CN107831297A - HTHP crude oil pyrolysis is into gas analogue experiment installation and method - Google Patents
HTHP crude oil pyrolysis is into gas analogue experiment installation and method Download PDFInfo
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- CN107831297A CN107831297A CN201710568005.8A CN201710568005A CN107831297A CN 107831297 A CN107831297 A CN 107831297A CN 201710568005 A CN201710568005 A CN 201710568005A CN 107831297 A CN107831297 A CN 107831297A
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- 239000010779 crude oil Substances 0.000 title claims abstract description 82
- 238000000197 pyrolysis Methods 0.000 title claims abstract description 46
- 238000002474 experimental method Methods 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000009434 installation Methods 0.000 title claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 124
- 239000000463 material Substances 0.000 claims abstract description 49
- 239000003921 oil Substances 0.000 claims abstract description 35
- 229910052751 metal Inorganic materials 0.000 claims abstract description 24
- 239000002184 metal Substances 0.000 claims abstract description 24
- 238000010521 absorption reaction Methods 0.000 claims abstract description 16
- 238000005336 cracking Methods 0.000 claims abstract description 9
- 238000005245 sintering Methods 0.000 claims abstract description 8
- 238000003466 welding Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 44
- 238000003860 storage Methods 0.000 claims description 30
- 238000007599 discharging Methods 0.000 claims description 21
- 238000004140 cleaning Methods 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000012530 fluid Substances 0.000 claims description 6
- 239000003153 chemical reaction reagent Substances 0.000 claims description 5
- 238000004458 analytical method Methods 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 3
- 239000007943 implant Substances 0.000 claims description 3
- 239000007769 metal material Substances 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 238000001228 spectrum Methods 0.000 claims description 2
- 238000004088 simulation Methods 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 42
- 239000011148 porous material Substances 0.000 description 7
- 230000003075 superhydrophobic effect Effects 0.000 description 7
- 229910000831 Steel Inorganic materials 0.000 description 6
- 239000010959 steel Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 238000010146 3D printing Methods 0.000 description 4
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 4
- 239000010931 gold Substances 0.000 description 4
- 229910052737 gold Inorganic materials 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
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 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
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 239000012736 aqueous medium Substances 0.000 description 2
- 239000011248 coating agent Substances 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
- 239000000843 powder Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- HFQQZARZPUDIFP-UHFFFAOYSA-M sodium;2-dodecylbenzenesulfonate Chemical compound [Na+].CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O HFQQZARZPUDIFP-UHFFFAOYSA-M 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 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
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- -1 cracking Substances 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 150000002085 enols Chemical class 0.000 description 1
- 238000001914 filtration 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
- 238000007654 immersion Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 239000012528 membrane Substances 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
- 238000007639 printing Methods 0.000 description 1
- 239000010734 process oil Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000013589 supplement Substances 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
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc 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 & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Medicinal Chemistry (AREA)
- Biochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Food Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Processing Of Solid Wastes (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention discloses HTHP crude oil pyrolysis into gas analogue experiment installation and method, including high-temperature high-pressure reaction kettle, high-temperature high-pressure reaction kettle bottom entrance connection suction line, high-temperature high-pressure reaction kettle top export connection outlet pipeline, the high-temperature high-pressure reaction kettle include kettle and the oil absorption material layer being arranged on inside kettle.The oil absorption material layer is at least provided with one layer.The material of the oil absorption material layer is to be arranged on cavity wall in kettle by sintering or welding method with oil loving metal polyporous material, metal polyporous material.The present invention is used for Pintsch process of the Simulation of Crude Oil under the conditions of subsurface pressure into gas process, crude oil outflow when can prevent from taking gas in autoclave, continuous cracking into gas simulated experiment can be carried out to same crude oil sample, and can simulate underground it is semiclosed it is semi-open under the conditions of crude oil pyrolysis into gas process.
Description
Technical field
The present invention relates to petroleum geology analogue experiment installation, specifically HTHP crude oil pyrolysis is into gas simulated experiment
Device and method.
