CN107831297B - High-temperature high-pressure crude oil cracking gas-forming simulation experiment device and method - Google Patents
High-temperature high-pressure crude oil cracking gas-forming simulation experiment device and method Download PDFInfo
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- 239000010779 crude oil Substances 0.000 title claims abstract description 76
- 238000005336 cracking Methods 0.000 title claims abstract description 39
- 238000004088 simulation Methods 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 25
- 229910052751 metal Inorganic materials 0.000 claims abstract description 30
- 239000002184 metal Substances 0.000 claims abstract description 30
- 239000011148 porous material Substances 0.000 claims abstract description 24
- 239000003921 oil Substances 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 17
- 238000010521 absorption reaction Methods 0.000 claims abstract description 11
- 238000005245 sintering Methods 0.000 claims abstract description 8
- 238000000197 pyrolysis Methods 0.000 claims abstract description 6
- 238000003466 welding Methods 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims description 131
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 60
- 238000003860 storage Methods 0.000 claims description 32
- 238000010438 heat treatment Methods 0.000 claims description 24
- 238000004140 cleaning Methods 0.000 claims description 12
- 238000011068 loading method Methods 0.000 claims description 11
- 238000002474 experimental method Methods 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 6
- 239000003153 chemical reaction reagent Substances 0.000 claims description 5
- 230000000149 penetrating effect Effects 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 239000011358 absorbing material Substances 0.000 abstract description 5
- 239000007789 gas Substances 0.000 description 52
- 230000003075 superhydrophobic effect Effects 0.000 description 7
- 229910001220 stainless steel Inorganic materials 0.000 description 6
- 239000010935 stainless steel Substances 0.000 description 6
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 5
- 239000010931 gold Substances 0.000 description 5
- 229910052737 gold Inorganic materials 0.000 description 5
- 238000010146 3D printing Methods 0.000 description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 3
- 239000000839 emulsion Substances 0.000 description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 229960001701 chloroform Drugs 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 229920002689 polyvinyl acetate Polymers 0.000 description 2
- 239000011118 polyvinyl acetate Substances 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- -1 cracking Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
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- 239000002270 dispersing agent Substances 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- HFQQZARZPUDIFP-UHFFFAOYSA-M sodium;2-dodecylbenzenesulfonate Chemical compound [Na+].CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O HFQQZARZPUDIFP-UHFFFAOYSA-M 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000002569 water oil cream Substances 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/26—Oils; Viscous liquids; Paints; Inks
- G01N33/28—Oils, i.e. hydrocarbon liquids
- G01N33/2823—Raw oil, drilling fluid or polyphasic mixtures
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a high-temperature high-pressure crude oil pyrolysis gas simulation experiment device and a high-temperature high-pressure crude oil pyrolysis gas simulation experiment method. The oil absorbing material layer is at least provided with one layer. The oil absorption material layer is made of a metal porous material with lipophilicity, and the metal porous material is arranged on the inner wall of the inner cavity of the kettle body through a sintering or welding method. The invention is used for simulating the high-temperature cracking gas-forming process of crude oil under the condition of underground pressure, can prevent crude oil in the autoclave from flowing out during gas taking, can continuously crack the same crude oil sample into gas, and can simulate the crude oil cracking gas-forming process under the condition of underground semi-closed-semi-open.
Description
Technical Field
The invention relates to a petroleum geology simulation experiment device, in particular to a simulation experiment device and a method for cracking high-temperature and high-pressure crude oil into gas.
Background
The cracking of crude oil into gas is an important cause of underground natural gas, and the cracking simulation experiment under the high-temperature and high-pressure conditions in a laboratory is an important means for researching the cracking mechanism of crude oil into gas and guiding the exploration of crude oil cracking gas. At present, the main working mode of the simulation experiment device is as follows: crude oil is placed in an autoclave, or the crude oil is sealed in a gold tube and then the gold tube is placed in the autoclave, and an outlet valve is closed. The crude oil or the gold tube is pressurized by fluid (water, helium, etc.) medium, and after one experiment is finished, the outlet valve of the autoclave is opened to collect the generated gas or the generated gas is taken out and the gold tube is punctured to collect the gas. When a valve is opened or a gold tube is punctured to collect gas, crude oil flows out due to the rapid release of pressure, so that a quantitative cracking experiment with higher evolution degree cannot be performed by using the sample; in addition, the system is closed throughout the heating simulation reaction, and cannot simulate semi-closed-semi-open conditions under underground conditions. The simulation experiment device is designed for solving the problems.
