CN114166680B - Device and method for measuring solid phase deposition amount of crude oil - Google Patents
Device and method for measuring solid phase deposition amount of crude oil Download PDFInfo
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- 239000010779 crude oil Substances 0.000 title claims abstract description 73
- 230000008021 deposition Effects 0.000 title claims abstract description 46
- 239000007790 solid phase Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 70
- 239000012528 membrane Substances 0.000 claims abstract description 27
- 238000001728 nano-filtration Methods 0.000 claims abstract description 27
- 238000007789 sealing Methods 0.000 claims abstract description 27
- 238000002347 injection Methods 0.000 claims abstract description 17
- 239000007924 injection Substances 0.000 claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 239000002184 metal Substances 0.000 claims abstract description 11
- 238000004891 communication Methods 0.000 claims description 43
- 238000005259 measurement Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 7
- 230000008859 change Effects 0.000 claims description 5
- 239000011148 porous material Substances 0.000 claims description 5
- 239000003921 oil Substances 0.000 abstract description 6
- 238000011161 development Methods 0.000 abstract description 4
- 238000002474 experimental method Methods 0.000 abstract description 4
- 230000003993 interaction Effects 0.000 abstract description 2
- 230000009471 action Effects 0.000 description 6
- 238000001556 precipitation Methods 0.000 description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000006073 displacement reaction Methods 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000012067 mathematical method Methods 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011158 quantitative evaluation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/02—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by absorbing or adsorbing components of a material and determining change of weight of the adsorbent, e.g. determining moisture content
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Abstract
The invention belongs to the technical field of oil and gas field development experiments, and discloses a device and a method for measuring solid phase deposition of crude oil. The device comprises a vacuumizing system, an intermediate container, an injection pump, a reaction container, a liquid collector and a temperature control system; the upper part of the reaction container is provided with a sealing cover, the sealing cover is provided with two inlets, one inlet is connected with the outlet of the intermediate container, and the other inlet is connected with the vacuumizing system; the bottom of the reaction container is provided with a groove; the lower part of the groove is connected with the liquid collector; the groove is internally provided with the following components from top to bottom: the device comprises a through hole bolt, a sealing ring, a nanofiltration membrane and a metal screen; the injection pump is connected with the inlet of the intermediate container; the temperature control system is used for controlling the temperature of the intermediate container and the reaction container. The invention can be used for quantitatively determining the solid phase deposition amount caused by the interaction of CO 2 and crude oil under different pressures through indoor experiments.
Description
Technical Field
The invention belongs to the technical field of oil and gas field development experiments, and particularly relates to a device and a method for measuring solid phase deposition of crude oil.
Background
Along with the maturation of CO 2 oil displacement technology, CO 2 injection has become an important technical measure for improving the development effect and the crude oil recovery ratio of oil fields. However, in the CO 2 flooding process, heavy organic matters such as asphaltene, colloid and paraffin in crude oil are easy to deposit due to the change of reservoir pressure and the extraction effect of CO 2 on the crude oil. Such solid phase deposition can severely impact reservoir permeability and porosity, reducing development effectiveness. Therefore, quantitative evaluation of crude oil solid phase deposition under the action of carbon dioxide is necessary, which is helpful for revealing key factors restricting the supercritical CO 2 flooding effect of the tight sandstone reservoir and providing theoretical guidance for improving the CO 2 flooding effect.
In the existing research, CN207144926U and CN107288615A propose a laser solid-phase deposition instrument and a testing method thereof, which are used for qualitatively judging whether solid-phase deposition exists in crude oil or not by a light transmission method, and can not quantitatively evaluate the solid-phase deposition amount; CN202383131U proposes a crude oil asphaltene deposition high-pressure simulation tester, which collects crude oil filtrate through a sampling tube, analyzes the oil sample, and calculates asphaltene deposition amount. CN107219322a proposes an experimental device for dynamically determining the amount of asphaltene precipitation generated by CO 2 -crude oil action, which adopts image analysis software to determine the area of asphaltene precipitation and the size distribution of particles, thereby obtaining the precipitation amount. CN103308667a proposes a method for measuring crude oil asphaltene precipitation during carbon dioxide immiscible phase flooding in an oil-containing core, which is to purify asphaltene from reservoir fluid produced after displacement, and calculate asphaltene content in a displacement product; zhang Wei et al, in the study of ultrasonic determination of solid deposition points, propose an ultrasonic method to qualitatively determine the solid deposition points. CN107209166a and literature, "prediction of asphaltene precipitation during CO 2 injection" use mathematical methods to predict the amount of asphaltene precipitation.
