CN110749644A - Shale free oil analysis device - Google Patents

Shale free oil analysis device Download PDF

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Publication number
CN110749644A
CN110749644A CN201911231869.6A CN201911231869A CN110749644A CN 110749644 A CN110749644 A CN 110749644A CN 201911231869 A CN201911231869 A CN 201911231869A CN 110749644 A CN110749644 A CN 110749644A
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CN
China
Prior art keywords
shale
sample
component
free oil
oil analysis
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Pending
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CN201911231869.6A
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Chinese (zh)
Inventor
徐志尧
朱地
张焕旭
仰云峰
彭宇
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Suzhou Guande Energy Technology Co Ltd
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Suzhou Guande Energy Technology Co Ltd
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Priority to CN201911231869.6A priority Critical patent/CN110749644A/en
Publication of CN110749644A publication Critical patent/CN110749644A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
    • G01N27/626Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using heat to ionise a gas
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising

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  • Chemical & Material Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

The invention discloses a shale free oil analysis device which comprises a crushing component, a temperature control component and a signal detection processing component, wherein the crushing component is used for placing a shale sample and crushing the shale sample, the temperature control component is used for providing a specific temperature environment for the shale sample, and the signal detection processing component is used for detecting hydrocarbon substances escaping from the shale sample. Through the mode, the blocky shale sample is crushed into powder by using the high-hardness blade in the closed sample bin, so that the loss of hydrocarbons is reduced to the maximum extent, conditions are created for completely and accurately detecting the content of free oil, and meanwhile, gaseous hydrocarbons such as A, B, propane and the like and other hydrocarbons escape separately by using a low-temperature environment, so that the determination of gas-oil ratio (GOR) parameters of the shale sample can be realized, the evaluation of the oil-gas content of the shale is effectively realized, and the characterization parameters of the content of the free oil of the shale are obtained.