The metal porous material and sintering technology are all the prior art.
Application number: 201610894797.3, publication No. 2017-05-10 discloses a metal porous material and a preparation method thereof, wherein the preparation method comprises the following steps: (1) Uniformly mixing titanium powder and boron powder, and printing the mixed metal powder into a material with a required shape at 2800-3200 ℃ by utilizing a 3D printing metal laser sintering technology; (2) Heating the material with the specific shape in the step (1) to 2500-2700 ℃ to liquefy boron and titanium which are not fully reacted, and flowing out of the material with the specific shape to obtain the metal porous material with the required shape. The invention adopts the 3D printing laser metal sintering technology to directly print the shape of the part without secondary processing; the modeling of the shape of the processed part is easier, and the flexibility is stronger; the 3D printing device family provides the energy required for the two powder chemical reactions. And setting proper 3D printing processing parameters, and printing and forming the boron powder and the titanium powder to obtain the metal porous material with higher hardness and melting point and pore size of 3-100 mu m.
Feng is described in 2004 in article "a Super-hydrophobic and Super-oleophilic coating mesh film for the separation of oil and water" (journal name "angel. Chem. Int. Ed.") as follows: PTFE emulsion was sprayed onto stainless steel mesh and treated in a dry oven at 350℃for about 30 minutes, the film surface exhibiting superhydrophobic/superoleophilic properties.
Feng equals 2004 also in: "A superhydrophobic and superoleophilic coating mesh film for the separation of oil and water" (journal name: "Angewandte Chemie International Edition") mentions: PTFE, adhesive polyvinyl acetate (PVAc), dispersing agent polyvinyl alcohol (PVA), surfactant sodium dodecyl sulfate (SDBS) and water are stirred to form mixed emulsion, and then the emulsion is sprayed on a stainless steel net and subjected to high-temperature treatment to form a coarse low-surface-energy PTFE coating with a micro-nano structure. The prepared stainless steel mesh has the characteristics of super-hydrophobicity and super-lipophilicity.
LEE was equal to 2011, and the article "The performance of superhydrophobic and superoleophilic Carbon nano tube meshes in water-oil filtration" (journal name: "Carbon") describes that the treated porous Carbon nanotubes are grown on a stainless steel mesh by chemical vapor deposition method to prepare a stainless steel mesh membrane material with super-hydrophobic-super-oleophilic properties for separation of oil-water emulsion.
WANG is equal to 2012 in the article "Ultraviolet-durable superhydrophobic zinc oxide-coated mesh films for surface and underwater-oil capture and transportation" (publication name: "Langmuir") which mentions that it adopts a hydrothermal method to form a ZnO microstructure coating on the surface of a stainless steel mesh, and that it has stable superhydrophobic/superoleophilic properties after Ultraviolet irradiation.
WANG is equal to 2014 in article "In situ separation and collection of oil from water surface via a novel superoleophilic and superhydrophobic oil containment boom" (publication name: langmuir ") which describes that a super-hydrophobic-super-oleophilic metal copper mesh film is prepared by a simple method of electrolytic deposition and solution soaking respectively by taking a copper mesh as a base material.
By searching the keywords such as crude oil, cracking, oil absorption or multiple holes, the similar experimental device is not found, and by searching the crude oil and cracking, some crude oil cracking devices and methods are found, but the disclosed technology with the same structure and principle as the invention is not found, and meanwhile, the device and the method do not belong to the experimental device.
Disclosure of Invention
The invention aims to provide a high-temperature high-pressure crude oil cracking gas-forming simulation experiment device and a high-temperature high-pressure crude oil cracking gas-forming simulation experiment method, which are used for simulating a high-temperature cracking gas-forming process of crude oil under the condition of underground pressure, can prevent crude oil in an autoclave from flowing out during gas taking, can continuously crack the same crude oil sample into gas-forming simulation experiment, and can simulate the crude oil cracking gas-forming process under the condition of underground semi-closure-semi-opening.
In order to achieve the aim, the invention adopts the following technical scheme that the high-temperature high-pressure crude oil pyrolysis gas simulation experiment device comprises a high-temperature high-pressure reaction kettle, wherein an inlet at the bottom end of the high-temperature high-pressure reaction kettle is connected with an inlet pipeline, an outlet at the top end of the high-temperature high-pressure reaction kettle is connected with an outlet pipeline, and the high-temperature high-pressure reaction kettle comprises a kettle body and an oil absorption material layer arranged in the kettle body.