Background technology
Crude oil pyrolysis in laboratory split under high-temperature and high-pressure conditions into a kind of important origin cause of formation that gas is underground natural gas
Solution simulated experiment is to study a kind of important means that crude oil pyrolysis gas exploration was managed and instructed in crude oil pyrolysis into mechanism of qi.At present, simulate
The main working method of experimental provision is：Crude oil is placed into autoclave, or crude oil inclosure gold tube is reloaded into autoclave, is closed
Close outlet valve.Pressure is applied to crude oil or gold tube with fluid (water, helium etc.) medium, after an experiment terminates, opened high
Pressure kettle outlet valve, which collects the gas generated or taking-up and punctures gold tube, collects gas.Received opening valve or puncturing gold tube
When collecting gas, due to the quick release of pressure, the outflow of crude oil can be caused, therefore higher evolutionary track can not be carried out using the sample
The quantitative cleavage experiment of degree；In addition, in whole heating simulation course of reaction, system is closing, can not simulate underground condition
Under semiclosed-semi-open condition.In view of the above-mentioned problems, devise this analogue experiment installation.
Metal polyporous material and sintering technology are prior art.
Application number：201610894797.3 publication date 2017-05-10 discloses a kind of metal polyporous material and its preparation
Method, the preparation method include：(1) titanium powder and boron powder are well mixed, existed using 3D printing metal laser sintering technology
Mixed metal powder is printed as to the material of required shape at 2800~3200 DEG C；(2) will there is given shape material in step (1)
Material is heated to 2500~2700 DEG C, makes boron and the titanium liquefaction do not reacted completely, flows out outside the given shape material, that is, obtain institute
Need the metal polyporous material of shape.The present invention can directly be printed as part shape using 3D printing laser metal sintering technology,
Secondary operation is not needed；Processing part shape modeling is easier, flexible stronger；It is anti-that 3D printing equipment division provides two kinds of powder chemistries
Answer required energy.Suitable 3D printing machined parameters are set, and by boron powder and titanium powder printing shaping, obtained metal is more
The hardness and fusing point of Porous materials are higher, and pore size is 3~100 μm.
Feng is equal to 2004 in article " A Super-hydrophobic and super-oleophilic coating
Mesh film for the separation of oil and water " (periodical is entitled " Angew.Chem.Int.Ed. ")
Elaborate：PTFE emulsion is sprayed on stainless (steel) wire, and about 30min is handled in 350 DEG C of drying boxes, film surface presents super thin
Water/super oil-wet behavior.
Feng is equal to 2004 also in article：“A superhydrophobic and superoleophilic
Coating mesh film for the separation of oil and water " (periodical titles：“Angewandte
Chemie International Edition ") mention：By PTFE, adhesive polyvinyl acetate (PVAc), the poly- second of dispersant
Enol (PVA), Surfactant SDS (SDBS) and water form mixed emulsion by stirring, then spray emulsion
It is applied on stainless (steel) wire, by high-temperature process, forms the low-surface-energy PTFE coatings of coarse micro nano structure.Prepare not
Rust steel mesh has the characteristic of super-hydrophobic and super oleophylic.
LEE is equal to 2011, in article " The performance of superhydrophobic and
Superoleophilic carbon nano tube meshes in water-oil filtration " (periodical titles：
" Carbon ") its method for utilizing chemical vapor deposition is elaborated, treated porous CNT is grown in stainless (steel) wire
On, prepare the stainless (steel) wire membrane material with super-hydrophobic-super-oleophilic energy, the separation for oil hydrosol.
WANG is equal to 2012 in article " Ultraviolet-durable superhydrophobic zinc oxide-
coated mesh films for surface and underwater-oil capture and transportation”
(journal name：" Langmuir ") it refer to it and use hydro-thermal method, ZnO microstructured coatings are formed in stainless (steel) wire surface, it is ultraviolet
After irradiation, it possesses stable super-hydrophobic/super-oleophilic performance.
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 " (journal names：" Langmuir ") it is elaborated using copper mesh as base material, it is heavy by being electrolysed respectively
Product and the short-cut method of solution immersion prepare the metallic copper mesh film of super-hydrophobic-super oleophylic.
By retrieving crude oil, cracking, oil suction or the keyword such as porous, similar experimental provision is not found, it is former by retrieval
Oil, cracking, it was found that some crude oil cracking devices and method, but without discovery with same structure of the present invention and the open skill of principle
Art, while also it is not admitted to experimental provision.
The content of the invention
It is an object of the invention to provide HTHP crude oil pyrolysis into gas analogue experiment installation and method, for simulating original
Pintsch process of the oil under the conditions of subsurface pressure is into gas process, and crude oil outflow when can prevent from taking gas in autoclave can be to same
Crude oil sample carries out continuous cracking into gas simulated experiment, and can simulate underground it is semiclosed-semi-open under the conditions of crude oil split
Solution is into gas process.
