CN115582085A - System and method for preparing supercritical multi-element thermal fluid in laboratory - Google Patents
System and method for preparing supercritical multi-element thermal fluid in laboratory Download PDFInfo
- Publication number
- CN115582085A CN115582085A CN202211135767.6A CN202211135767A CN115582085A CN 115582085 A CN115582085 A CN 115582085A CN 202211135767 A CN202211135767 A CN 202211135767A CN 115582085 A CN115582085 A CN 115582085A
- Authority
- CN
- China
- Prior art keywords
- pressure
- thermal fluid
- temperature
- reaction
- supercritical
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000012530 fluid Substances 0.000 title claims abstract description 111
- 238000000034 method Methods 0.000 title claims abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 145
- 239000002994 raw material Substances 0.000 claims abstract description 30
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000001301 oxygen Substances 0.000 claims abstract description 27
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 27
- 238000005070 sampling Methods 0.000 claims abstract description 25
- 238000004458 analytical method Methods 0.000 claims abstract description 21
- 238000012360 testing method Methods 0.000 claims abstract description 15
- 239000000047 product Substances 0.000 claims abstract description 14
- 239000012263 liquid product Substances 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 44
- 229910052757 nitrogen Inorganic materials 0.000 claims description 22
- 238000002474 experimental method Methods 0.000 claims description 18
- 238000002360 preparation method Methods 0.000 claims description 12
- 238000013461 design Methods 0.000 claims description 9
- 239000000523 sample Substances 0.000 claims description 5
- 230000008878 coupling Effects 0.000 claims description 3
- 238000010168 coupling process Methods 0.000 claims description 3
- 238000005859 coupling reaction Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 239000000295 fuel oil Substances 0.000 abstract description 11
- 238000011161 development Methods 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 7
- 238000005516 engineering process Methods 0.000 abstract description 7
- 238000002347 injection Methods 0.000 abstract description 5
- 239000007924 injection Substances 0.000 abstract description 5
- 238000007405 data analysis Methods 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 28
- 239000002283 diesel fuel Substances 0.000 description 16
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 10
- 239000003921 oil Substances 0.000 description 10
- 230000035484 reaction time Effects 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000013401 experimental design Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
- B01J19/20—Stationary reactors having moving elements inside in the form of helices, e.g. screw reactors
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention discloses a system and a method for preparing supercritical multi-element thermal fluid in a laboratory. The system of the present invention comprises: high temperature high pressure batch autoclave, and 2 middle containers, sampling bag, computer and a test tube connected to high temperature high pressure batch autoclave respectively. The method comprises the following steps: adding reaction raw materials into a high-temperature high-pressure reaction kettle; and then heating and pressurizing to a supercritical state, introducing oxygen, reacting to generate supercritical multi-element thermal fluid, simultaneously recording temperature and pressure data in the reaction by a computer, collecting liquid products after the reaction by a test tube, and collecting gaseous products after the reaction by a sampling bag. The reaction heat release and carrying capacity of the supercritical multi-element thermal fluid is obtained through component analysis and experimental data analysis of the prepared supercritical multi-element thermal fluid. The invention effectively improves the application effect of the supercritical multi-element thermal fluid injection technology in the heavy oil reservoir, and the analysis result can be used as a reference for technicians in the heavy oil reservoir development field.
Description
Technical Field
The invention belongs to the technical field of offshore heavy oil thermal recovery, and relates to a system and a method for preparing supercritical multi-element thermal fluid in a laboratory.
Background
Heavy oil is an important petroleum resource and is widely distributed worldwide. With the continuous increase of the demand for petroleum, the development of thickened oil in China is gradually increased. The supercritical multi-element thermal fluid has the characteristics of high dissolution, high diffusion, high reaction and the like, and in order to improve the development effect of offshore thick oil, the technology for exploiting thick oil by injecting the supercritical multi-element thermal fluid is proposed and rapidly develops application research in recent years, so that a certain foundation is laid for the application of mines.
