, a second backpressure valve 30 and a third backpressure valve 33 which are resistant to high temperature to be 23.4MPa, and setting the pressure of a safety valve 17 to be 30 MPa;
4. injecting pore pressure of 23.4MPa into the high-temperature high-pressure parallel reaction kettle through a pore pressure applying system;
5. the outer layer of the straight-barrel reaction kettle 34 is wrapped with the heat-insulating layer 10, and is connected with the supercritical water generation system and the oxygen injection system, and circulating water is introduced into the water circulation cooling cavity 7 and the multi-stage water circulation cooling cavity 43;
6. preparing supercritical water with the pressure of 23.4MPa and the temperature of 400 ℃ by a supercritical water generator 13, injecting the supercritical water into a pyrolysis sample 31, observing whether a gas product is produced at the outlet of a gas-water separation device 19 in the sample heating process, stopping injecting the supercritical water after a period of time when the gas product is continuously produced, fully utilizing the return water in an L-shaped reaction kettle 35 to supplement moisture to the sample, injecting oxygen into the sample by an oxygen injection system, so that the oxygen reacts with pyrolysis residual carbon in a supercritical water oxygen reaction area I to release heat, serving as a heat source for sample pyrolysis in an area II, monitoring the temperature changes of a second thermocouple 11, a third thermocouple 16, a fourth thermocouple 24, a fifth thermocouple 25 and a sixth thermocouple 26, and reasonably reducing the preparation temperature of the supercritical water generator according to the temperature changes;
7. alternately carrying out supercritical water injection work and oxygen injection work, collecting oil and water through an oil-water condensation collecting device when a steam-water interface is in a visible range, placing the collected oil and water in an oil groove 42, and injecting supercritical water into the sample 31 when the steam-water interface is too low, so that the steam-water interface is always kept at an observable section of the liquid level meter 20;
8. when the gas cannot be extracted from the outlet of the gas-water separation device 19 and the gas-water interface of the liquid level meter 20 has no oil layer, the test is stopped, the high-temperature and high-pressure resistant valve 32 is opened, and sewage and salt are discharged. And when the temperature of the parallel high-temperature and high-pressure reaction kettles is reduced to room temperature, splitting the straight-tube reaction kettle 34 and the L-shaped reaction kettle 35, taking out the pyrolysis sample 31, and completing the test.
Example 2
When the burial depth of the ore bed is 1200m and the heat injection temperature is 380 ℃, the reaction device provided by the invention comprises the following specific operation steps:
1. a perforated plate 15 is placed on a snap ring 14 of the straight-barrel reaction kettle 34, a columnar crack-containing organic rock 31 is placed on the perforated plate 15, and a high-temperature-resistant packing is filled in a gap between the pyrolysis sample 31 and the straight-barrel reaction kettle 34;
2. fixing a high-temperature high-pressure first flange 8, extruding a disk root 9 through a groove 39 at the bottom of an axial pressure transmission rod 3, and applying a pressure of 30MPa to a blocky sample;
3. connecting a straight barrel reaction kettle 34, an L-shaped reaction kettle 35, a drainage (salt) system and an oil gas condensation and collection system, setting the pressure of a first backpressure valve 29, a second backpressure valve 30 and a third backpressure valve 33 which are resistant to high temperature to be 30MPa, and setting the pressure of a safety valve 17 to be 35 MPa;
4. injecting pore pressure of 30MPa into the parallel high-temperature high-pressure reaction kettle through a pore pressure applying system;
5. the outer layer of the straight-barrel reaction kettle 34 is wrapped with the heat-insulating layer 10, and is connected with the supercritical water generation system and the oxygen injection system, and circulating water is introduced into the water circulation cooling cavity 7 and the multi-stage water circulation cooling cavity 43;
6. preparing supercritical water with the pressure of 30MPa and the temperature of 380 ℃ by a supercritical water generator 13, injecting the supercritical water into a pyrolysis sample 31, observing whether a gas product is produced at the outlet of a gas-water separation device 19 in the sample heating process, stopping injecting the supercritical water after a period of time when the gas product is continuously produced, fully utilizing the return water in an L-shaped reaction kettle 35 to supplement moisture to the sample, injecting oxygen into the sample by an oxygen injection system, so that the oxygen reacts with pyrolysis residual carbon in an I area of a supercritical water oxygen reaction area to release heat, serving as a heat source for sample pyrolysis in an II area, monitoring the temperature changes of a second thermocouple 11, a third thermocouple 16, a fourth thermocouple 24, a fifth thermocouple 25 and a sixth thermocouple 26, and reasonably reducing the preparation temperature of the supercritical water generator according to the temperature changes;
7. alternately carrying out supercritical water injection work and oxygen injection work, collecting oil and water through an oil-water condensation collecting device when a steam-water interface is in a visible range, placing the collected oil and water in an oil groove 42, and injecting supercritical water into the sample 31 when the steam-water interface is too low, so that the steam-water interface is always kept at an observable section of the liquid level meter 20;
8. when the gas cannot be extracted from the outlet of the gas-water separation device 19 and the gas-water interface of the liquid level meter 20 has no oil layer, the test is stopped, the high-temperature and high-pressure resistant valve 32 is opened, and sewage and salt are discharged. And when the temperature of the parallel high-temperature high-pressure reaction kettle is reduced to room temperature, splitting the straight-tube reaction kettle 34 and the L-shaped reaction kettle 35, taking out the pyrolysis sample 31, and finishing the test.