In order to reach above-mentioned purpose, present invention employs following technical scheme, HTHP crude oil pyrolysis is simulated real into gas
Experiment device, including high-temperature high-pressure reaction kettle, high-temperature high-pressure reaction kettle bottom entrance connection suction line, high-temperature high-voltage reaction
Kettle top export connection outlet pipeline, the high-temperature high-pressure reaction kettle include kettle and the oil absorption material being arranged on inside kettle
Layer.
The oil absorption material layer is at least provided with one layer.
The material of the oil absorption material layer be with oil loving metal polyporous material, metal polyporous material by sintering or
Welding method is arranged on cavity wall in kettle.
High-temperature high-pressure reaction kettle is connected by high-temperature high-pressure reaction kettle bottom entrance with bottom adapter with suction line.
High-temperature high-pressure reaction kettle is connected by the high-temperature high-pressure reaction kettle top export with kettle cover adapter with outlet line
Connect.
The high-temperature high-pressure reaction kettle is placed in high-temperature heater.
On the suction line constant pressure pump, high-pressure water container, high pressure check valve have been sequentially connected in series by flow direction.
Worn successively by flow direction on the outlet line and be connected to pressure gauge, overflow valve, air storage chamber, take air valve, the overflow
Valve connects pressure vernier control pump, described to take air chamber bottom to set discharging valve.
The kettle is high-temperature metal material, can bear 500 DEG C of high temperature, can bear pressure 70MPa；The metal porous material
Material can 500 DEG C of bearing temperature；500 DEG C of bottom adapter and kettle cover adapter the energy bearing temperature.
The high pressure check valve is connected between high-pressure water container and high-temperature high-pressure reaction kettle, and fluid internally can be from high pressure
Water receptacle flows to high-temperature high-pressure reaction kettle, can bear pressure 80MPa.
The overflow valve is connected between autoclave outlet line and air storage chamber, 0~80MPa of pressure regulation spectrum.
The vernier control pump discharge is connected to overflow valve, 0~80MPa of operating pressure, control accuracy ± 0.1MPa.
Between the air storage chamber is connected to overflow valve outlet and takes air valve, its underpart is discharging valve, air storage chamber pressure-bearing
80MPa。
In order to reach above-mentioned purpose, present invention employs following technical scheme, HTHP crude oil pyrolysis is simulated real into gas
Proved recipe method, its step are：
Step 1, crude oil sample is loaded into high-temperature high-pressure reaction kettle.A certain amount of crude oil sample is weighed, by high temperature high pressure reverse
Answer kettle to be inverted, crude oil sample is loaded into high-temperature high-pressure reaction kettle at high-temperature high-pressure reaction kettle lower openings, load onto bottom switching
Head and kettle cover adapter.Load onto the connection high pressure line of bottom adapter and kettle cover adapter.
Step 2, connect each part of experimental provision.High-temperature high-pressure reaction kettle is loaded into high-temperature heater.Connected with high pressure line
Connect constant pressure pump, high-pressure water container, high pressure individual event valve, high-temperature high-pressure reaction kettle, pressure gauge, overflow valve, pressure vernier control pump, storage
Air chamber and take air valve.
Step 3, device vacuumize.Close high pressure check valve and take air valve, open overflow valve and discharging valve.By vacuum
Pump is connected to discharging valve outlet line, and minute is vacuumized using vavuum pump.Close discharging valve.
Step 4, to high-temperature high-pressure reaction kettle pre-implant water.High pressure check valve is opened, using constant pressure pump by high-pressure water container
In water be injected into high-temperature high-pressure reaction kettle and connecting pipeline.
Step 5, reaction temperature and pressure condition are set.By setting high-temperature heater temperature setting high-temperature high-voltage reaction
The analog temperature of kettle, to cause course of reaction reclaimed water to keep not gasifying in high-temperature high-pressure reaction kettle, reaction temperature is arranged on water
Critical-temperature (374.15 DEG C) below.350 DEG C are traditionally arranged to be, time mode is become using constant temperature to simulate different evolution grades
Crude oil pyrolysis process.Reaction pressure is arranged on more than the liquid-vapor equilibrium pressure of water.Ground lamination according to required for simulated experiment
Power condition, the spill pressure of overflow valve is set i.e. inside high-temperature high-pressure reaction kettle by setting the pressure of pressure vernier control pump
Reaction pressure.Ftercompction is carried out to high-temperature high-pressure reaction kettle inside using constant pressure pump, the outlet pressure of constant pressure pump, which is set, to be slightly below
The outlet pressure of overflow valve.