When the supercritical multi-element thermal fluid injection technology is used for offshore heavy oil exploitation, the heating effect of the supercritical multi-element thermal fluid on a reservoir stratum is an important factor influencing the heavy oil exploitation effect, and when the proportion of each component in the supercritical multi-element thermal fluid and the temperature and pressure condition are changed, the reaction heat release capacity and the heat carrying capacity of the supercritical multi-element thermal fluid are also changed, so that the application effect of the supercritical multi-element thermal fluid injection technology is influenced. Therefore, before the heavy oil development is carried out by applying the supercritical multi-element thermal fluid injection technology, if the supercritical multi-element thermal fluid under different raw material proportions and different temperature and pressure conditions can be prepared by a certain method, and the reaction heat release and heat carrying capacity of the supercritical multi-element thermal fluid are analyzed and optimized, the application effect of the technology in a heavy oil reservoir can be effectively improved. Therefore, a research method capable of preparing supercritical multi-element thermal fluid under different raw material proportions and different temperature and pressure conditions and analyzing reaction heat release and heat carrying capacity of the supercritical multi-element thermal fluid in a laboratory is needed.
Disclosure of Invention
The invention aims to provide a system and a method for preparing supercritical multi-element hot fluid in a laboratory.
The supercritical multi-element thermal fluid can be conveniently prepared under laboratory conditions, and the supercritical multi-element thermal fluid under different temperature and pressure conditions and different component proportions can be prepared by controlling the raw material proportion and the temperature and pressure conditions of the reaction kettle in the experimental process. After the experiment is finished, components of the produced supercritical multi-element thermal fluid are determined by using a chromatograph, and reaction heat release and heat carrying capacity of the supercritical multi-element thermal fluid prepared under different raw material proportions and different temperature and pressure conditions can be further analyzed by combining temperature and pressure data of a reaction kettle recorded in the preparation process, so that the feeding proportion and the temperature and pressure conditions in the supercritical multi-element thermal fluid preparation process are optimized, and an analysis result can be used as a technical worker for referring to a heavy oil reservoir development field.
The invention provides a system for preparing supercritical multi-element thermal fluid in a laboratory, which comprises:
the device comprises a high-temperature high-pressure reaction kettle, and 2 intermediate containers, a sampling bag, a computer and a test tube which are respectively connected to the high-temperature high-pressure reaction kettle;
a one-way valve is arranged on a pipeline between the 2 intermediate containers and the high-temperature high-pressure reaction kettle; the 2 intermediate containers are all driven by a high-precision constant-pressure constant-flow pump;
the sampling bag controls outlet pressure through a hand pump, and a back pressure valve is arranged between the sampling bag and the hand pump;
a temperature and pressure probe is arranged on a pipeline between the computer and the high-temperature high-pressure reaction kettle;
all through the tube coupling between the above-mentioned part, and all set up the valve on the pipeline.
In the invention, the high-temperature high-pressure reaction kettle is used for controlling temperature and pressure conditions to prepare supercritical multi-element hot fluid; the test tube is used for collecting liquid products after reaction;
the 2 intermediate containers are respectively used for providing oxygen and nitrogen;
the sampling bag is used for collecting gaseous products after reaction;
and the computer is used for recording the temperature and pressure data of the reaction process in the high-temperature high-pressure reaction kettle.
In the system for preparing the supercritical multi-component thermal fluid in the laboratory, the system for preparing the supercritical multi-component thermal fluid in the laboratory further comprises a chromatograph for analyzing the components of the supercritical multi-component thermal fluid.
In the invention, raw materials (including oil and water) and nitrogen are controlled to be introduced into the high-temperature high-pressure reaction kettle, the raw materials and the nitrogen are heated and pressurized to be prepared into a supercritical state, then oxygen is introduced into the high-temperature high-pressure reaction kettle for reaction to generate the supercritical multi-element thermal fluid.
