阅读说明：本技术 页岩流体饱和度测试装置及测试方法 (Shale fluid saturation testing device and testing method ) 是由 于振锋 乔晋 鲁博 郝春生 朱雷 姚立朋 宋新亚 魏若飞 郭振宇 云剑 于 2019-12-13 设计创作，主要内容包括：本申请公开一种页岩流体饱和度测试装置及测试方法,该测试装置包括：反应容器,所述反应容器内设有用于承载样品的承载部,所述承载部上设有通孔,用于流出所述样品产生的流体；用于对所述反应容器加热的加热组件,所述加热组件与所述反应容器相连；用于冷凝所述流体的冷凝组件,所述冷凝组件设于所述反应容器的下游；用于收集经所述冷凝组件冷凝后的流体的收集组件,所述收集组件位于所述冷凝组件的下游；所述收集组件设有用于计量流体体积的计量部。本申请所提供的页岩流体饱和度测试装置及测试方法,能精确测试页岩的流体饱和度,提高页岩油水饱和度测试数据的准确性。(The application discloses shale fluid saturation testing arrangement and test method, this testing arrangement includes: the device comprises a reaction container, a sample collecting device and a sample processing device, wherein a bearing part for bearing a sample is arranged in the reaction container, and a through hole is formed in the bearing part and is used for allowing fluid generated by the sample to flow out; the heating assembly is used for heating the reaction vessel and is connected with the reaction vessel; a condensing assembly for condensing the fluid, the condensing assembly being disposed downstream of the reaction vessel; a collection assembly for collecting fluid condensed by the condensing assembly, the collection assembly being located downstream of the condensing assembly; the collection assembly is provided with a metering portion for metering the volume of fluid. The shale fluid saturation testing device and the testing method provided by the application can be used for accurately testing the fluid saturation of shale and improving the accuracy of shale oil-water saturation testing data.)

1. A shale fluid saturation testing arrangement, characterized by includes:

the device comprises a reaction container, a sample collecting device and a sample processing device, wherein a bearing part for bearing a sample is arranged in the reaction container, and a through hole is formed in the bearing part and is used for allowing fluid generated by the sample to flow out;

the heating assembly is used for heating the reaction vessel and is connected with the reaction vessel;

a condensing assembly for condensing the fluid, the condensing assembly being disposed downstream of the reaction vessel;

a collection assembly for collecting fluid condensed by the condensing assembly, the collection assembly being located downstream of the condensing assembly; the collection assembly is provided with a metering portion for metering the volume of fluid.

2. The shale fluid saturation testing apparatus of claim 1, wherein the sample is granular; the reaction vessel is provided with a conical structure below the bearing part.

3. The shale fluid saturation testing apparatus of claim 1, wherein the reaction vessel is provided with an upper cover, and a sealing member is arranged between the upper cover and the reaction vessel; the reaction vessel is provided with a plurality of reaction vessels.

4. The shale fluid saturation testing apparatus of claim 1, wherein the carrier is mesh-shaped, and the diameter of the carrier through hole is smaller than the diameter of the sample.

5. The shale fluid saturation testing apparatus of claim 1, wherein the heating assembly comprises an incubator disposed outside the reaction vessel, a heating element and a temperature measuring element disposed within the incubator.

6. The shale fluid saturation testing apparatus of claim 1, wherein the heating assembly controls the temperature of the reaction vessel to be 121.11 ℃, 315.56 ℃, 704.44 ℃.

7. The shale fluid saturation testing apparatus of claim 1, wherein the condensing assembly comprises a condenser tube connected to the reaction vessel outlet, and a cooling tank disposed outside the condenser tube.

8. The shale fluid saturation testing apparatus of claim 1, wherein the collection assembly comprises a collection tube connected to the outlet of the condensing assembly, the metering portion comprises a camera imaging system facing the collection tube, the camera imaging system comprising a camera, a backlight, and a motor.