Step 6, constant temperature cracking.Crude oil is collected with air storage chamber and flowed out by overflow valve when constant temperature Imitating is tested
Gas, during collection, close the discharging valve of air storage chamber and take air valve.
Step 7, reactor is cooled down, collect gas.During crude oil pyrolysis to the predetermined reaction time, constant pressure pump, high pressure are closed
Check valve and heating furnace, high-temperature high-pressure reaction kettle is progressively cooled to close to room temperature.Slowly until opening overflow valve completely, and beat
Open and take air valve.The gas of crude oil pyrolysis generation is collected, measures and carries out component analysis.
Step 8, carry out the crude oil pyrolysis experiment of next evolution grade.Repeat step five, step 6 and step 7, directly
To the crude oil pyrolysis experiment for completing all time points.
Step 9, cleaning device are simultaneously collected, measure residual crude oil.With highly polar low boiling point organic solvent (chloroform etc.)
Deng reagent cleaning high-temperature high-pressure reaction kettle, each connection member and annexation, and cleaning fluid is collected, volatilize cleaning reagent, and counts
Quantitative response residual crude oil amount.
Compared to prior art, the invention has the advantages that：
Metal polyporous material in high-temperature high-pressure reaction kettle is porous oleophylic material, and surrounding sinters or be welded in autoclave chamber
It is interior, be advantageous to hold onto crude oil.The overflow valve is connected between high-temperature high-pressure reaction kettle outlet line and air storage chamber, can control
High-temperature high-pressure reaction kettle cavity pressure and gas conditions of discharge.The crude oil when analogue experiment installation can prevent from taking gas in autoclave
Outflow, continuous cracking into gas simulated experiment can be carried out to same crude oil sample；The aerial drainage pressure of Oil Cracked Gas can also be set
Power condition, is realized under sealing condition, and different discharge pressure it is semiclosed-semi-open under the conditions of crude oil pyrolysis into gas process mould
Intend.
Brief description of the drawings
Fig. 1 is the structural representation of HTHP crude oil pyrolysis of the invention into gas analogue experiment installation.
In figure：1st, high-temperature high-pressure reaction kettle, 11, kettle, 12, metal polyporous material, 13, bottom adapter, 14, kettle cover turns
Joint, 2, high-temperature heater, 3, constant pressure pump, 4, high-pressure water container, 5, high pressure check valve, 6, pressure gauge, 7, overflow valve, 8, pressure
Vernier control pump, 9, air storage chamber, 91, discharging valve, 10, take air valve.
Embodiment
Detailed description for the present invention and technology contents, coordinate brief description of the drawings as follows, but accompanying drawing is only with reference to saying
It is bright to be used, not it is used for being any limitation as the present invention.
Embodiment 1：
As shown in Figure 1, HTHP crude oil pyrolysis is into gas analogue experiment installation, including high-temperature high-pressure reaction kettle 1, high temperature
Heating furnace 2, constant pressure pump 3, high-pressure water container 4, high pressure check valve 5, pressure gauge 6, overflow valve 7, pressure vernier control pump 8, gas storage
Room 9, take air valve 10.High-temperature high-pressure reaction kettle bottom entrance connection suction line, high-temperature high-pressure reaction kettle top export
Connection outlet pipeline, the high-temperature high-pressure reaction kettle include kettle 11 and the oil absorption material layer being arranged on inside kettle.It is described
Oil absorption material layer is at least provided with one layer.The material of the oil absorption material layer is more with oil loving metal polyporous material, metal
Porous materials 12 are arranged on cavity wall in kettle by sintering or welding method.High-temperature high-pressure reaction kettle bottom entrance is with bottom
High-temperature high-pressure reaction kettle is connected by adapter 13 with suction line.The high-temperature high-pressure reaction kettle top export is with kettle cover adapter
14 are connected high-temperature high-pressure reaction kettle with outlet line.The high-temperature high-pressure reaction kettle is placed in high-temperature heater.
On the suction line constant pressure pump 3, high-pressure water container 4, high pressure check valve 5 have been sequentially connected in series by flow direction.