The invention also provides a method for preparing supercritical multi-element thermal fluid in a laboratory by adopting the system for preparing supercritical multi-element thermal fluid in the laboratory, which comprises the following steps:
adding reaction raw materials (comprising oil and water) into the high-temperature high-pressure reaction kettle before the experiment; and then introducing nitrogen into the high-temperature high-pressure reaction kettle through 1 intermediate container, heating and pressurizing to a supercritical state after the pressure is raised to a design pressure, introducing oxygen into the high-temperature high-pressure reaction kettle through the other 1 intermediate container, controlling the ratio of the raw materials to the oxygen and the temperature and pressure conditions in the high-temperature high-pressure reaction kettle to react to generate supercritical multi-element thermal fluid, recording temperature and pressure data in the reaction by the computer, collecting liquid products after the reaction by the test tube, and collecting gaseous products after the reaction by the sampling bag.
In the invention, the nitrogen is introduced to determine the sealing property of the high-temperature high-pressure reaction kettle and remove air in the high-temperature high-pressure reaction kettle, and the nitrogen is continuously introduced to the required design pressure.
The invention further provides a method for preparing supercritical multi-element thermal fluid in a laboratory and analyzing the reaction heat release and heat carrying capacity of the supercritical multi-element thermal fluid, which comprises the following steps:
(1) The system for preparing supercritical multi-element hot fluid in laboratory is adopted to prepare supercritical multi-element hot fluid
Adding reaction raw materials (oil and water) into the high-temperature high-pressure reaction kettle before the beginning of the experiment; then introducing nitrogen into the high-temperature high-pressure reaction kettle through 1 intermediate container, heating and pressurizing to a supercritical state after the pressure is raised to a design pressure, introducing oxygen into the high-temperature high-pressure reaction kettle through the other 1 intermediate container, controlling the ratio of the raw materials to the oxygen and the pressure condition in the high-temperature high-pressure reaction kettle to react to generate supercritical multi-element thermal fluid, simultaneously recording temperature and pressure data in the reaction by the computer, collecting liquid products after the reaction by the test tube, and collecting gaseous products after the reaction by the sampling bag;
(2) Supercritical multi-element thermal fluid composition analysis
Analyzing the components of the collected liquid product and the collected gaseous product in the supercritical multi-element hot fluid by using a chromatograph to determine the proportion of the components;
(3) Analysis of Experimental data
Summarizing the temperature and pressure data obtained by the experiment, and drawing a curve graph of the temperature and the time and a curve graph of the pressure and the time; and analyzing the influences of the proportions of the components and the temperature and the pressure on the reaction heat release and the heat carrying capacity of the supercritical multi-element thermal fluid by combining the component analysis results of the chromatograph, so as to obtain the reaction heat release and heat carrying capacity data of the prepared supercritical multi-element thermal fluid.
In the invention, the proportion of each component is obtained according to the measurement result of a chromatograph, the reaction heat release and heat carrying data are respectively obtained by calculating through reaction temperature and pressure curves, and the calculation method is a conventional method known by professionals in the field.
The invention has the following beneficial effects:
the invention innovatively designs a system and a method for preparing supercritical multi-element thermal fluid in a laboratory. The supercritical multi-element thermal fluid under different raw material proportions and different temperature and pressure conditions can be prepared before the development and production practice of injecting the supercritical multi-element thermal fluid is carried out, the reaction heat release and heat carrying capacity of the supercritical multi-element thermal fluid are analyzed and optimized, the application effect of the supercritical multi-element thermal fluid injection technology in a heavy oil reservoir is effectively improved, and the analysis result can be used as a reference for technicians in the heavy oil reservoir development field.
Drawings
FIG. 1 is a flow diagram of a system for preparing supercritical multi-element thermal fluid in a laboratory according to the present invention.
The individual labels in FIG. 1 are as follows:
1, sampling bag; 2, a warm-pressing probe; 3, a computer; 4, a one-way valve; 5 intermediate container (oxygen); 6 intermediate vessel (nitrogen); 7, a high-precision constant-pressure constant-flow pump; 8, test tubes; 9, manually operating the pump; 10, a back pressure valve; 11 high-temperature high-pressure reaction kettle.