The above-mentioned various measurement methods in the prior art have insufficient accuracy and efficiency, and therefore, it is necessary to provide a device and a method for rapidly, efficiently and accurately measuring the solid phase deposition amount of crude oil.
Disclosure of Invention
The invention aims at overcoming the defects of the prior art and provides a device and a method for measuring the solid phase deposition amount of crude oil. The invention can quantitatively determine the solid phase deposition amount of crude oil under the action of CO 2 with different pressures, and the determination method is simple and direct.
In order to achieve the above object, the present invention provides, in one aspect, an apparatus for determining solid phase deposition amount of crude oil, the apparatus comprising a vacuum pumping system, an intermediate container, an injection pump, a reaction container, a liquid collector, and a temperature control system, wherein:
The upper part of the reaction container is provided with a sealing cover, the sealing cover is provided with two inlets, one inlet is connected with the outlet of the intermediate container through a first communication valve, and the other inlet is connected with the vacuumizing system through a second communication valve;
the bottom of the reaction container is provided with a groove; the groove is connected with the liquid collector through a third communication valve; the groove is internally provided with the following components from top to bottom: the device comprises a through hole bolt, a sealing ring, a nanofiltration membrane and a metal screen;
the injection pump is connected with the inlet at the lower end of the intermediate container;
the temperature control system is used for controlling the temperature of the intermediate container and the reaction container.
In another aspect, the present invention provides a method for determining the solid phase deposition of crude oil, the method using the device for determining the solid phase deposition of crude oil, comprising the steps of:
S1: closing the first communication valve and the third communication valve, opening the second communication valve, vacuumizing the reaction vessel through the vacuum system, closing the second communication valve, injecting the crude oil into the intermediate vessel, and heating the intermediate vessel and the reaction vessel to a measured temperature through the temperature control system;
S2: inverting the reaction container, positioning the sealing cover below, opening a first communication valve, injecting heated crude oil into the reaction container through the injection pump, and closing the first communication valve; replacing residual crude oil in an intermediate container with CO 2 gas, heating the CO 2 gas in the intermediate container to a measured temperature, then injecting the heated gas into the reaction container to a measured pressure, and standing the reaction container to fully react the crude oil with CO 2 gas;
S3: inverting the reaction vessel back to an initial state; opening a third communication valve to collect crude oil flowing out of the reaction vessel; after the crude oil is collected, taking out the nanofiltration membrane from the reaction vessel, airing and measuring the weight;
S4: and calculating to obtain the solid phase deposition amount of the crude oil at the measuring temperature and the measuring pressure according to the weight change of the nanofiltration membrane before and after the measurement.
The invention has the following beneficial effects:
(1) The invention can be used for quantitatively determining the solid phase deposition amount caused by the interaction of CO 2 and crude oil under different pressures by an indoor experiment, and the testing method is simple, direct, quick, efficient and accurate.
(2) The method and the device can be applied to indoor CO 2 flooding and recovery efficiency improvement mechanism evaluation, can quantitatively determine the solid phase deposition amount of crude oil under the action of CO 2, and have important significance for on-site CO 2 flooding scheme formulation.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Drawings
The foregoing and other objects, features and advantages of the invention will be apparent from the following more particular descriptions of exemplary embodiments of the invention as illustrated in the accompanying drawings wherein like reference numbers generally represent like parts throughout the exemplary embodiments of the invention.
FIG. 1 shows a schematic diagram of an apparatus for measuring the solid phase deposition amount of crude oil according to the present invention.
Reference numerals illustrate:
The device comprises an injection pump 1, an intermediate container 2, a first communication valve 3, a reaction container 4, a through hole bolt 5, a sealing ring 6, a nanofiltration membrane 7, a metal screen 8, a third communication valve 9, a liquid collector 10, a second communication valve 11, a vacuumizing system 12 and a temperature control system 13.