9. The shale fluid saturation testing apparatus of claim 1, further comprising a control assembly, the control assembly being electrically connected to the heating assembly and the metering portion.

10. The shale fluid saturation testing method is characterized by comprising the following steps of:

taking shale and measuring its total density rho₁Crushing shale to obtain a sample, and measuring the density rho of rock particles₂；

Measuring the mass m of a reaction vessel₁The sample is placed in a reaction vessel, and the mass m of the reaction vessel at that time is measured₂；

Opening a heating component connected with the reaction container to enable the fluid in the sample to flow out, enabling the fluid to flow into a collection component through a condensation component, enabling the collection component to utilize a metering part to measure the volume of the fluid, wherein the volume of water is V_wVolume of oil is V_o；

Calculating the water saturation, oil saturation, gas saturation of the sample according to the following formulas:

Technical Field

The application relates to the technical field of oil exploration, in particular to a shale fluid saturation testing device and a testing method.

Background

The fluid saturation is used for describing the degree of fluid filling in rock pores of the reservoir, and the parameter influences the size of reserves of the oil and gas reservoir and can be used for evaluating the advantages and disadvantages of the reservoir. When multiple fluids (crude oil, formation water, or natural gas) are present in the pores of a reservoir rock simultaneously, the volume percentage of a certain fluid is referred to as the saturation of that fluid.

The current testing method applied to the oil-water saturation of the conventional reservoir mainly comprises the following steps: distillation extraction, coulometry, immersion, etc.

The principle of the distillation extraction method is that weighed rock cores are placed in a core chamber, water in a rock sample is distilled by utilizing a solvent (such as toluene and the like) which has a boiling point higher than that of water, is insoluble in water, has a density lower than that of water and has a good oil washing effect, the rock sample is cleaned, dried and weighed, and the water content is subtracted from the mass difference before and after extraction to obtain the oil content. The method is suitable for testing the oil-water saturation of the rock sample with high permeability, and the measurement result of the method on the compact rock core is inaccurate.

The coulometry method is based on the principle that water in a rock sample with known mass is dissolved in quantitative ethanol by utilizing the characteristic of unlimited miscibility of water and ethanol, and then the water in an ethanol water solution is measured by using a trace moisture determinator.

The principle of the soaking method is similar to that of a coulometric method, a rock sample with known mass is soaked in quantitative ethanol at normal temperature, and the water content in the ethanol water solution is measured by a trace water content measuring instrument when the water content in the ethanol water solution is not changed any more.

However, the above methods must be used under certain conditions, reservoirs with different lithologies can only be applied to one or more analysis methods, and if the methods are selected improperly, the results of oil and water saturation tests may have larger errors.

Disclosure of Invention

In view of the defects of the prior art, one of the purposes of the present application is to provide a shale fluid saturation testing apparatus and a testing method, which can accurately test the fluid saturation of shale and improve the accuracy of shale oil-water saturation testing data.

In order to achieve the purpose, the technical scheme is as follows:

a shale fluid saturation testing apparatus, comprising:

the device comprises a reaction container, a sample collecting device and a sample processing device, wherein a bearing part for bearing a sample is arranged in the reaction container, and a through hole is formed in the bearing part and is used for allowing fluid generated by the sample to flow out;

the heating assembly is used for heating the reaction vessel and is connected with the reaction vessel;

a condensing assembly for condensing the fluid, the condensing assembly being disposed downstream of the reaction vessel;

a collection assembly for collecting fluid condensed by the condensing assembly, the collection assembly being located downstream of the condensing assembly; the collection assembly is provided with a metering portion for metering the volume of fluid.

As a preferred embodiment, the sample is in the form of particles; the reaction vessel is provided with a conical structure below the bearing part.

In a preferred embodiment, the reaction vessel is provided with an upper cover, and a sealing member is arranged between the upper cover and the reaction vessel; the reaction vessel is provided with a plurality of reaction vessels.