The device can realize the grading reaction of supercritical water, is used for simulating the process and the characteristics of in-situ efficient pyrolysis and fracturing of supercritical water and simultaneously exploiting oil and gas in real time, is suitable for the environment with the mineral bed burial depth of more than 882m, the heat injection temperature needs to be more than 374.3 ℃, and in the specific operation, the parameter values of pressure, temperature and the like at each part in the reaction device are adaptively adjusted according to the mine depth and the heat injection temperature, wherein the set pressure of the first back pressure valve 29, the second back pressure valve 30 and the third back pressure valve 33 is higher than 22.05 MPa.
While the invention has been described in further detail with reference to specific preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (7)
- The device is characterized by comprising a parallel L-shaped reaction kettle, a supercritical water generating system, an axial pressure transmission rod, a pore pressure applying system, an oxygen injection system, a water and salt discharging system and an oil and gas condensing and collecting system;the parallel connection L-shaped reaction kettle comprises a straight-barrel reaction kettle and an L-shaped reaction kettle, a gasket is arranged at the parallel connection position of the straight-barrel reaction kettle and the L-shaped reaction kettle, the area of the straight-barrel reaction kettle is a supercritical water oxygen reaction area, the supercritical water oxygen reaction area is divided into an area I, an area II and an area III for heating in a sectional mode, the temperature of the area I is highest in the pyrolysis process, the area I is firstly used as a pyrolysis area, and the area II and the area III are used as preheating areas; after oxygen injection, the I area is used as an oxidation heat release area, the II area is used as a pyrolysis area, and the III area is used as a preheating area; after pyrolysis in the area II is finished, the area II is used as an oxidation heat release area, and the area III is used as a pyrolysis area; a snap ring is arranged at a position close to the gasket inside the straight-barrel reaction kettle, a perforated plate is arranged on the snap ring, a fourth thermocouple, a fifth thermocouple and a sixth thermocouple are connected on the kettle body of the straight-barrel reaction kettle, and the outer surface of the straight-barrel reaction kettle is wrapped with a heat insulation layer,the axial pressure transmission rod is arranged in the straight-barrel reaction kettle and is connected with the straight-barrel reaction kettle through a first flange, a groove is arranged at one end of the axial pressure transmission rod arranged in the straight-barrel reaction kettle, a supercritical water-oxygen reaction area is formed by the groove and the area between the groove and the porous plate, a pyrolysis sample is filled in the supercritical water-oxygen reaction area, a packing is arranged between the pyrolysis sample and the straight-barrel reaction kettle, a high-temperature oil-water area is arranged in the area between the porous plate and the transverse edge kettle body side of the L-shaped reaction kettle, and a low-temperature gas area is arranged on the longitudinal edge kettle body side of the L-shaped reaction kettle;the bottom of the kettle body of the L-shaped reaction kettle in the high-temperature oil-water area is provided with a water and salt discharging hole and is connected with the water and salt discharging system, a second thermocouple and a pressure sensor are arranged at the position, close to the porous plate, of the straight barrel reaction kettle, and the water and salt discharging system comprises a second back pressure valve, a second heat exchanger and a water tank;one side of the axial pressure transmission rod is provided with a supercritical water injection cavity and is connected with the supercritical water generation system, the other side of the axial pressure transmission rod is provided with an air inlet cavity and is connected with the oxygen injection system, and the axial pressure transmission rod is provided with a water circulation cooling cavity; the supercritical water generation system comprises a water pump, a first one-way valve, a supercritical water generator and a third one-way valve, and is used for injecting water into the pyrolysis sample through the supercritical water injection cavity when the pyrolysis sample is in water shortage; the oxygen injection system comprises an oxygen cylinder and a second one-way valve and is used for injecting oxygen into the pyrolysis sample through the air inlet cavity after the pyrolysis sample starts to generate oil gas products;a hole is arranged on the L-shaped reaction kettle at the same level with the axis of the straight-barrel reaction kettle and is connected with the pore pressure applying system, a liquid level meter is arranged above the connecting position of the pore pressure applying system and the L-shaped reaction kettle, the bottom of the liquid level meter is flush with the corner of the L-shaped reaction kettle, a third thermocouple is arranged at the middle upper part of the L-shaped reaction kettle, a second flange is arranged at the top end of the L-shaped reaction kettle, the second flange is provided with a safety valve, the oil gas condensing and collecting system comprises an air water condensing and collecting device and an oil water condensing and collecting device, the gas-water condensation collecting device comprises a first backpressure valve, a first heat exchanger and a gas-water separating device, the oil-water condensation and collection device comprises a third back pressure valve, a third heat exchanger and an oil groove, a hole is arranged on the second flange, the oil-water condensation and collection device is arranged at the lower part of the kettle body of the L-shaped reaction kettle in the low-temperature gas area; the device comprises a low-temperature gas zone, a low-temperature gas zone and a low-temperature gas zone, wherein a kettle body of the L-shaped reaction kettle in the low-temperature gas zone is provided with a multistage water circulation cooling cavity, and a pore pressure applying system comprises a nitrogen gas cylinder, a pressure gauge and a fourth one-way valve and is used for injecting pore pressure into the L-shaped reaction kettle in a forward and parallel connection manner in a pyrolysis test.