The oil absorbing material layer is at least provided with one layer.
The oil absorption material layer is made of a metal porous material with lipophilicity, and the metal porous material is arranged on the inner wall of the inner cavity of the kettle body through a sintering or welding method.
And the high-temperature high-pressure reaction kettle is connected with an inlet pipeline through a kettle bottom adapter at the bottom end inlet of the high-temperature high-pressure reaction kettle.
And the outlet at the top end of the high-temperature high-pressure reaction kettle is connected with an outlet pipeline through a kettle cover adapter.
The high-temperature high-pressure reaction kettle is arranged in a high-temperature heating furnace.
The inlet pipeline is sequentially connected with a constant pressure pump, a high-pressure water container and a high-pressure one-way valve in series according to the flow direction.
The outlet pipeline is sequentially connected with a pressure gauge, an overflow valve, an air storage chamber and an air taking valve in a penetrating way according to the flow direction, the overflow valve is connected with a pressure fine adjustment control pump, and the bottom of the air taking chamber is provided with a water drain valve.
The kettle body is made of high-temperature metal, can bear the high temperature of 500 ℃ and can bear the pressure of 70MPa; the metal porous material can bear the temperature of 500 ℃; the kettle bottom adapter and the kettle cover adapter can bear the temperature of 500 ℃.
The high-pressure one-way valve is connected between the high-pressure water container and the high-temperature high-pressure reaction kettle, and fluid can flow from the high-pressure water container to the high-temperature high-pressure reaction kettle in the high-pressure reaction kettle and can bear the pressure of 80MPa.
The overflow valve is connected between the autoclave outlet pipeline and the air storage chamber, and the pressure regulating range is 0-80 MPa.
The fine adjustment control pump is connected with the overflow valve, the working pressure is 0-80 MPa, and the control precision is +/-0.1 MPa.
The air storage chamber is connected between the outlet of the overflow valve and the air taking valve, the lower part of the air storage chamber is provided with a water drain valve, and the pressure of the air storage chamber is 80MPa.
In order to achieve the purpose, the invention adopts the following technical scheme that the simulation experiment method for cracking high-temperature and high-pressure crude oil into gas comprises the following steps:
step one, loading a crude oil sample into a high-temperature high-pressure reaction kettle. Weighing a certain amount of crude oil sample, inverting the high-temperature high-pressure reaction kettle, loading the crude oil sample into the high-temperature high-pressure reaction kettle at the opening of the lower part of the high-temperature high-pressure reaction kettle, and loading a kettle bottom adapter and a kettle cover adapter. And the high-pressure pipeline is connected with the kettle bottom adapter and the kettle cover adapter.
And step two, connecting all parts of the experimental device. And loading the high-temperature high-pressure reaction kettle into a high-temperature heating furnace. The high-pressure pipeline is connected with a constant-pressure pump, a high-pressure water container, a high-pressure single valve, a high-temperature high-pressure reaction kettle, a pressure gauge, an overflow valve, a pressure fine-tuning control pump, an air storage chamber and an air taking valve.
And step three, vacuumizing the device. And closing the high-pressure one-way valve and the air taking valve, and opening the overflow valve and the water drain valve. A vacuum pump was connected to the outlet line of the drain valve and was used to evacuate for minutes. The drain valve is closed.
And fourthly, pre-injecting water into the high-temperature high-pressure reaction kettle. And opening the high-pressure one-way valve, and injecting water in the high-pressure water container into the high-temperature high-pressure reaction kettle and the connecting pipeline by using the constant-pressure pump.
And fifthly, setting reaction temperature and pressure conditions. The simulation temperature of the high-temperature high-pressure reaction kettle is set by setting the temperature of the high-temperature heating furnace, so that water is not gasified in the high-temperature high-pressure reaction kettle in the reaction process, and the reaction temperature is set below the critical temperature (374.15 ℃) of water. The temperature is generally set to 350 ℃, and the crude oil cracking processes with different evolution degrees are simulated by adopting a constant temperature time-varying mode. The reaction pressure is set above the gas-liquid equilibrium pressure of water. And setting the overflow pressure of the overflow valve, namely the reaction pressure in the high-temperature high-pressure reaction kettle by setting the pressure of the pressure fine-tuning control pump according to the stratum pressure condition required by the simulation experiment. And the pressure inside the high-temperature high-pressure reaction kettle is supplemented by a constant-pressure pump, and the outlet pressure of the constant-pressure pump is slightly lower than the outlet pressure of the overflow valve.