Description

Shale free oil analysis device
Technical Field
The invention relates to the technical field of geochemical analysis and test, in particular to a shale free oil analysis device.
Background
Increasingly demanding energyThe rising, the continuous consumption of the conventional oil gas resources and the contradiction between the global oil gas supply and demand are increasingly prominent, so that the unconventional oil gas resources are more and more emphasized. People gradually aim at shale oil under the inspiration of shale gas development and the regulation and control of natural gas price reduction. The research on the global shale oil is still in a starting stage, and the resource evaluation process is indispensable. In the shale oil evaluation process of the prior, the content of free oil is an important index of the oil-gas-bearing property of shale, and the content of free oil is generally characterized by pyrolysis parameters. The current general method for operating the pyrolysis of rock samples is influenced by a plurality of factors such as sample storage, transportation, grinding and the like, and the measured S0、S1The value is the residual content and does not directly indicate the original oil-gas-containing state, in particular S0The sample analysis value is small or even zero. But S0、S1The represented free oil content is a parameter which is crucial to evaluating the oil-gas content of shale, so the current rock pyrolysis technology cannot meet the requirement of shale oil exploration and development.
Disclosure of Invention
The invention mainly solves the technical problem of providing a shale free oil analysis device which can completely and accurately detect and analyze free oil of a shale sample and complete evaluation of oil-gas containing property of the shale sample.
In order to solve the technical problems, the invention adopts a technical scheme that: the shale free oil analysis device comprises a crushing component for placing and crushing a shale sample, a temperature control component for providing a specific temperature environment for the shale sample, and a signal detection processing component for detecting hydrocarbon substances escaping from the shale sample, wherein the temperature control component is positioned near the crushing component, and the crushing component is connected with the signal detection processing component.
The utility model provides a shale free oil analytical equipment, includes broken part, temperature control part, signal detection processing unit, broken part includes the sample storehouse, smashes part and first driver part, it is located to smash the part in the sample storehouse, first driver part with it connects to smash the part, temperature control part includes refrigeration part and heating part, refrigeration part is located in the sample storehouse or outside, heating part is located in the sample storehouse or outside, signal detection processing unit includes hydrogen flame ionization detection device, air supply and control unit, control unit with hydrogen flame ionization detection device connects, the air supply is to shale free oil analytical equipment air feed.
In a preferred embodiment of the present invention, the material of the sample chamber is stainless steel.
In a preferred embodiment of the present invention, the breaking component is a blade, and the blade is made of a high hardness alloy material.
In a preferred embodiment of the invention, the first drive member comprises a bearing and a motor, the motor and the breaking member being connected by the bearing.
In a preferred embodiment of the present invention, the bearing is a ceramic bearing, and the motor is a high-speed dc motor.
In a preferred embodiment of the present invention, the refrigeration component includes a semiconductor refrigeration sheet, a cold guide block and a heat sink, the semiconductor refrigeration sheet is disposed between the cold guide block and the heat sink, and the cold guide block is disposed adjacent to the wall of the sample chamber.
In a preferred embodiment of the present invention, the temperature control unit further comprises a second driving unit, and the second driving unit is connected with the refrigerating unit.
In a preferred embodiment of the present invention, the temperature control part further comprises a temperature sensor disposed in the sample chamber.
In a preferred embodiment of the present invention, the gas source is respectively connected to the hydrogen inlet of the hydrogen flame ionization detection device, the air inlet of the hydrogen flame ionization detection device, and the air inlet of the sample chamber.
The invention has the beneficial effects that: according to the shale free oil analysis device, the high-hardness blade is used in the closed sample bin to crush the blocky shale sample into powder, so that loss of hydrocarbons is reduced to the maximum extent, conditions are created for completely and accurately detecting the content of free oil, gaseous hydrocarbons such as A, B and propane and other hydrocarbons escape separately by using a low-temperature environment, the determination of gas-oil ratio (GOR) parameters of shale samples can be realized, the evaluation of the oil-gas content of shale is effectively realized, and the characterization parameters of the content of free oil of shale are obtained.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention will be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without inventive efforts, wherein:
FIG. 1 is a schematic structural diagram of a shale free oil analysis apparatus according to a preferred embodiment of the present invention;
the parts in the drawings are numbered as follows: 100-a crushing member; 200-a temperature control component; 300-signal detection processing means; 1-a sample bin; 2-a blade; 3-a bearing; 4-a motor; 5-semiconductor refrigerating sheet; 6-a cold conducting block; 7-a radiator; 8-an electric heating rod; 9-a temperature sensor; 10-hydrogen flame ionization detection device; 11-nitrogen source; 12-a source of hydrogen gas; 13-a source of air; 14-control means.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
To make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings, and it is apparent that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, a shale free oil analysis apparatus is provided, which includes a crushing unit 100, a temperature control unit 200, and a signal detection processing unit 300. The whole shale free oil analysis device works in a sealed environment. Broken part 100 includes sample storehouse 1, smashes part and first drive assembly, it is located to smash the part sample storehouse 1 is interior, first drive assembly with it connects to smash the part. The crushing member 100 is used for placing a rock sample, i.e. placing a rock sample in the sample chamber 1. The breaking member may be a blade 2. The first driving part comprises a bearing 3 and a motor 4, and the motor 4 is connected with the smashing part through the bearing 3. The first driving part is positioned at the lower part of the smashing part, the bearing 3 is integrated at the bottom of the sample bin 1, the blade 2 is arranged on the bearing 3, and the motor 4 drives the blade 2 to rotate through the bearing 3, so that the sample is smashed. The massive rock sample is broken into powder by the blade 2 in the sample chamber 1. The material of the sample bin 1 can be stainless steel material. The blade 2 may be made of a high-hardness alloy material, and specifically, SKD 11. The bearing can be a ceramic bearing, the motor can be a high-speed direct current motor, and the rotating speed of the direct current motor is 20000 revolutions per minute.