FIG. 2 is a technical flow chart of a method for preparing supercritical multi-element thermal fluid and analyzing reaction heat release and heat carrying capacity of the supercritical multi-element thermal fluid in a laboratory.
FIG. 3 is a graph showing the temperature inside the reactor varying with the reaction time at different oil-water ratios.
FIG. 4 is a graph showing the pressure inside the reactor varying with the reaction time at different oil-water ratios.
FIG. 5 is a graph showing the temperature inside the reactor with the reaction time under different temperature and pressure conditions.
FIG. 6 is a graph showing the pressure inside the reactor with the reaction time at different oil-water ratios.
Detailed Description
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
In order to facilitate the technical solution for those skilled in the art to understand, the present invention will be further explained with reference to the drawings in the following embodiments, which are not intended to limit the present invention. All other embodiments, which can be obtained by a person skilled in the art without invasive work on the basis of the present invention, fall within the scope of protection of the present invention.
Fig. 1 is a flow chart of a system for preparing supercritical multi-element thermal fluid in a laboratory according to the present invention. The invention provides a system for preparing supercritical multi-element hot fluid in a laboratory, which comprises: a high-temperature high- pressure reaction kettle 11, and 2 intermediate containers (an intermediate container (oxygen) 5 and an intermediate container (nitrogen) 6), a sampling bag 1, a computer 3 and a test tube 8 which are respectively connected on the high-temperature high-pressure reaction kettle 11.
Wherein, the high-temperature high-pressure reaction kettle 11 is used for controlling the temperature and pressure conditions to prepare the supercritical multi-element hot fluid; a one-way valve 4 is arranged on a pipeline between the 2 intermediate containers and the high-temperature high-pressure reaction kettle 11;
the high-temperature high-pressure reaction kettle 11 is connected with a test tube 8 through a pipeline and used for collecting liquid products after reaction. The sampling bag 1 is used for collecting gaseous products after reaction, the outlet pressure is controlled by a hand pump, and a back pressure valve 10 is arranged between the sampling bag 1 and the hand pump 9;
the computer 3 is used for recording temperature and pressure data in the reaction process in the high-temperature high-pressure reaction kettle 11, and a pipeline between the computer 3 and the high-temperature high-pressure reaction kettle 11 is provided with a temperature and pressure probe 2;
the middle container (oxygen) 5 and the middle container (nitrogen) 6 are respectively used for providing oxygen and nitrogen and are driven by a high-precision constant-pressure constant-flow pump 7;
all through the tube coupling between the above-mentioned part, and all set up the valve on the pipeline.
Further, the system for preparing the supercritical multi-element thermal fluid in the laboratory also comprises a chromatograph for analyzing the components of the supercritical multi-element thermal fluid.
The invention discloses a method for preparing supercritical multi-element thermal fluid in a laboratory, which comprises the following steps:
adding reaction raw materials (including oil and water) into a high-temperature high-pressure reaction kettle 11 before the beginning of an experiment; adding the raw materials of the supercritical multi-element thermal fluid in the sampling bag 1 into a high-temperature high-pressure reaction kettle 11; then introducing nitrogen into the high-temperature high-pressure reaction kettle 11 through an intermediate container (nitrogen) 6, heating and pressurizing to a supercritical state after the pressure is raised to a design pressure, introducing oxygen into the high-temperature high-pressure reaction kettle 11 through an intermediate container (oxygen) 5, reacting through the controlled ratio of raw materials (oil and water) to the oxygen and the temperature and pressure conditions in the high-temperature high-pressure reaction kettle 11 to generate supercritical multi-element thermal fluid, simultaneously recording temperature and pressure data in the reaction by a computer 3, collecting liquid products after the reaction by a test tube 8, and collecting gaseous products after the reaction by a sampling bag 1.
Fig. 2 is a technical flow chart of a method for preparing supercritical multi-element thermal fluid and analyzing the exothermic and heat-carrying capacity of the reaction in the laboratory according to the present invention.