And step six, constant-temperature cracking. When crude oil is subjected to a simulation experiment under the constant temperature condition, gas flowing out through an overflow valve is collected by the gas storage chamber, and when the gas is collected, a water drain valve and a gas taking valve of the gas storage chamber are closed.
And seventhly, cooling the reaction kettle and collecting gas. When the crude oil is cracked to a preset reaction time, the constant pressure pump, the high pressure one-way valve and the heating furnace are closed, and the high temperature and high pressure reaction kettle is gradually cooled to be close to the room temperature. Slowly until the overflow valve is completely opened, and opening the gas taking valve. The gas generated by the cracking of crude oil is collected, measured and subjected to component analysis.
And step eight, carrying out a crude oil cracking experiment of the next evolution degree. Repeating the step five, the step six and the step seven until the crude oil cracking experiment at all time points is completed.
And step nine, cleaning the device and collecting and metering residual crude oil. Cleaning the high-temperature high-pressure reaction kettle, each connecting part and the connection relation by using reagents such as a strong-polarity low-boiling-point organic solvent (such as trichloromethane) and the like, collecting cleaning liquid, volatilizing the cleaning reagent, and measuring the residual crude oil quantity of the reaction.
Compared with the prior art, the invention has the following beneficial effects:
the metal porous material in the high-temperature high-pressure reaction kettle is made of porous oleophylic material, and the periphery of the metal porous material is sintered or welded in the cavity of the high-pressure kettle, so that the crude oil is bound. The overflow valve is connected between the high-temperature high-pressure reaction kettle outlet pipeline and the air storage chamber, and can control the pressure in the high-temperature high-pressure reaction kettle cavity and the gas discharge condition. The simulation experiment device can prevent crude oil in the autoclave from flowing out during gas taking, and can continuously crack the same crude oil sample into gas simulation experiments; the method can also set the discharge pressure condition of crude oil pyrolysis gas, and realize the simulation of crude oil pyrolysis gas production process under the closed condition and under the semi-closed-semi-open condition with different discharge pressures.
Drawings
FIG. 1 is a schematic structural diagram of a simulation experiment device for cracking high-temperature and high-pressure crude oil into gas.
In the figure: 1. a high-temperature high-pressure reaction kettle, 11, a kettle body, 12, a metal porous material, 13, a kettle bottom adapter, 14, a kettle cover adapter, 2, a high-temperature heating furnace, 3, a constant pressure pump, 4, a high-pressure water container, 5, a high-pressure one-way valve, 6, a pressure gauge, 7, an overflow valve, 8, a pressure fine-tuning control pump, 9, an air storage chamber, 91, a water drain valve, 10 and an air taking valve.
Detailed Description
The detailed description and technical content of the present invention are described below with reference to the accompanying drawings, which are, however, only for reference and description, and are not intended to limit the present invention.
Example 1:
as shown in figure 1, the experimental device for simulating cracking of high-temperature and high-pressure crude oil into gas comprises a high-temperature and high-pressure reaction kettle 1, a high-temperature heating furnace 2, a constant-pressure pump 3, a high-pressure water container 4, a high-pressure one-way valve 5, a pressure gauge 6, an overflow valve 7, a pressure fine-tuning control pump 8, a gas storage chamber 9 and a gas taking valve 10. The inlet at the bottom end of the high-temperature high-pressure reaction kettle is connected with an inlet pipeline, the outlet at the top end of the high-temperature high-pressure reaction kettle is connected with an outlet pipeline, and the high-temperature high-pressure reaction kettle comprises a kettle body 11 and an oil absorption material layer arranged inside the kettle body. The oil absorbing material layer is at least provided with one layer. The oil absorption material layer is made of a metal porous material with lipophilicity, and the metal porous material 12 is arranged on the inner wall of the inner cavity of the kettle body through a sintering or welding method. The high-temperature high-pressure reaction kettle is connected with an inlet pipeline through a kettle bottom adapter 13 at the bottom end inlet of the high-temperature high-pressure reaction kettle. The outlet of the top end of the high-temperature high-pressure reaction kettle is connected with an outlet pipeline through a kettle cover adapter 14. The high-temperature high-pressure reaction kettle is arranged in a high-temperature heating furnace.