Worn successively by flow direction on the outlet line and be connected to pressure gauge 6, overflow valve 7, air storage chamber 9, take air valve 10, it is described
Overflow valve connection pressure vernier control pump 8, it is described to take air chamber bottom that discharging valve 91 is set.
HTHP crude oil pyrolysis is into gas analogue experiment method, its step：
Step 1, crude oil sample is loaded into high-temperature high-pressure reaction kettle.A certain amount of crude oil sample is weighed, by high temperature high pressure reverse
Answer kettle 1 to be inverted, crude oil sample is loaded into high-temperature high-pressure reaction kettle 1 at the lower openings of high-temperature high-pressure reaction kettle 1, load onto bottom and turn
Joint 13 and kettle cover adapter 14.Load onto the connection high pressure line of bottom adapter 13 and kettle cover adapter 14.
Step 2, connect each part of experimental provision.High-temperature high-pressure reaction kettle 1 is loaded into high-temperature heater 2.With high pressure line
Connect constant pressure pump 3, high-pressure water container 4, high pressure individual event valve 5, high-temperature high-pressure reaction kettle 1, pressure gauge 6, overflow valve 7, pressure fine setting
Controlling pump 8, air storage chamber 9 and take air valve 10.
Step 3, device vacuumize.Close high pressure check valve 5 and take air valve 10, open overflow valve 7 and discharging valve 91.
Vavuum pump is connected to the outlet line of discharging valve 91, vacuumized 5 minutes using vavuum pump.Close discharging valve 91.
Step 4, to high-temperature high-pressure reaction kettle pre-implant water.High pressure check valve 5 is opened, using constant pressure pump 3 by the high pressure water capacity
Water in device 4 is injected into high-temperature high-pressure reaction kettle 1 and connecting pipeline.
Step 5, reaction temperature and pressure condition are set.By setting the temperature setting high-temperature high-voltage reaction of high-temperature heater 2
The analog temperature of kettle 1, to cause course of reaction reclaimed water to keep not gasifying in high-temperature high-pressure reaction kettle 1, reaction temperature is arranged on
The critical-temperature (374.15 DEG C) of water is below.350 DEG C are traditionally arranged to be, time mode is become using constant temperature to simulate different evolutionary tracks
The crude oil pyrolysis process of degree.Reaction pressure is arranged on more than the liquid-vapor equilibrium pressure of water.Stratum according to required for simulated experiment
Pressure condition, the spill pressure of overflow valve 7 i.e. high-temperature high-pressure reaction kettle is set by setting the pressure of pressure vernier control pump 8
Reaction pressure inside 1.Ftercompction is carried out to high-temperature high-pressure reaction kettle inside using constant pressure pump 3, the outlet pressure of constant pressure pump 3 is set
The slightly below outlet pressure of overflow valve 7.
Step 6, constant temperature cracking.Crude oil is collected with air storage chamber 9 and flowed by overflow valve 7 when constant temperature Imitating is tested
The gas gone out, during collection, close the discharging valve 91 of air storage chamber 9 and take air valve 10.
Step 7, reactor is cooled down, collect gas.During crude oil pyrolysis to the predetermined reaction time, constant pressure pump 3, height are closed
Check valve 5 and heating furnace 2 are pressed, high-temperature high-pressure reaction kettle 1 is progressively cooled to close to room temperature.Slowly until opening overflow valve completely
7, and open and take air valve 10.The gas of crude oil pyrolysis generation is collected, measures and carries out component analysis.
Step 8, carry out the crude oil pyrolysis experiment of next evolution grade.Repeat step five, step 6 and step 7, directly
To the crude oil pyrolysis experiment for completing all time points.
Step 9, cleaning device are simultaneously collected, measure residual crude oil.With highly polar low boiling point organic solvent (chloroform etc.)
Deng reagent cleaning high-temperature high-pressure reaction kettle 1, each connection member and annexation, and cleaning fluid is collected, volatilize cleaning reagent, and counts
Quantitative response residual crude oil amount.
The kettle 11 of high-temperature high-pressure reaction kettle 1 is high-temperature metal material, can bear 500 DEG C of high temperature, allowable stress
70MPa。
Metal polyporous material 12 is oleophylic material, and surrounding sinters or be welded in autoclave intracavitary, utilizes its lipophile and more
Pore property, for adsorbing crude oil, prevent crude oil from flowing into outlet line in heating or when taking atmospheric pressure to discharge.It can bear 500
DEG C high temperature.