Temperature control unit 200 includes refrigeration part, heating unit, second driver part and temperature sensor 9, refrigeration part is located in the sample storehouse or outside, heating unit is located in the sample storehouse or outside. The temperature control component 200 is used to provide a specific temperature environment for the shale sample in the sample chamber 1. The refrigeration component comprises a semiconductor refrigeration piece 5, a cold guide block 6 and a radiator 7, the semiconductor refrigeration piece 5 is arranged between the cold guide block 6 and the radiator 7, and the cold guide block 6 is arranged adjacent to the wall of the sample bin 1. In this embodiment, the refrigeration component is located outside the sample compartment 1. The second driving part is connected with the refrigerating part and can drive the refrigerating part to move left and right, so that the cold guide block 6 is in contact with and separated from the sample bin 1, and the refrigerating effect is achieved. The heating component comprises an electric heating rod 8, the electric heating rod 8 is inserted into the wall of the sample chamber 1, and the temperature is conducted to the shale sample by heating the sample chamber 1. The temperature sensor 9 is arranged in the sample chamber 1, and the temperature sensor 9 is used for monitoring the temperature in the sample chamber 1.
The signal detection processing component 300 comprises the hydrogen flame ionization detection device 10, the gas source and control component 14, and the signal detection processing component 300 can be used for detecting and analyzing hydrocarbon substances escaping from the shale sample. And the gas source is respectively connected with a hydrogen inlet of the hydrogen flame ionization detection device, an air inlet of the hydrogen flame ionization detection device and an air inlet of the sample bin. The air supply includes nitrogen gas source 11, hydrogen gas source 12, air source 13, in this embodiment, nitrogen gas source 11 with the air inlet of sample storehouse 1 is connected, hydrogen gas source 12 with hydrogen flame ionization detection device 10's hydrogen inlet connection, air source 13 with hydrogen flame ionization detection device 10's air inlet connection. The control unit 14 is connected to the hydrogen flame ionization detection device 10. The control unit 14 may be an electronic computer, and the hydrogen flame ionization detection device 10 is a commercially available product, and this detection is also a detection method commonly used in this field. The control component 14 can control the operation of the first driving component and the second driving component, and the control component 14 can also control the refrigerating device and the heating device by reading the value of the temperature sensor 9, so as to control the temperature of the shale sample. The control unit 14 is also a commercially available product.
In particular, the temperature control unit 200 breaks the sample compartment 1When the crushed sample reaches a certain temperature, specific hydrocarbons are emitted from the shale sample in a gaseous state at a certain temperature, nitrogen in a nitrogen gas source 11 is taken as carrier gas and enters a sample bin 1, the hydrocarbon gas is replaced and enters a hydrogen flame ionization detection device 10 to detect signals, and a control part 14 processes the signals to obtain the content of the hydrocarbons emitted at a certain temperature, namely S0Or S1The value is obtained.
The specific operation of this embodiment is as follows:
the hydrogen gas source 12 and the air source 13 are opened, and the hydrogen flame ionization detection device 10 is controlled by the control component 14 to achieve a stable working state. The shale sample is placed in the sample bin 1, the control part 14 is used for controlling the refrigerating device, the temperature sensor 9 is enabled to reach-15-5 ℃, the motor 4 is started, the operation lasts for 3 minutes, and the sample is crushed into powder. Opening a nitrogen gas source 11, taking nitrogen as carrier gas to carry hydrocarbon gas in the sample bin 1 into the hydrogen flame ionization detection device 10, and obtaining a signal of the stage by a control part 14; the control part 14 is continuously used for controlling the heating device, so that the temperature sensor 9 reaches 90-100 ℃, nitrogen is continuously used as carrier gas to carry hydrocarbon gas escaped from the sample in the sample bin 1 at the temperature into the hydrogen flame ionization detection device 10, and the control part 14 obtains signals at the stage; and continuously using the control part 14 to control the heating device, enabling the temperature sensor 9 to reach 300-400 ℃, continuously using nitrogen as carrier gas to carry hydrocarbon gas escaped from the sample in the sample bin 1 at the temperature into the hydrogen flame ionization detection device 10, and obtaining a signal of the stage by the control part 14.
In addition, in the description of the embodiments of the present invention, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the several embodiments provided in the present application, it should be understood that the disclosed system, apparatus and method may be implemented in other ways. The above-described embodiments of the apparatus are merely illustrative, and for example, the division of the units is only one logical division, and there may be other divisions when actually implemented, and for example, a plurality of units or components may be combined or integrated into another system, or some features may be omitted, or not executed. In addition, the shown or discussed mutual coupling or direct coupling or communication connection may be an indirect coupling or communication connection of devices or units through some communication interfaces, and may be in an electrical, mechanical or other form.
The units described as separate parts may or may not be physically separate, and parts displayed as units may or may not be physical units, may be located in one place, or may be distributed on a plurality of network units. Some or all of the units can be selected according to actual needs to achieve the purpose of the solution of the embodiment.
In addition, functional units in the embodiments of the present invention may be integrated into one processing unit, or each unit may exist alone physically, or two or more units are integrated into one unit.
Finally, it should be noted that: the above-mentioned embodiments are only specific embodiments of the present invention, which are used for illustrating the technical solutions of the present invention and not for limiting the same, and the protection scope of the present invention is not limited thereto, although the present invention is described in detail with reference to the foregoing embodiments, those skilled in the art should understand that: any person skilled in the art can modify or easily conceive the technical solutions described in the foregoing embodiments or equivalent substitutes for some technical features within the technical scope of the present disclosure; such modifications, changes or substitutions do not depart from the spirit and scope of the embodiments of the present invention, and they should be construed as being included therein. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.