The inlet pipeline is sequentially connected with a constant pressure pump 3, a high-pressure water container 4 and a high-pressure one-way valve 5 in series according to the flow direction.
The outlet pipeline is sequentially connected with a pressure gauge 6, an overflow valve 7, an air storage chamber 9 and an air taking valve 10 in a penetrating way according to the flow direction, the overflow valve is connected with a pressure fine adjustment control pump 8, and the bottom of the air taking chamber is provided with a water drain valve 91.
The high-temperature high-pressure crude oil cracking gas-forming simulation experiment method comprises the following steps:
step one, loading a crude oil sample into a high-temperature high-pressure reaction kettle. Weighing a certain amount of crude oil sample, inverting the high-temperature high-pressure reaction kettle 1, loading the crude oil sample into the high-temperature high-pressure reaction kettle 1 at the opening of the lower part of the high-temperature high-pressure reaction kettle 1, and loading a kettle bottom adapter 13 and a kettle cover adapter 14. And a high-pressure pipeline connected with the kettle bottom adapter 13 and the kettle cover adapter 14 is arranged.
And step two, connecting all parts of the experimental device. The high-temperature high-pressure reaction kettle 1 is filled into a high-temperature heating furnace 2. The high-pressure pipeline is connected with a constant-pressure pump 3, a high-pressure water container 4, a high-pressure single valve 5, a high-temperature high-pressure reaction kettle 1, a pressure gauge 6, an overflow valve 7, a pressure fine-tuning control pump 8, an air storage chamber 9 and an air taking valve 10.
And step three, vacuumizing the device. The high-pressure check valve 5 and the air taking valve 10 are closed, and the overflow valve 7 and the drain valve 91 are opened. A vacuum pump was connected to the outlet line of the drain valve 91, and vacuum was applied for 5 minutes using the vacuum pump. The drain valve 91 is closed.
And fourthly, pre-injecting water into the high-temperature high-pressure reaction kettle. The high-pressure check valve 5 is opened, and water in the high-pressure water container 4 is injected into the high-temperature high-pressure reaction kettle 1 and the connecting pipeline by the constant-pressure pump 3.
And fifthly, setting reaction temperature and pressure conditions. The simulation temperature of the high-temperature high-pressure reaction kettle 1 is set by setting the temperature of the high-temperature heating furnace 2, and the reaction temperature is set below the critical temperature (374.15 ℃) of water in order to keep the water in the high-temperature high-pressure reaction kettle 1 from gasification in the reaction process. The temperature is generally set to 350 ℃, and the crude oil cracking processes with different evolution degrees are simulated by adopting a constant temperature time-varying mode. The reaction pressure is set above the gas-liquid equilibrium pressure of water. The overflow pressure of the overflow valve 7, that is, the reaction pressure inside the high-temperature high-pressure reaction kettle 1 is set by setting the pressure of the pressure fine-tuning control pump 8 according to the formation pressure condition required for the simulation experiment. The pressure inside the high-temperature high-pressure reaction kettle is supplemented by the constant-pressure pump 3, and the outlet pressure of the constant-pressure pump 3 is slightly lower than the outlet pressure of the overflow valve 7.
And step six, constant-temperature cracking. When crude oil is subjected to a simulation experiment under a constant temperature condition, the gas flowing out through the overflow valve 7 is collected by the gas storage chamber 9, and the water drain valve 91 and the gas taking valve 10 of the gas storage chamber 9 are closed during collection.
And seventhly, cooling the reaction kettle and collecting gas. When the crude oil is cracked to a preset reaction time, the constant pressure pump 3, the high pressure one-way valve 5 and the heating furnace 2 are closed, and the high temperature and high pressure reaction kettle 1 is gradually cooled to be close to the room temperature. Slowly until the overflow valve 7 is fully opened and the gas take valve 10 is opened. The gas generated by the cracking of crude oil is collected, measured and subjected to component analysis.
And step eight, carrying out a crude oil cracking experiment of the next evolution degree. Repeating the step five, the step six and the step seven until the crude oil cracking experiment at all time points is completed.
And step nine, cleaning the device and collecting and metering residual crude oil. Cleaning the high-temperature high-pressure reaction kettle 1, each connecting part and the connection relation by using reagents such as a strong-polarity low-boiling-point organic solvent (trichloromethane and the like), collecting cleaning liquid, volatilizing the cleaning reagent, and measuring the residual crude oil quantity of the reaction.