The invention further provides a method for preparing the supercritical multi-element thermal fluid in a laboratory and analyzing the reaction heat release and heat carrying capacity of the supercritical multi-element thermal fluid, which comprises the following steps: the method comprises three parts of supercritical multi-element thermal fluid preparation, supercritical multi-element thermal fluid component analysis and experimental data analysis. The preparation of the supercritical multi-element hot fluid comprises the steps of adding raw materials in a certain proportion into a high-temperature high-pressure reaction kettle, heating and pressurizing the reaction kettle according to set conditions, enabling the raw materials to react in the reaction kettle to generate the supercritical multi-element hot fluid, and in the process, the supercritical multi-element hot fluid under different proportions and different temperature and pressure conditions can be generated by controlling the raw material proportion and the temperature and pressure conditions of the reaction kettle; the supercritical multi-element thermal fluid component analysis means that the collected reaction products are subjected to component analysis, and the proportion of each component in the generated supercritical multi-element thermal fluid is further determined; the experimental data analysis refers to that after the proportion of each component in the generated supercritical multi-element thermal fluid is determined, the reaction heat release and heat carrying capacity of the supercritical multi-element thermal fluid generated under different feeding proportions and different temperature and pressure conditions are analyzed by combining the temperature and pressure data of the reaction kettle recorded in the preparation process. The method specifically comprises the following steps:
(1) Supercritical multi-element thermal fluid preparation system adopting system for preparing supercritical multi-element thermal fluid in laboratory
Adding reaction raw materials (including oil and water) into a high-temperature high-pressure reaction kettle 11 before the experiment; then introducing nitrogen into the high-temperature high-pressure reaction kettle 11 through an intermediate container (nitrogen) 6, heating and pressurizing to a supercritical state after raising the pressure to a design pressure, introducing oxygen into the high-temperature high-pressure reaction kettle 11 through an intermediate container (oxygen) 5, reacting through the controlled ratio of raw materials (oil and water) to oxygen and the temperature and pressure conditions in the high-temperature high-pressure reaction kettle 11 to generate supercritical multi-element thermal fluid, simultaneously recording temperature and pressure data in the reaction by a computer 3, collecting a liquid product after the reaction by a test tube 8, and collecting a gaseous product after the reaction by a sampling bag 1;
(2) Supercritical multi-element thermal fluid component analysis
Analyzing the components of the collected liquid product and gaseous product in the supercritical multi-element hot fluid by using a chromatograph to determine the proportion of each component;
(3) Analysis of Experimental data
Summarizing temperature and pressure data obtained by experiments, and drawing a curve graph of temperature and time and a curve graph of pressure and time; and analyzing the influence of the proportion of each component, the temperature and the pressure on the reaction heat release and the heat carrying capacity of the supercritical multi-element thermal fluid by combining the component analysis results of the chromatograph to obtain the reaction heat release and heat carrying capacity data of the prepared supercritical multi-element thermal fluid.