During experiment, a small amount of crude oil sample is loaded from the bottom of high-temperature high-pressure reaction kettle 1, high-temperature high-pressure reaction kettle 1 is placed
Come out of the stove in high-temperature heating in 2.All parts are connected with high pressure line as shown in Figure 1.With bottom adapter 13 by high temperature high pressure reverse
Answer kettle 1 to be connected with suction line, high-temperature high-pressure reaction kettle 1 is connected with outlet line with kettle cover adapter 14.
High-temperature heater 2 is used to heat to high-temperature high-pressure reaction kettle 1 and control temperature.Can be heated to its middle portion temperature is
500 DEG C, temperature control precision is ± the 0.5% of actual temperature.
Constant pressure pump 3 is directly the aqueous medium pressurization in high-pressure water container 4, for the aqueous medium in high-pressure water container to be driven in
High-temperature high-pressure reaction kettle 1, and supplement pressure in high-temperature high-pressure reaction kettle 1.0~the 100Ma of operating pressure of constant pressure pump 3, the high pressure water capacity
Device 4 can pressure-bearing 80MPa.
High pressure check valve 5 can prevent heating or course of reaction in, pressure rise in high-temperature high-pressure reaction kettle 1 and cause crude oil
Blow back into suction line.It can pressure-bearing 80MPa.
Pressure gauge 6 is connected to the outlet line of high-temperature high-pressure reaction kettle 1, for monitoring pressure in kettle.When pressure is remote in kettle
During less than required pressure, the reclaimed water of high-pressure water container 4, the ftercompction into high-temperature high-pressure reaction kettle 1 are driven by constant pressure pump 3.It is measured
0~100MPa of scope, precision ± 1MPa.
Overflow valve 7 is connected between the outlet line of high-temperature high-pressure reaction kettle 1 and air storage chamber 9, for controlling high temperature high pressure reverse
The cavity pressure of kettle 1 is answered, when pressure exceedes the setting pressure of overflow valve 7 in high-temperature high-pressure reaction kettle 1, overflow valve is opened, gas row
Go out.The pressure adjustable of overflow valve 7, by setting the Opening pressure of overflow valve 7 to realize sealing condition simulated experiment, the open pressure of difference
Semiclosed-semi-open condition simulation experiment.
Pressure vernier control pump 8 is connected to overflow valve 7, for the pressure of adjustment control overflow valve 7, adjusts HTHP indirectly
The gas discharge pressure of reactor 1.0~80MPa of its operating pressure, control accuracy ± 0.1MPa.
Air storage chamber 9 is connected to overflow valve outlet, and the port of export is with taking air valve 10 to be connected.For receiving high-temperature high-pressure reaction kettle
Pressure is higher than the gas discharged during 7 pressure of overflow valve in 1, and slowly until opening overflow valve 7 completely takes the gas discharged during gas
Body.0~the 80MPa of operating pressure of air storage chamber 7.
Discharging valve 91 is connected to the bottom of air storage chamber 9, and ponding is condensed for discharging steam in air storage chamber.
When taking the opening of air valve 10, the gas in air storage chamber 9 enters metering and collector, if real time measure takes gas,
Then take air valve 10 to be in open mode, if the stage takes gas, take gas early gate 10 to be closed.
Embodiment 2：
As shown in Figure 1, HTHP crude oil pyrolysis is into gas analogue experiment installation, including high-temperature high-pressure reaction kettle 1, high temperature
Heating furnace 2, constant pressure pump 3, high-pressure water container 4, high pressure check valve 5, pressure gauge 6, overflow valve 7, pressure vernier control pump 8, gas storage
Room 9, take air valve 10.High-temperature high-pressure reaction kettle bottom entrance connection suction line, high-temperature high-pressure reaction kettle top export
Connection outlet pipeline, the high-temperature high-pressure reaction kettle include kettle 11 and the oil absorption material layer being arranged on inside kettle.It is described
Oil absorption material layer is at least provided with one layer.The material of the oil absorption material layer is more with oil loving metal polyporous material, metal
Porous materials 12 are arranged on cavity wall in kettle by sintering or welding method.High-temperature high-pressure reaction kettle bottom entrance is with bottom
High-temperature high-pressure reaction kettle is connected by adapter 13 with suction line.The high-temperature high-pressure reaction kettle top export is with kettle cover adapter
14 are connected high-temperature high-pressure reaction kettle with outlet line.The high-temperature high-pressure reaction kettle is placed in high-temperature heater.