In a preferred embodiment, the carrier has a mesh shape, and the diameter of the through hole of the carrier is smaller than the diameter of the sample.

In a preferred embodiment, the heating unit includes an oven disposed outside the reaction vessel, a heating element disposed in the oven, and a temperature measuring element.

In a preferred embodiment, the heating module controls the temperature of the reaction vessel to 121.11 ℃, 315.56 ℃ and 704.44 ℃.

As a preferred embodiment, the condensation assembly comprises a condensation pipe connected with the outlet of the reaction vessel, and a cooling tank arranged outside the condensation pipe.

In a preferred embodiment, the collecting assembly includes a collecting pipe connected to the outlet of the condensing assembly, and the metering portion includes a camera imaging system facing the collecting pipe, the camera imaging system including a camera, a backlight, and a motor.

In a preferred embodiment, the apparatus further comprises a control unit electrically connected to the heating unit and the metering unit.

A shale fluid saturation testing method comprises the following steps:

taking shale and measuring its total density rho₁Crushing shale to obtain a sample, and measuring the density rho of rock particles₂；

Measuring the mass m of a reaction vessel₁The sample is placed in a reaction vessel, and the mass m of the reaction vessel at that time is measured₂；

Opening a heating component connected with the reaction container to enable the fluid in the sample to flow out, enabling the fluid to flow into a collection component through a condensation component, enabling the collection component to utilize a metering part to measure the volume of the fluid, wherein the volume of water is V_wVolume of oil is V_o；

Calculating the water saturation, oil saturation, gas saturation of the sample according to the following formulas:

has the advantages that:

the shale fluid saturation testing arrangement and the test method that this application embodiment provided through the bearing part that sets up the through-hole, make the fluid in the test procedure in the sample can flow, through setting up the condensation subassembly, make the steam in the reaction vessel change into liquid outflow into more accurately, make the data that record. Through the combined action of the reaction vessel, the heating assembly, the condensing assembly and the collecting assembly, oil and water contained in the shale are effectively metered.

The shale fluid saturation testing device provided by the embodiment of the application is simple in structure and convenient to assemble, and the shale fluid saturation testing method is simple, scientific and reasonable in steps, can accurately test the fluid saturation of shale, and improves the accuracy of shale oil water saturation testing data.

Specific embodiments of the present application are disclosed in detail with reference to the following description and drawings, indicating the manner in which the principles of the application may be employed. It should be understood that the embodiments of the present application are not so limited in scope.

Features that are described and/or illustrated with respect to one embodiment may be used in the same way or in a similar way in one or more other embodiments, in combination with or instead of the features of the other embodiments.

It should be emphasized that the term "comprises/comprising" when used herein, is taken to specify the presence of stated features, integers, steps or components but does not preclude the presence or addition of one or more other features, integers, steps or components.

Drawings

In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below, it is obvious that the drawings in the following description are only some embodiments of the present application, and for those skilled in the art, other drawings can be obtained according to the drawings without inventive exercise.

Fig. 1 is a schematic structural diagram of a shale fluid saturation testing apparatus provided in an embodiment of the present application;

FIG. 2 is a schematic diagram of a reaction vessel provided in an embodiment of the present application;

fig. 3 is a flowchart illustrating steps of a shale fluid saturation testing method according to an embodiment of the present disclosure.

Description of reference numerals:

1. a reaction vessel; 11. a tapered structure; 12. an upper cover; 13. a seal member; 14. a bearing part;

21. a thermostat; 22. a heating element; 23. a temperature measuring element; 24. a thermal insulation material;

31. a condenser tube; 32. a cooling tank;

41. a collection pipe; 42. a metering section;

5. and a control component.

Detailed Description

In order to make those skilled in the art better understand the technical solutions in the present application, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all of the 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 application.

It will be understood that when an element is referred to as being "disposed on" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may be present. The terms "vertical," "horizontal," "left," "right," and the like as used herein are for illustrative purposes only and do not represent the only embodiments.