Detailed Description
Preferred embodiments of the present invention will be described in more detail below. While the preferred embodiments of the present invention are described below, it should be understood that the present invention may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
In one aspect, the invention provides a device for determining solid phase deposition of crude oil, the device comprising a vacuum pumping system, an intermediate container, an injection pump, a reaction container, a liquid collector and a temperature control system, wherein:
The upper part of the reaction container is provided with a sealing cover, the sealing cover is provided with two inlets, one inlet is connected with the outlet of the intermediate container through a first communication valve, and the other inlet is connected with the vacuumizing system through a second communication valve;
the bottom of the reaction container is provided with a groove; the groove is connected with the liquid collector through a third communication valve; the groove is internally provided with the following components from top to bottom: the device comprises a through hole bolt, a sealing ring, a nanofiltration membrane and a metal screen;
the injection pump is connected with the inlet at the lower end of the intermediate container;
the temperature control system is used for controlling the temperature of the intermediate container and the reaction container.
According to the invention, preferably, the bottom of the reaction vessel is in a cone structure, so that crude oil flowing out of the reaction vessel can completely flow out.
According to the present invention, preferably,
The lower surface of the head of the through hole bolt is contacted with the upper surface of the sealing ring, or
The lower surface of the bottom of the screw rod of the through hole bolt is contacted with the upper surface of the sealing ring.
According to the present invention, preferably, the metal screen has a pore size of 50 to 100 μm.
According to the invention, preferably the nanofiltration membrane is sized to fit the recess.
According to the present invention, it is preferable that the nanofiltration membrane has a pore size of 0.5 to 5 μm.
In the invention, the through hole bolt and the sealing ring are used for preventing crude oil flowing out of the reaction container from flowing through a place except the nanofiltration membrane; the metal screen is used for supporting the nanofiltration membrane.
In another aspect, the present invention provides a method for determining the solid phase deposition of crude oil, the method using the device for determining the solid phase deposition of crude oil, comprising the steps of:
S1: closing the first communication valve and the third communication valve, opening the second communication valve, vacuumizing the reaction vessel through the vacuum system, closing the second communication valve, injecting the crude oil into the intermediate vessel, and heating the intermediate vessel and the reaction vessel to a measured temperature through the temperature control system;
S2: inverting the reaction container, positioning the sealing cover below, opening a first communication valve, injecting heated crude oil into the reaction container through the injection pump, and closing the first communication valve; replacing residual crude oil in an intermediate container with CO 2 gas, heating the CO 2 gas in the intermediate container to a measured temperature, then injecting the heated gas into the reaction container to a measured pressure, and standing the reaction container to fully react the crude oil with CO 2 gas;
S3: inverting the reaction vessel back to an initial state; opening a third communication valve to collect crude oil flowing out of the reaction vessel; after the crude oil is collected, taking out the nanofiltration membrane from the reaction vessel, airing and measuring the weight;
S4: and calculating to obtain the solid phase deposition amount of the crude oil at the measuring temperature and the measuring pressure according to the weight change of the nanofiltration membrane before and after the measurement.
According to the present invention, preferably, the pressure in the reaction vessel is-0.1 to-0.15 MPa after the reaction vessel is evacuated by the vacuum system.
The pressures in the invention are gauge pressures.
According to the invention, preferably, the time of rest is not less than 48 hours.
According to the invention, the nanofiltration membrane is preferably weighed to be m 0, the weight measured in step S3 is m 1, and the crude oil solid phase deposition amount is m d＝m1-m0.
An apparatus and method for measuring solid phase deposition amount of crude oil according to the present invention will be described in detail with reference to FIG. 1.