The kettle body 11 of the high-temperature high-pressure reaction kettle 1 is made of high-temperature metal, can bear the high temperature of 500 ℃ and can bear the pressure of 70MPa.
The metal porous material 12 is made of oleophilic material, and is sintered or welded in the autoclave cavity around, and is used for absorbing crude oil by utilizing the oleophilic and porous properties of the metal porous material, so that the crude oil is prevented from flowing into an outlet pipeline when being heated or the pressure of the crude oil is released. It can withstand high temperatures of 500 ℃.
In the experiment, a small amount of crude oil sample is filled from the bottom of the high-temperature high-pressure reaction kettle 1, and the high-temperature high-pressure reaction kettle 1 is placed in the high-temperature heating furnace outlet 2. The various components are connected by high pressure lines as shown in figure 1. The high-temperature high-pressure reaction kettle 1 is connected with an inlet pipeline through a kettle bottom adapter 13, and the high-temperature high-pressure reaction kettle 1 is connected with an outlet pipeline through a kettle cover adapter 14.
The high-temperature heating furnace 2 is used for heating the high-temperature high-pressure reaction kettle 1 and controlling the temperature. Can be heated to the middle temperature of 500 ℃ and the temperature control precision is +/-0.5 percent of the actual temperature.
The constant pressure pump 3 directly pressurizes the water medium in the high pressure water container 4, and is used for driving the water medium in the high pressure water container into the high temperature high pressure reaction kettle 1 and supplementing the pressure in the high temperature high pressure reaction kettle 1. The working pressure of the constant pressure pump 3 is 0-100 Ma, and the high pressure water container 4 can bear 80MPa.
The high-pressure check valve 5 can prevent crude oil from flowing back into the inlet pipeline due to the rising of the pressure in the high-temperature high-pressure reaction kettle 1 in the heating or reaction process. It can bear 80MPa.
The pressure gauge 6 is connected to an outlet pipeline of the high-temperature high-pressure reaction kettle 1 and is used for monitoring the pressure in the kettle. When the pressure in the kettle is far lower than the required pressure, the constant pressure pump 3 drives the water in the high pressure water container 4 to supplement the pressure in the high temperature and high pressure reaction kettle 1. The measuring range is 0-100 MPa, and the precision is +/-1 MPa.
The overflow valve 7 is connected between the outlet pipeline of the high-temperature high-pressure reaction kettle 1 and the air storage chamber 9 and is used for controlling the pressure in the cavity of the high-temperature high-pressure reaction kettle 1, and when the pressure in the high-temperature high-pressure reaction kettle 1 exceeds the set pressure of the overflow valve 7, the overflow valve is opened, and the air is discharged. The pressure of the overflow valve 7 is adjustable, and the closed condition simulation experiment and the semi-closed-semi-open condition simulation experiment with different opening pressures can be realized by setting the opening pressure of the overflow valve 7.
The pressure fine-tuning control pump 8 is connected with the overflow valve 7 and used for adjusting and controlling the pressure of the overflow valve 7 and indirectly adjusting the gas discharge pressure of the high-temperature high-pressure reaction kettle 1. The working pressure is 0-80 MPa, and the control precision is +/-0.1 MPa.
The air storage chamber 9 is connected with an outlet of the overflow valve, and the outlet end of the air storage chamber is connected with the air taking valve 10. For receiving the gas discharged when the pressure in the high-temperature high-pressure reaction kettle 1 is higher than the pressure of the overflow valve 7 and slowly discharging the gas until the overflow valve 7 is fully opened for taking the gas. The working pressure of the air storage chamber 7 is 0-80 MPa.
A drain valve 91 is connected to the lower part of the air reservoir 9 for draining condensed water from the air reservoir.
When the gas taking valve 10 is opened, the gas in the gas storage chamber 9 enters a metering and gas taking device, if the gas taking valve 10 is in an opened state when metering and taking in real time, and if the gas is taken in stages, the valve 10 is in a closed state before taking the gas.