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein in the description of the present application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.

For convenience of explanation, in this specification, an upward direction when the reader faces fig. 1 is defined as an upper side of the shale fluid saturation testing apparatus, and a downward direction when the reader faces fig. 1 is defined as a lower side of the shale fluid saturation testing apparatus.

Please refer to fig. 1. The embodiment of the application provides a shale fluid saturation testing arrangement, and this testing arrangement includes reaction vessel 1, heating element, condensation subassembly and collection subassembly.

Wherein, a bearing part 14 for bearing a sample is arranged in the reaction container 1. The carrier 14 is provided with a through hole for flowing out the fluid generated by the sample. The heating assembly is used for heating the reaction vessel 1. The heating assembly is connected to the reaction vessel 1. The condensing assembly is used for condensing the fluid. The condensing assembly is disposed downstream of the reaction vessel 1. The collection component is used for collecting the fluid condensed by the condensation component. The collection assembly is located downstream of the condensing assembly. The collection assembly is provided with a metering portion 42 for metering the volume of fluid.

The shale fluid saturation testing arrangement that this application embodiment provided is equipped with the bearing part 14 of through-hole through the setting, makes the fluid in the test procedure sample can flow, through setting up the condensation subassembly, makes the steam in the reaction vessel 1 change into liquid outflow into, makes the data that record more accurate. Through the combined action of the reaction vessel 1, the heating assembly, the condensing assembly and the collecting assembly, oil and water contained in the shale are effectively metered.

The shale fluid saturation testing device provided by the embodiment of the application has the advantages of simple structure and convenience in assembly, and can accurately test the fluid saturation of shale and improve the accuracy of shale oil-water saturation testing data.

The shape and size of the reaction vessel 1 are not particularly limited in the embodiments of the present application. Preferably, as shown in fig. 2, the reaction vessel 1 may be provided in a cylindrical shape. For example, the reaction vessel 1 may be cylindrical with an inner diameter of 35 mm. In order to better enable the fluid in the sample to flow out of the reaction container 1, the reaction container 1 is provided with a conical structure 11 below the bearing part 14. The diameter of the conical structure 11 decreases gradually from top to bottom.

In the present embodiment, as shown in fig. 2, the reaction vessel 1 is provided with an upper lid 12. A sealing member 13 is arranged between the upper cover 12 and the reaction vessel 1. The sealing member 13 may be a red copper gasket and a heat-resistant asbestos pad. The testing arrangement that this application embodiment provided can be equipped with a plurality ofly reaction vessel 1 to carry out the fluid saturation test to different samples simultaneously, improve work efficiency.

In the present embodiment, the bearing part 14 may be a net, which may be a stainless steel net. The diameter of the through hole of the bearing part 14 is smaller than that of the sample, so that the bearing part 14 can bear the sample and prevent the sample from falling off, and the through hole of the bearing part can enable the fluid in the sample to flow down. The sample in the embodiment of the application is crushed into particles, which is helpful for better extracting the oil and water in the sample.

In the present embodiment, the heating unit includes an oven 21 provided outside the reaction vessel 1, and a heating element 22 and a temperature measuring element 23 provided in the oven 21. The incubator 21 heats the reaction vessel 1 mainly by means of the heating element 22 and has a constant temperature effect. The wall surface of the oven 21 may be filled with a heat insulating material 24. The heating element 22 may be a heating tube arranged inside the incubator 21 in contact with the reaction vessel 1. The temperature measuring element 23 can be a temperature sensor, for example, a K-type thermocouple can be selected, and the temperature measuring precision reaches +/-0.5 ℃. The heating component can realize the control of the temperature of the reaction vessel 1 by combining the temperature measuring function of the temperature measuring element 23.

Specifically, the heating module can control the temperature of the reaction vessel 1 to be 121.11 ℃, 315.56 ℃ and 704.44 ℃. Of course, according to different testing requirements, the heating assembly may be adjusted to maintain the reaction vessel 1 at different temperatures, which is not limited in the embodiments of the present application.