Example 1
The invention discloses a method for preparing supercritical multi-element hot fluid in a laboratory, which comprises the following steps:
(1) Supercritical multi-element thermal fluid preparation
The supercritical multi-element thermal fluid preparation system shown in fig. 1 is used for preparing the supercritical multi-element thermal fluid, and the specific steps are as follows:
(1) before the experiment begins, a supercharging device (specifically a booster pump is used for compressing gas and then pumping the compressed gas into an intermediate container) is used for pumping sufficient (20 MPa) nitrogen and oxygen into corresponding intermediate containers respectively, and an inlet valve and an outlet valve are closed;
(2) connecting experimental equipment according to an experimental flow chart, and closing all valves after the connection is finished and the sealing performance of an experimental system is determined;
(3) and opening the sealing cover of the high-temperature high-pressure reaction kettle 11, and putting the reaction raw materials into the high-temperature high-pressure reaction kettle 11 according to the proportion designed by the experiment after determining that no residue exists in the high-temperature high-pressure reaction kettle 11. After the feeding is finished, tightly closing a sealing cover of the high-temperature high-pressure reaction kettle 11;
(4) lightly opening an outlet valve of the intermediate container (nitrogen) 6, opening an inlet of the high-temperature high-pressure reaction kettle 11, and filling nitrogen into the high-temperature high-pressure reaction kettle 11 to ensure that the high-temperature high-pressure reaction kettle 11 is sealed;
(5) after the high-temperature high-pressure reaction kettle 11 is determined to be sealed, an outlet valve and a sampling valve of the high-temperature high-pressure reaction kettle 11 are opened in sequence, the back pressure is 0MPa, and nitrogen is continuously filled for more than 10min to exhaust the air in the reaction kettle;
(6) after the air in the high-temperature high-pressure reaction kettle 11 is exhausted, the sampling valve and the outlet valve of the high-temperature high-pressure reaction kettle 11 are closed, and the nitrogen is continuously filled into the high-temperature high-pressure reaction kettle 11 to reach the experimental design pressure;
(7) after the pressure of the high-temperature high-pressure reaction kettle 11 rises to the design pressure, all valves are closed, the power supply of the high-temperature high-pressure reaction kettle 11 is opened, and heating is started;
(8) after the temperature and the pressure in the high-temperature high-pressure reaction kettle 11 reach the supercritical condition, the heating is closed, the shaking is started, a high-precision constant-pressure constant-flow pump 7 is started to pressurize an intermediate container (oxygen) 5, oxygen is filled into the kettle body of the high-temperature high-pressure reaction kettle 11 until the reaction is finished, and the temperature and the pressure in the high-temperature high-pressure reaction kettle 11 are monitored and recorded in real time in the whole reaction process;
(9) after the reaction is finished, the high-temperature high-pressure reaction kettle 11 is kept stand to cool, after the temperature in the high-temperature high-pressure reaction kettle 11 is reduced to normal temperature, a sampling opening valve is opened slightly, the sampling bag 1 collects a gas sample in the kettle, then the pressure is relieved, the high-temperature high-pressure reaction kettle 11 is opened, and the test tube 8 collects liquid and solid (if any) in the kettle.
Note: in the experimental process, the liquid outlet valve below the high-temperature high-pressure reaction kettle 11 can be continuously fed into the reaction kettle to maintain the continuous reaction and continuously generate the supercritical multi-element hot fluid.
(2) Supercritical multi-element thermal fluid component analysis
And (4) carrying out component analysis on the collected in-kettle samples by using a chromatograph, and determining the proportion of each component.
(3) Analysis of Experimental data
Temperature and pressure data obtained by experiments are collected and drawn into a curve chart, and the influence of the proportion of each component and the temperature and pressure on reaction heat release and heat carrying capacity of supercritical multi-element thermal fluid is analyzed by combining the component analysis results of a chromatograph.
The method comprises the steps of selecting 0# diesel oil, water and oxygen as raw materials, preparing supercritical multi-element thermal fluids under different raw material proportions and different temperature and pressure conditions, and analyzing the reaction heat release and heat carrying capacity of the supercritical multi-element thermal fluids.
TABLE 1 supercritical water-diesel reaction experiment parameters under different oil-water ratio conditions
Serial number | Reactants | Initial temperature and |
1 | 45mL of water, 5mL of diesel oil and |
400℃/ |
2 | 28.3mL of water, 5mL of diesel oil and |
400℃/ |
3 | 20mL of water, 5mL of diesel oil and |
400℃/ |
4 | 15mL of water, 5mL of diesel oil and |
400℃/ |
5 | 11.67mL of water, 5mL of diesel oil and |
400℃/25MPa |
The raw materials and control conditions were as shown in table 1, and the experiment was carried out according to the above procedure and the experimental data was recorded.