On the suction line constant pressure pump 3, high-pressure water container 4, high pressure check valve 5 have been sequentially connected in series by flow direction.
Embodiment 3：
As shown in Figure 1, HTHP crude oil pyrolysis is into gas analogue experiment installation, including high-temperature high-pressure reaction kettle 1, high temperature
Heating furnace 2, constant pressure pump 3, high-pressure water container 4, high pressure check valve 5, pressure gauge 6, overflow valve 7, pressure vernier control pump 8, gas storage
Room 9, take air valve 10.High-temperature high-pressure reaction kettle bottom entrance connection suction line, high-temperature high-pressure reaction kettle top export
Connection outlet pipeline, the high-temperature high-pressure reaction kettle include kettle 11 and the oil absorption material layer being arranged on inside kettle.It is described
Oil absorption material layer is at least provided with one layer.The material of the oil absorption material layer is more with oil loving metal polyporous material, metal
Porous materials 12 are arranged on cavity wall in kettle by sintering or welding method.High-temperature high-pressure reaction kettle bottom entrance is with bottom
High-temperature high-pressure reaction kettle is connected by adapter 13 with suction line.The high-temperature high-pressure reaction kettle top export is with kettle cover adapter
14 are connected high-temperature high-pressure reaction kettle with outlet line.The high-temperature high-pressure reaction kettle is placed in high-temperature heater.
Worn successively by flow direction on the outlet line and be connected to pressure gauge 6, overflow valve 7, air storage chamber 9, take air valve 10, it is described
Overflow valve connection pressure vernier control pump 8, it is described to take air chamber bottom that discharging valve 91 is set.
Presently preferred embodiments of the present invention is the foregoing is only, is not used to limit the scope of the claims of the present invention, other are with this
The equivalence changes of patent of invention spirit, it all should all belong to the scope of the claims of the present invention.
Claims (14)
1. HTHP crude oil pyrolysis is into gas analogue experiment installation, including high-temperature high-pressure reaction kettle, the high-temperature high-pressure reaction kettle
Bottom entrance connection suction line, high-temperature high-pressure reaction kettle top export connection outlet pipeline, it is characterised in that the high temperature is high
Pressure reactor includes kettle and the oil absorption material layer being arranged on inside kettle.
2. HTHP crude oil pyrolysis according to claim 1 is into gas analogue experiment installation, it is characterised in that the oil suction
Material layer is at least provided with one layer.
3. HTHP crude oil pyrolysis according to claim 1 is into gas analogue experiment installation, it is characterised in that the oil suction
The material of material layer is to be arranged on kettle by sintering or welding method with oil loving metal polyporous material, metal polyporous material
Internal cavity wall.
4. HTHP crude oil pyrolysis according to claim 1 or 2 or 3 is into gas analogue experiment installation, it is characterised in that institute
High-temperature high-pressure reaction kettle bottom entrance is stated high-temperature high-pressure reaction kettle is connected with suction line with bottom adapter.
5. HTHP crude oil pyrolysis according to claim 4 is into gas analogue experiment installation, it is characterised in that the high temperature
High-temperature high-pressure reaction kettle is connected by autoclave top export with kettle cover adapter with outlet line.
6. HTHP crude oil pyrolysis according to claim 5 is into gas analogue experiment installation, it is characterised in that the high temperature
Autoclave is placed in high-temperature heater.
7. HTHP crude oil pyrolysis according to claim 5 is into gas analogue experiment installation, it is characterised in that the entrance
On pipeline constant pressure pump, high-pressure water container, high pressure check valve have been sequentially connected in series by flow direction.
8. HTHP crude oil pyrolysis according to claim 5 is into gas analogue experiment installation, it is characterised in that the outlet
Worn successively by flow direction on pipeline and be connected to pressure gauge, overflow valve, air storage chamber, take air valve, the overflow valve connection pressure fine setting control
Pump processed, it is described to take air chamber bottom that discharging valve is set.
9. HTHP crude oil pyrolysis according to claim 5 is into gas analogue experiment installation, it is characterised in that the kettle
For high-temperature metal material, 500 DEG C of high temperature can be born, pressure 70MPa can be born；The metal polyporous material energy bearing temperature 500
℃；500 DEG C of bottom adapter and kettle cover adapter the energy bearing temperature.