In the present embodiment, the condensing assembly includes a condensing pipe 31 connected to the outlet of the reaction vessel 1, and a cooling tank 32 provided outside the condensing pipe 31. The condensing pipe 31 can cool the vapor and liquid products generated after the dry distillation of the sample. The cooling tank 32 is used for providing circulating cooling liquid to the condensation pipe 31 so as to rapidly cool the distilled vapor and liquid products. The cooling tank 32 can cool the condensation pipe 31 by means of a low-temperature thermostatic water bath.

In the present embodiment, the collection module comprises a collection tube 41 connected to the outlet of the condensation module. Specifically, the collecting pipe 41 is connected to an outlet of the condensing pipe 31. The metering portion 42 of the collection assembly may be a graduated line disposed on the collection tube 41.

In order to avoid errors in the manual readings and to make the fluid saturation more accurate, it is preferred that the metering section 42 comprises a camera imaging system facing the collection tube 41. The camera imaging system may include a camera, a backlight, and a motor.

Specifically, the change of the liquid level in the collection pipe 41 can be monitored by the camera, and the position information of the fluid interface can be directly converted into the volume of the fluid. The error precision is less than 0.05 ml. The camera may be a high resolution camera, for example, a 44-thousand pixel camera, with a measurement resolution of 0.02 mm, a minimum field of view of 10 mm, a volume measurement accuracy of 0.01 ml, and a volume measurement range of 100 ml. The camera can also distinguish whether it is oil or water according to the observed form of the liquid bead. Therefore, even if a liquid bead remains on the inner wall of the collection pipe 41, the camera imaging system can distinguish the property and the volume of the liquid bead through the camera, so that the measured fluid saturation is more accurate.

The backlight may be powered at 150 watts. The motor is preferably a high precision motor that is connected to a 230 volt ac power source at 50 or 60 hz.

In the embodiment of the present application, the testing device may further include a control assembly 5, and the control assembly 5 is electrically connected to the heating assembly and the metering portion 42. The control unit 5 may be a Personal Computer (PC), and the control unit 5 may be in other forms, and the present application is not limited thereto. For example, the control assembly 5 may include a control box and control circuitry. The control circuit may include elements such as a temperature secondary meter, a solid state relay, a power switch, and the like.

The control component 5 is electrically connected with the heating component, can control the on-off of the heating component, and can also obtain the real-time temperature of the reaction container 1. The control unit 5 is electrically connected to the measuring section 42, and can acquire data measured by the measuring section 42. The control component 5 can also be provided with a calculating part which can calculate the oil-water saturation of the shale sample according to the obtained data.

Please refer to fig. 3. The embodiment of the application also provides a shale fluid saturation testing method. The method comprises the following steps:

step S10: taking shale and measuring its total density rho₁Crushing shale to obtain a sample, and measuring the density rho of rock particles₂。

In this step, ρ₁Total density, p, calculated based on the Archimedes buoyancy principle₂Is the crystal grain density measured based on boyle's law. Rho₁And ρ₂Can be measured by a true densitometer. The true densitometer may be a true densitometer manufactured by SCAL 2010. The crushed shale particles may have a particle size of less than 0.154 mm, i.e., pass through a 100 mesh screen. The crushed shale particles need to be packaged and taken by a closed plastic packaging bag, and the next experiment is carried out in a short time. The time should be within half a day, and the crushed sample should be stored in the shade.