- 2. The device for supercritical water and oxygen collaborative pyrolysis of L-shaped columnar organic rock according to claim 1, wherein a snap ring is welded inside the straight-barrel reaction kettle at a position close to the gasket.
- 3. The device for supercritical water and oxygen collaborative pyrolysis of L-shaped columnar organic rock according to claim 1, wherein the length of the supercritical water-oxygen reaction zone is 200 mm-500 mm.
- 4. The apparatus for supercritical water and oxygen collaborative pyrolysis of L-shaped columnar organic rock according to claim 1, wherein the pyrolysis sample is a crack-containing columnar organic rock with an outer diameter smaller than the inner diameter of the reactor body of the straight-tube reaction kettle.
- 5. The apparatus for supercritical water and oxygen collaborative pyrolysis of L-type columnar organic rock of claim 1, wherein the pore pressure is greater than 22.05 MPa.
- 6. The device for supercritical water and oxygen collaborative pyrolysis of L-shaped columnar organic rock according to claim 1, wherein a horizontal pipeline connecting the third back pressure valve with the kettle body of the L-shaped reaction kettle is higher than the bottom end position of the liquid level meter.
- 7. The use method of the device according to any one of claims 1 to 6, characterized by comprising the following steps:(1) placing a perforated plate on a clamping ring of the straight-barrel reaction kettle, filling a pyrolysis sample, and tightly filling a packing in a gap between the pyrolysis sample and the straight-barrel reaction kettle;(2) fixing a first flange, extruding a packing through a groove at the bottom of the axial pressure transmission rod, and applying pressure to a sample;(3) connecting the straight-tube reaction kettle, the L-shaped reaction kettle, the water and salt discharging system and the oil-gas condensation and collection system, and setting the pressure of a first backpressure valve, a second backpressure valve and a third backpressure valve which are resistant to high temperature and the pressure of a safety valve;(4) injecting pore pressure into the high-temperature high-pressure parallel reaction kettle through a pore pressure applying system;(5) the outer layer of the straight-barrel reaction kettle is wrapped with a heat-insulating layer, and is simultaneously connected with a supercritical water generation system and an oxygen injection system, and circulating water is introduced into a water circulation cooling cavity and a multi-stage water circulation cooling cavity;(6) preparing supercritical water through a supercritical water generator, injecting the supercritical water into a pyrolysis sample, observing whether a gas product is produced at an outlet of a gas-water separation device or not in the sample heating process, stopping injecting the supercritical water after a period of time when the gas product is continuously produced, fully utilizing return water in an L-shaped reaction kettle to supplement moisture to the sample, injecting oxygen into the sample through an oxygen injection system, monitoring the temperature changes of a second thermocouple, a third thermocouple, a fourth thermocouple, a fifth thermocouple and a sixth thermocouple, and reasonably reducing the preparation temperature of the supercritical water generator according to the temperature changes;(7) alternately carrying out supercritical water injection work and oxygen injection work, collecting oil and water through an oil-water condensation collection device when a steam-water interface is in a visible range, and injecting supercritical water into a sample when the steam-water interface is too low;(8) stopping the test when the gas cannot be extracted from the outlet of the gas-water separation device and the gas-water interface of the liquid level meter has no oil layer, opening a valve, and discharging sewage and salt;(9) and when the temperature of the parallel L-shaped reaction kettle is reduced to the room temperature, splitting the straight-tube reaction kettle and the L-shaped reaction kettle, taking out the pyrolysis sample, and finishing the test.
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