Example 2:
as shown in figure 1, the experimental device for simulating cracking of high-temperature and high-pressure crude oil into gas comprises a high-temperature and high-pressure reaction kettle 1, a high-temperature heating furnace 2, a constant-pressure pump 3, a high-pressure water container 4, a high-pressure one-way valve 5, a pressure gauge 6, an overflow valve 7, a pressure fine-tuning control pump 8, a gas storage chamber 9 and a gas taking valve 10. The inlet at the bottom end of the high-temperature high-pressure reaction kettle is connected with an inlet pipeline, the outlet at the top end of the high-temperature high-pressure reaction kettle is connected with an outlet pipeline, and the high-temperature high-pressure reaction kettle comprises a kettle body 11 and an oil absorption material layer arranged inside the kettle body. The oil absorbing material layer is at least provided with one layer. The oil absorption material layer is made of a metal porous material with lipophilicity, and the metal porous material 12 is arranged on the inner wall of the inner cavity of the kettle body through a sintering or welding method. The high-temperature high-pressure reaction kettle is connected with an inlet pipeline through a kettle bottom adapter 13 at the bottom end inlet of the high-temperature high-pressure reaction kettle. The outlet of the top end of the high-temperature high-pressure reaction kettle is connected with an outlet pipeline through a kettle cover adapter 14. The high-temperature high-pressure reaction kettle is arranged in a high-temperature heating furnace.
The inlet pipeline is sequentially connected with a constant pressure pump 3, a high-pressure water container 4 and a high-pressure one-way valve 5 in series according to the flow direction.
Example 3:
as shown in figure 1, the experimental device for simulating cracking of high-temperature and high-pressure crude oil into gas comprises a high-temperature and high-pressure reaction kettle 1, a high-temperature heating furnace 2, a constant-pressure pump 3, a high-pressure water container 4, a high-pressure one-way valve 5, a pressure gauge 6, an overflow valve 7, a pressure fine-tuning control pump 8, a gas storage chamber 9 and a gas taking valve 10. The inlet at the bottom end of the high-temperature high-pressure reaction kettle is connected with an inlet pipeline, the outlet at the top end of the high-temperature high-pressure reaction kettle is connected with an outlet pipeline, and the high-temperature high-pressure reaction kettle comprises a kettle body 11 and an oil absorption material layer arranged inside the kettle body. The oil absorbing material layer is at least provided with one layer. The oil absorption material layer is made of a metal porous material with lipophilicity, and the metal porous material 12 is arranged on the inner wall of the inner cavity of the kettle body through a sintering or welding method. The high-temperature high-pressure reaction kettle is connected with an inlet pipeline through a kettle bottom adapter 13 at the bottom end inlet of the high-temperature high-pressure reaction kettle. The outlet of the top end of the high-temperature high-pressure reaction kettle is connected with an outlet pipeline through a kettle cover adapter 14. The high-temperature high-pressure reaction kettle is arranged in a high-temperature heating furnace.
The outlet pipeline is sequentially connected with a pressure gauge 6, an overflow valve 7, an air storage chamber 9 and an air taking valve 10 in a penetrating way according to the flow direction, the overflow valve is connected with a pressure fine adjustment control pump 8, and the bottom of the air taking chamber is provided with a water drain valve 91.
The foregoing description of the preferred embodiments of the present invention is not intended to limit the scope of the invention, but rather to limit the scope of the invention to the equivalents of the claims to which the invention pertains.
Claims (2)
1. The high-temperature high-pressure crude oil cracking gas simulation experiment device comprises a high-temperature high-pressure reaction kettle, wherein an inlet at the bottom end of the high-temperature high-pressure reaction kettle is connected with an inlet pipeline, and an outlet at the top end of the high-temperature high-pressure reaction kettle is connected with an outlet pipeline;
the oil absorption material layer is made of a metal porous material with lipophilicity, and the metal porous material is arranged on the inner wall of the inner cavity of the kettle body through a sintering or welding method;
the high-temperature high-pressure reaction kettle is connected with an inlet pipeline through a kettle bottom adapter at the bottom end inlet of the high-temperature high-pressure reaction kettle; the outlet of the top end of the high-temperature high-pressure reaction kettle is connected with an outlet pipeline through a kettle cover adapter; the high-temperature high-pressure reaction kettle is arranged in a high-temperature heating furnace; the inlet pipeline is sequentially connected with a constant pressure pump, a high-pressure water container and a high-pressure one-way valve in series according to the flow direction; the outlet pipeline is sequentially connected with a pressure gauge, an overflow valve, an air storage chamber and an air taking valve in a penetrating way according to the flow direction, the overflow valve is connected with a pressure fine adjustment control pump, and the bottom of the air storage chamber is provided with a water drain valve;
the kettle body is made of high-temperature metal, can bear the high temperature of 500 ℃ and can bear the pressure of 70MPa; the metal porous material can bear the temperature of 500 ℃; the kettle bottom adapter and the kettle cover adapter can bear the temperature of 500 ℃;
the high-pressure one-way valve is connected between the high-pressure water container and the high-temperature high-pressure reaction kettle, and fluid can flow from the high-pressure water container to the high-temperature high-pressure reaction kettle in the high-pressure reaction kettle and can bear the pressure of 80MPa;
the overflow valve is connected between an autoclave outlet pipeline and the air storage chamber, and the pressure regulating range is 0-80 MPa;
the pressure fine-tuning control pump is connected with the overflow valve, the working pressure is 0-80 MPa, and the control precision is +/-0.1 MPa;
the air storage chamber is connected between the outlet of the overflow valve and the air taking valve, the lower part of the air storage chamber is provided with a water drain valve, and the pressure of the air storage chamber is 80MPa.