Claims (10)

1. The shale free oil analysis device is characterized by comprising a crushing component for placing and crushing a shale sample, a temperature control component for providing a specific temperature environment for the shale sample, and a signal detection processing component for detecting hydrocarbon substances escaping from the shale sample, wherein the temperature control component is positioned near the crushing component, and the crushing component is connected with the signal detection processing component.
2. The utility model provides a shale free oil analytical equipment, its characterized in that includes broken part, temperature control part, signal detection processing unit, broken part includes the sample storehouse, smashes part and first driver part, it is located to smash the part in the sample storehouse, first driver part with it connects to smash the part, temperature control part includes refrigeration part and heating part, refrigeration part is located in the sample storehouse or outside, heating part is located in the sample storehouse or outside, signal detection processing unit includes hydrogen flame ionization detection device, air supply and control unit, control unit with hydrogen flame ionization detection device connects, the air supply is to shale free oil analytical equipment air feed.
3. The shale free oil analysis apparatus of claim 2, wherein the sample bin is made of stainless steel.
4. The shale free oil analysis apparatus of claim 2, wherein the fragmentation component is a blade, and the blade is made of a high hardness alloy material.
5. The shale free oil analysis apparatus of claim 2, wherein the first drive component comprises a bearing and a motor, the motor and the fragmentation component being connected by the bearing.
6. The shale free oil analysis apparatus of claim 2, wherein the bearing is a ceramic bearing and the motor is a high speed dc motor.
7. The shale free oil analysis apparatus of claim 2, wherein the refrigeration component comprises a semiconductor refrigeration sheet, a cold conducting block and a heat sink, the semiconductor refrigeration sheet is disposed between the cold conducting block and the heat sink, and the cold conducting block is disposed adjacent to the sample bin wall.
8. The shale free oil analysis apparatus of claim 2, wherein the temperature control component further comprises a second drive component, the second drive component being connected with the refrigeration component.
9. The shale free oil analysis apparatus of claim 2, wherein the temperature control component further comprises a temperature sensor disposed within the sample bin.
10. The shale free oil analysis device of claim 2, wherein the gas source is connected with a hydrogen inlet of the hydrogen flame ionization detection device, an air inlet of the hydrogen flame ionization detection device, and an air inlet of the sample bin, respectively.
CN201911231869.6A 2019-12-05 2019-12-05 Shale free oil analysis device Pending CN110749644A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
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CN114428166A (en) * 2020-09-29 2022-05-03 中国石油化工股份有限公司 Method and system for evaluating oil-gas-containing property of stratum

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Publication number Priority date Publication date Assignee Title
CN114428166A (en) * 2020-09-29 2022-05-03 中国石油化工股份有限公司 Method and system for evaluating oil-gas-containing property of stratum
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Application publication date: 20200204