Example 1
The present embodiment provides an apparatus for measuring solid phase deposition amount of crude oil, as shown in fig. 1, which comprises a vacuum pumping system 12, an intermediate container 2, an injection pump 1, a reaction container 4, a liquid collector 10 and a temperature control system 13, wherein:
The upper part of the reaction vessel 4 is provided with a sealing cover, the sealing cover is provided with two inlets, one inlet is connected with the outlet of the intermediate vessel 2 through a first communication valve 3, and the other inlet is connected with the vacuumizing system 12 through a second communication valve 11;
The bottom of the reaction container 4 is of a cone structure, and a groove is arranged at the bottom of the reaction container 4 and is connected with the liquid collector 10 through a third communication valve 9; the groove is internally provided with the following components from top to bottom: the device comprises a through hole bolt 5, a sealing ring 6, a nanofiltration membrane 7 and a metal screen 8; wherein the lower surface of the bottom of the screw of the through hole bolt 5 is contacted with the upper surface of the sealing ring 6; the aperture of the metal screen 8 is 60 mu m; the size of the nanofiltration membrane 7 is adapted to the grooves, the pore size of the nanofiltration membrane 7 being 1 μm. The through-hole bolt 5 and the sealing ring 6 are used for preventing crude oil flowing out of the reaction vessel 4 from flowing through a place except the nano-filtration membrane 7; the metal screen 8 is used to support the nanofiltration membrane 7.
The injection pump 1 is connected with the inlet of the lower end of the intermediate container 2;
the temperature control system 13 is used to control the temperature of the intermediate vessel 2 and the reaction vessel 4.
Example 2
This example provides a method for determining the amount of solid phase deposition of crude oil using the apparatus for determining the amount of solid phase deposition of crude oil described in example 1.
The nanofiltration membrane was weighed before measurement, in m 0,m0 = 0.01g; the measurement temperature used in this example was 80 ℃; the measurement pressure used in this example was 20MPa.
The method comprises the following steps:
S1: closing the first communication valve 3 and the third communication valve 9, opening the second communication valve 11, vacuumizing the reaction vessel 4 to a pressure of-0.1 MPa in the reaction vessel 4 through the vacuum system 12, then closing the second communication valve 11, injecting the crude oil into the intermediate vessel 2, and heating the intermediate vessel 2 and the reaction vessel 4 to a measured temperature through the temperature control system 13;
S2: inverting the reaction vessel 4 so that the sealing cover is positioned below, opening the first communication valve 3, injecting 10mL of heated crude oil into the reaction vessel 4 by the injection pump, and closing the first communication valve 3; the residual crude oil in the intermediate container 2 is replaced by CO 2 gas, the CO 2 gas is heated to 80 ℃ in the intermediate container 2 and then is slowly injected into the reaction container 4 until the reaction container 4 reaches the measured pressure of 20MPa, and the reaction container is kept stand for more than 48 hours, so that the crude oil and CO 2 gas fully act.
S3: inverting the reaction vessel 4 back to the original state; opening a third communication valve 9, and collecting crude oil flowing out of the reaction vessel 4 under the action of CO 2 pressure; after the crude oil is collected, taking the nanofiltration membrane out of the reaction vessel 4, airing, and measuring the weight m 1 =0.15 g;
S4: according to the weight change of the nanofiltration membrane before and after the measurement, the measurement temperature is 80 ℃ and the measurement pressure is 20MPa, and the crude oil solid phase deposition amount m d is m 1-m0 =0.14 g under the action of the pressure of CO 2.
The foregoing description of embodiments of the invention has been presented for purposes of illustration and description, and is not intended to be exhaustive or limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the various embodiments described.
Claims (9)
1. A method for measuring the solid phase deposition of crude oil, which is characterized in that the device for measuring the solid phase deposition of crude oil adopted by the method comprises a vacuumizing system, an intermediate container, an injection pump, a reaction container, a liquid collector and a temperature control system, wherein:
The upper part of the reaction container is provided with a sealing cover, the sealing cover is provided with two inlets, one inlet is connected with the outlet of the intermediate container through a first communication valve, and the other inlet is connected with the vacuumizing system through a second communication valve;
the bottom of the reaction container is provided with a groove; the groove is connected with the liquid collector through a third communication valve; the groove is internally provided with the following components from top to bottom: the device comprises a through hole bolt, a sealing ring, a nanofiltration membrane and a metal screen;
the injection pump is connected with the inlet at the lower end of the intermediate container;
The temperature control system is used for controlling the temperatures of the intermediate container and the reaction container;
The method comprises the following steps:
S1: closing the first communication valve and the third communication valve, opening the second communication valve, vacuumizing the reaction vessel through the vacuum system, closing the second communication valve, injecting the crude oil into the intermediate vessel, and heating the intermediate vessel and the reaction vessel to a measured temperature through the temperature control system;
S2: inverting the reaction container, positioning the sealing cover below, opening a first communication valve, injecting heated crude oil into the reaction container through the injection pump, and closing the first communication valve; replacing residual crude oil in an intermediate container with CO 2 gas, heating the CO 2 gas in the intermediate container to a measured temperature, injecting the heated gas into the reaction container until the reaction container reaches a measured pressure, and standing the reaction container to fully react the crude oil with CO 2 gas;
S3: inverting the reaction vessel back to an initial state; opening a third communication valve to collect crude oil flowing out of the reaction vessel; after the crude oil is collected, taking out the nanofiltration membrane from the reaction vessel, airing and measuring the weight;
S4: and calculating to obtain the solid phase deposition amount of the crude oil at the measuring temperature and the measuring pressure according to the weight change of the nanofiltration membrane before and after the measurement.