Step S20: measuring the mass m of a reaction vessel₁The sample is placed in a reaction vessel, and the mass m of the reaction vessel at that time is measured₂。

In this step, pass m₂And m₁The difference in the ratio can be used to obtain the quality of the sample. Therefore, the total volume measured based on the Archimedes buoyancy principle can be obtained

The volume of the crystal particles measured based on Boyle's law is

Step S30: opening a heating component connected with the reaction container to enable the fluid in the sample to flow out, enabling the fluid to flow into a collection component through a condensation component, enabling the collection component to utilize a metering part to measure the volume of the fluid, wherein the volume of water is V_wVolume of oil is V_o。

In this step, the sample may be retorted at a temperature sequence of 121.11 ℃, 315.56 ℃ and 704.44 ℃, the volumes of water and oil produced during each retorting are recorded and finally added to give a volume V of water contained in the sample_wVolume of oil is V_o。

Step S40: calculating the water saturation, oil saturation, gas saturation of the sample according to the following formulas:

in this step, a pore volume of

Effective pore volume

Porosity of gas containing

Effective porosity

In the formula rho₃Denotes the particle density, p, of the sample after the test experiment_oDenotes the density of the oil, p_wIndicating the density of the water.

Saturation of gas

The shale fluid saturation test method that this application embodiment provided through setting up the portion 14 that bears who is equipped with the through-hole, makes the fluid in the test procedure sample can flow, through setting up the condensation subassembly, makes the steam in the reaction vessel 1 change into liquid outflow more, makes the data that record more accurate. Through the combined action of the reaction vessel 1, the heating assembly, the condensing assembly and the collecting assembly, oil and water contained in the shale are effectively metered.

The shale fluid saturation testing method provided by the embodiment of the application is simple, scientific and reasonable in steps, can be used for accurately testing the fluid saturation of shale, and improves the accuracy of shale oil-water saturation testing data.

Any numerical value recited herein includes all values from the lower value to the upper value, in increments of one unit, provided that there is a separation of at least two units between any lower value and any higher value. For example, if it is stated that the number of a component or a value of a process variable (e.g., temperature, pressure, time, etc.) is from 1 to 90, preferably from 20 to 80, and more preferably from 30 to 70, it is intended that equivalents such as 15 to 85, 22 to 68, 43 to 51, 30 to 32 are also expressly enumerated in this specification. For values less than 1, one unit is suitably considered to be 0.0001, 0.001, 0.01, 0.1. These are only examples of what is intended to be explicitly recited, and all possible combinations of numerical values between the lowest value and the highest value that are explicitly recited in the specification in a similar manner are to be considered.

"plurality" means two or more unless otherwise specified. All ranges include the endpoints and all numbers between the endpoints. The use of "about" or "approximately" with a range applies to both endpoints of the range. Thus, "about 20 to about 30" is intended to cover "about 20 to about 30", including at least the endpoints specified.

All articles and references disclosed, including patent applications and publications, are hereby incorporated by reference for all purposes. The term "consisting essentially of …" describing a combination shall include the identified element, ingredient, component or step as well as other elements, ingredients, components or steps that do not materially affect the basic novel characteristics of the combination. The use of the terms "comprising" or "including" to describe combinations of elements, components, or steps herein also contemplates embodiments that consist essentially of such elements, components, or steps. By using the term "may" herein, it is intended to indicate that any of the described attributes that "may" include are optional.

A plurality of elements, components, parts or steps can be provided by a single integrated element, component, part or step. Alternatively, a single integrated element, component, part or step may be divided into separate plural elements, components, parts or steps. The disclosure of "a" or "an" to describe an element, ingredient, component or step is not intended to foreclose other elements, ingredients, components or steps.

It is to be understood that the above description is intended to be illustrative, and not restrictive. Many embodiments and many applications other than the examples provided will be apparent to those of skill in the art upon reading the above description. The scope of the present teachings should, therefore, be determined not with reference to the above description, but should instead be determined with reference to the appended claims, along with the full scope of equivalents to which such claims are entitled. The disclosures of all articles and references, including patent applications and publications, are hereby incorporated by reference for all purposes. The omission in the foregoing claims of any aspect of subject matter that is disclosed herein is not intended to forego such subject matter, nor should the inventors be construed as having contemplated such subject matter as being part of the disclosed subject matter.