Analyzing the sampled samples one by one, wherein the analysis result table comprises the following steps: under the condition of sufficient oxygen, diesel oil can completely react to generate supercritical multi-element hot fluid, and no diesel oil residue exists in the sampling liquid. As can be seen from FIG. 3, the higher the volume ratio of diesel oil, the higher the highest temperature reached in the reactor, compared with the lower the diesel oil ratio, the higher the heat quantity released and the higher the temperature of the system, so the lower the highest temperature in the reactor.
The produced supercritical multi-element thermal fluid heat carrying capacity (table 2) is calculated based on the produced fluid components, and only from the produced fluid heat carrying capacity, the water proportion is higher, the product heat carrying capacity is higher, the supercritical water heat carrying capacity is mainly adopted in the thermal fluid, and the supercritical water proportion is highest at the moment. As can be seen from FIG. 4, the higher the supercritical water proportion in the product is, the larger the heat capacity is, the less the condensation amount in the cooling process is, and the longer the pressure can be maintained.
TABLE 2 Heat carrying capacity of reaction product under different oil-water ratio conditions
Example 2
The method comprises the steps of selecting 0# diesel oil, water and oxygen as raw materials, and preparing supercritical multi-element thermal fluid under different raw material proportions and different temperature and pressure conditions. The materials and control conditions were as shown in Table 3, and the experiment was carried out in accordance with the method of the present invention in example 1, and the experimental data was recorded.
TABLE 3 supercritical water-diesel reaction experiment parameters under different temperature and pressure conditions
Serial number | Reactants | Initial temperature and |
6 | 45mL of water, 5mL of diesel oil and |
400℃/23MPa |
7 | 45mL of water, 5mL of diesel oil and |
400℃/ |
8 | 45mL of water, 5mL of diesel oil and pure oxygen | 450℃/ |
9 | 45mL of water, 5mL of diesel oil and |
500℃/ |
10 | 45mL of water, 5mL of diesel oil and |
500℃/23MPa |
The experimental results are shown in fig. 5 and fig. 6, and the experimental processes comparing different initial temperature and pressure conditions show that the temperature rise amplitude in the kettle is very close, the reaction heat release is considered to be close, the initial temperature and pressure conditions have small influence on the reaction, the enthalpy value of the hot fluid is converted to the same temperature and pressure, the value is very close, and the average value is 1962.36J/g.
Claims (4)
1. A system for preparing supercritical multi-element thermal fluid in a laboratory, comprising:
the device comprises a high-temperature high-pressure reaction kettle, and 2 intermediate containers, a sampling bag, a computer and a test tube which are respectively connected to the high-temperature high-pressure reaction kettle;
a one-way valve is arranged on a pipeline between the 2 intermediate containers and the high-temperature high-pressure reaction kettle; the 2 intermediate containers are all driven by a high-precision constant-pressure constant-flow pump;
the sampling bag controls outlet pressure through a hand pump, and a back pressure valve is arranged between the sampling bag and the hand pump;
a temperature and pressure probe is arranged on a pipeline between the computer and the high-temperature high-pressure reaction kettle;
all through the tube coupling between the above-mentioned part, and all set up the valve on the pipeline.
2. The system for laboratory preparation of supercritical multi-component thermal fluid of claim 1 wherein the system for laboratory preparation of supercritical multi-component thermal fluid further comprises a chromatograph for analyzing the composition of the supercritical multi-component thermal fluid.
3. A method for preparing supercritical multi-component thermal fluid in laboratory using the system for preparing supercritical multi-component thermal fluid in laboratory according to claim 1, comprising the steps of:
adding reaction raw materials into the high-temperature high-pressure reaction kettle before the beginning of the experiment; and then introducing nitrogen into the high-temperature high-pressure reaction kettle through 1 intermediate container, heating and pressurizing to a supercritical state after the pressure is raised to the design pressure, introducing oxygen into the high-temperature high-pressure reaction kettle through the other 1 intermediate container, controlling the ratio of the raw materials to the oxygen and the pressure condition in the high-temperature high-pressure reaction kettle to react to generate supercritical multi-element thermal fluid, simultaneously recording temperature and pressure data in the reaction by the computer, collecting liquid products after the reaction by the test tube, and collecting gaseous products after the reaction by the sampling bag.