10. HTHP crude oil pyrolysis according to claim 7 is into gas analogue experiment installation, it is characterised in that the height
Pressure check valve is connected between high-pressure water container and high-temperature high-pressure reaction kettle, and fluid internally can be from high-pressure water container to high temperature height
Reactor flowing is pressed, pressure 80MPa can be born.
11. HTHP crude oil pyrolysis according to claim 8 is into gas analogue experiment installation, it is characterised in that described to overflow
Stream valve is connected between autoclave outlet line and air storage chamber, 0~80MPa of pressure regulation spectrum.
12. HTHP crude oil pyrolysis according to claim 8 is into gas analogue experiment installation, it is characterised in that described micro-
Regulation and control pump discharge processed is connected to overflow valve, 0~80MPa of operating pressure, control accuracy ± 0.1MPa.
13. HTHP crude oil pyrolysis according to claim 8 is into gas analogue experiment installation, it is characterised in that the storage
Between air chamber is connected to overflow valve outlet and takes air valve, its underpart is discharging valve, air storage chamber pressure-bearing 80MPa.
14. HTHP crude oil pyrolysis is into gas analogue experiment method, its step：
Step 1, crude oil sample is loaded into high-temperature high-pressure reaction kettle；High-temperature high-pressure reaction kettle is inverted, in high-temperature high-pressure reaction kettle
Crude oil sample is loaded into high-temperature high-pressure reaction kettle at lower openings, loads onto bottom adapter and kettle cover adapter；Bottom is loaded onto to turn
The connection high pressure line of joint and kettle cover adapter；
Step 2, connect each part of experimental provision；High-temperature high-pressure reaction kettle is loaded into high-temperature heater；Connected with high pressure line permanent
Press pump, high-pressure water container, high pressure individual event valve, high-temperature high-pressure reaction kettle, pressure gauge, overflow valve, pressure vernier control pump, air storage chamber
With take air valve；
Step 3, device vacuumize；Close high pressure check valve and take air valve, open overflow valve and discharging valve；Vavuum pump is connected
Discharging valve outlet line is connected to, is vacuumized 5 minutes using vavuum pump；Close discharging valve；
Step 4, to high-temperature high-pressure reaction kettle pre-implant water；High pressure check valve is opened, using constant pressure pump by high-pressure water container
Water is injected into high-temperature high-pressure reaction kettle and connecting pipeline；
Step 5, reaction temperature and pressure condition are set；By setting high-temperature heater temperature setting high-temperature high-pressure reaction kettle
Analog temperature, to cause course of reaction reclaimed water to keep not gasifying in high-temperature high-pressure reaction kettle, reaction temperature is arranged on facing for water
Below boundary's temperature, i.e., less than 374.15 DEG C；Time mode is become using constant temperature to simulate the crude oil pyrolysis process of different evolution grades；
Reaction pressure is arranged on more than the liquid-vapor equilibrium pressure of water；Condition of formation pressure according to required for simulated experiment, pass through setting
The pressure of pressure vernier control pump sets reaction pressure of the spill pressure of overflow valve i.e. inside high-temperature high-pressure reaction kettle；Utilize
Constant pressure pump carries out ftercompction to high-temperature high-pressure reaction kettle inside, and the outlet pressure of constant pressure pump is set lower than the outlet pressure of overflow valve；
Step 6, constant temperature cracking；Crude oil collects the gas by overflow valve outflow when constant temperature Imitating is tested, with air storage chamber
Body, during collection, close the discharging valve of air storage chamber and take air valve；
Step 7, reactor is cooled down, collect gas；During crude oil pyrolysis to the predetermined reaction time, it is unidirectional to close constant pressure pump, high pressure
Valve and heating furnace, high-temperature high-pressure reaction kettle is progressively cooled to close to room temperature；Slowly until opening overflow valve completely, and open and take
Air valve；The gas of crude oil pyrolysis generation is collected, measures and carries out component analysis；
Step 8, carry out the crude oil pyrolysis experiment of next evolution grade；Repeat step five, step 6 and step 7, until complete
Crude oil pyrolysis into all time points is tested；
Step 9, cleaning device are simultaneously collected, measure residual crude oil；High-temperature high-voltage reaction is cleaned with highly polar low boiling point organic solvent
Kettle, each connection member and annexation, and cleaning fluid is collected, volatilize cleaning reagent, and measures reaction residual crude oil amount.
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