2. An experimental method using the high-temperature and high-pressure crude oil cracking gas simulation experimental device as set forth in claim 1, comprising the following steps:
step one, loading a crude oil sample into a high-temperature high-pressure reaction kettle; inverting the high-temperature high-pressure reaction kettle, loading a crude oil sample into the high-temperature high-pressure reaction kettle at an opening at the lower part of the high-temperature high-pressure reaction kettle, and loading a kettle bottom adapter and a kettle cover adapter; the high-pressure pipeline is connected with the kettle bottom adapter and the kettle cover adapter;
step two, connecting all parts of an experimental device; loading the high-temperature high-pressure reaction kettle into a high-temperature heating furnace; the high-pressure pipeline is connected with a constant-pressure pump, a high-pressure water container, a high-pressure one-way valve, a high-temperature high-pressure reaction kettle, a pressure gauge, an overflow valve, a pressure fine-tuning control pump, an air storage chamber and an air taking valve;
step three, vacuumizing the device; closing the high-pressure one-way valve and the air taking valve, and opening the overflow valve and the water drain valve; connecting a vacuum pump to an outlet pipeline of a water drain valve, and vacuumizing for 5 minutes by using the vacuum pump; closing the water drain valve;
step four, pre-injecting water into the high-temperature high-pressure reaction kettle; opening a high-pressure one-way valve, and injecting water in the high-pressure water container into the high-temperature high-pressure reaction kettle and the connecting pipeline by utilizing the constant-pressure pump;
step five, setting reaction temperature and pressure conditions; setting the simulation temperature of a high-temperature high-pressure reaction kettle by setting the temperature of a high-temperature heating furnace, wherein the reaction temperature is below the critical temperature of water, namely below 374.15 ℃ in order to ensure that water is not gasified in the high-temperature high-pressure reaction kettle in the reaction process; simulating crude oil cracking processes with different evolution degrees by adopting a constant temperature time-varying mode; the reaction pressure is set above the gas-liquid equilibrium pressure of water; according to stratum pressure conditions required by the simulation experiment, setting overflow pressure of an overflow valve, namely reaction pressure in the high-temperature high-pressure reaction kettle, by setting pressure of a pressure fine-tuning control pump; the pressure inside the high-temperature high-pressure reaction kettle is supplemented by a constant pressure pump, and the outlet pressure of the constant pressure pump is lower than the outlet pressure of the overflow valve;
step six, constant-temperature cracking; when crude oil is subjected to a simulation experiment under a constant temperature condition, collecting gas flowing out through an overflow valve by using a gas storage chamber, and closing a water drain valve and a gas taking valve of the gas storage chamber during collection;
step seven, cooling the reaction kettle and collecting gas; when crude oil is cracked to a preset reaction time, the constant pressure pump, the high-pressure one-way valve and the heating furnace are closed, and the high-temperature high-pressure reaction kettle is gradually cooled to be close to the room temperature; slowly opening the overflow valve until the overflow valve is completely opened, and opening the air taking valve; collecting gas generated by crude oil pyrolysis, metering and analyzing components;
step eight, carrying out a crude oil cracking experiment of the next evolution degree; repeating the step five, the step six and the step seven until the crude oil cracking experiment at all time points is completed;
step nine, cleaning the device and collecting and metering residual crude oil; and cleaning the high-temperature high-pressure reaction kettle, each connecting part and the connection relation by using a strong-polarity low-boiling-point organic solvent, collecting cleaning liquid, volatilizing a cleaning reagent, and metering the residual crude oil quantity of the reaction.
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