2. The method for determining solid phase deposition of crude oil according to claim 1, wherein the bottom of the reaction vessel has a cone structure.
3. The method for determining solid phase deposition amount of crude oil according to claim 1, wherein,
The lower surface of the head of the through hole bolt is contacted with the upper surface of the sealing ring, or
The lower surface of the bottom of the screw rod of the through hole bolt is contacted with the upper surface of the sealing ring.
4. The method for determining solid phase deposition amount of crude oil according to claim 1, wherein the pore diameter of the metal screen is 50-100 μm.
5. The method for determining the amount of solid phase deposition of crude oil according to claim 1, wherein the nanofiltration membrane is sized to fit within the recess.
6. The method for determining solid phase deposition amount of crude oil according to claim 1, wherein the pore size of the nanofiltration membrane is 0.5-5 μm.
7. The method for determining solid phase deposition amount of crude oil according to claim 1, wherein in step S1, after the reaction vessel is evacuated by the vacuum system, the pressure in the reaction vessel is-0.1 to-0.15 MPa.
8. The method for determining solid phase deposition amount of crude oil according to claim 1, wherein in the step S2, the standing time is not less than 48 hours.
9. The method for determining solid phase deposition of crude oil according to claim 1, wherein the nanofiltration membrane is weighed to be m 0 before the determination, the weight determined in step S3 is m 1, and the solid phase deposition of crude oil is m d＝m1-m0.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0761276A2 (en) * | 1995-09-02 | 1997-03-12 | Kodak Limited | Apparatus for separating effluent into solid and liquid phases |
| DE102006060107A1 (en) * | 2006-12-08 | 2008-06-12 | Westfalia Separator Ag | Method for separation of solids from fluid product, involves passing of solids in solid bowl centrifuge and its purification by membrane filtration device |
| KR101532586B1 (en) * | 2015-01-16 | 2015-06-30 | 이상호 | Solid Phase Extraction Device |
| CN111189736A (en) * | 2020-02-17 | 2020-05-22 | 中海油能源发展股份有限公司工程技术分公司 | High-temperature high-pressure fluid solid phase deposition simulation device |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106761498B (en) * | 2016-12-20 | 2018-11-30 | 中国科学院广州能源研究所 | A kind of experimental provision and method for gas hydrates drilling fluid progress multi-phase separation |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0761276A2 (en) * | 1995-09-02 | 1997-03-12 | Kodak Limited | Apparatus for separating effluent into solid and liquid phases |
| DE102006060107A1 (en) * | 2006-12-08 | 2008-06-12 | Westfalia Separator Ag | Method for separation of solids from fluid product, involves passing of solids in solid bowl centrifuge and its purification by membrane filtration device |
| KR101532586B1 (en) * | 2015-01-16 | 2015-06-30 | 이상호 | Solid Phase Extraction Device |
| CN111189736A (en) * | 2020-02-17 | 2020-05-22 | 中海油能源发展股份有限公司工程技术分公司 | High-temperature high-pressure fluid solid phase deposition simulation device |
Non-Patent Citations (1)
| Title |
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| HQ油藏烟道气驱固相沉积试验研究;秦松涛;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑(月刊)》;第36-37页 * |
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