4. A method for preparing supercritical multi-element thermal fluid in a laboratory and analyzing reaction heat release and heat carrying capacity of the supercritical multi-element thermal fluid comprises the following steps:
(1) Preparation of supercritical multi-element thermal fluid using the system for laboratory preparation of supercritical multi-element thermal fluid according to claim 1 or 2
Adding reaction raw materials into the high-temperature high-pressure reaction kettle before the beginning of the experiment; then introducing nitrogen into the high-temperature high-pressure reaction kettle through 1 intermediate container, heating and pressurizing to a supercritical state after the pressure is raised to a design pressure, introducing oxygen into the high-temperature high-pressure reaction kettle through the other 1 intermediate container, controlling the ratio of the raw materials to the oxygen and the pressure condition in the high-temperature high-pressure reaction kettle to react to generate supercritical multi-element thermal fluid, simultaneously recording temperature and pressure data in the reaction by the computer, collecting liquid products after the reaction by the test tube, and collecting gaseous products after the reaction by the sampling bag;
(2) Supercritical multi-element thermal fluid component analysis
Analyzing the components of the liquid product and the gaseous product in the supercritical multi-element hot fluid by using a chromatograph to determine the proportion of the components;
(3) Analysis of Experimental data
Summarizing the temperature and pressure data obtained by the experiment, and drawing a curve graph of the temperature and the time and a curve graph of the pressure and the time; and analyzing the influence of the proportion of the components and the temperature and the pressure on the reaction heat release and the heat carrying capacity of the supercritical multi-element thermal fluid by combining the component analysis results of the chromatograph, so as to obtain the reaction heat release and heat carrying capacity data of the supercritical multi-element thermal fluid.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202211135767.6A CN115582085A (en) | 2022-09-19 | 2022-09-19 | System and method for preparing supercritical multi-element thermal fluid in laboratory |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202211135767.6A CN115582085A (en) | 2022-09-19 | 2022-09-19 | System and method for preparing supercritical multi-element thermal fluid in laboratory |
Publications (1)
Publication Number | Publication Date |
---|---|
CN115582085A true CN115582085A (en) | 2023-01-10 |
Family
ID=84778614
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202211135767.6A Pending CN115582085A (en) | 2022-09-19 | 2022-09-19 | System and method for preparing supercritical multi-element thermal fluid in laboratory |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN115582085A (en) |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20070264175A1 (en) * | 2003-11-19 | 2007-11-15 | Iversen Steen B | Method And Process For Controlling The Temperature, Pressure-And Density Profiles In Dense Fluid Processes |
CN110711548A (en) * | 2019-09-25 | 2020-01-21 | 太原理工大学 | Device and method for converting methane in supercritical water |
CN112664176A (en) * | 2020-12-28 | 2021-04-16 | 西安交通大学 | Supercritical multi-element thermal fluid huff and puff oil production test simulation device and method |
CN113685811A (en) * | 2021-08-31 | 2021-11-23 | 武汉武锅能源工程有限公司 | Supercritical hydrothermal combustion composite thermal fluid generation platform |
-
2022
- 2022-09-19 CN CN202211135767.6A patent/CN115582085A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20070264175A1 (en) * | 2003-11-19 | 2007-11-15 | Iversen Steen B | Method And Process For Controlling The Temperature, Pressure-And Density Profiles In Dense Fluid Processes |
CN110711548A (en) * | 2019-09-25 | 2020-01-21 | 太原理工大学 | Device and method for converting methane in supercritical water |
CN112664176A (en) * | 2020-12-28 | 2021-04-16 | 西安交通大学 | Supercritical multi-element thermal fluid huff and puff oil production test simulation device and method |
CN113685811A (en) * | 2021-08-31 | 2021-11-23 | 武汉武锅能源工程有限公司 | Supercritical hydrothermal combustion composite thermal fluid generation platform |
Non-Patent Citations (2)
Title |
---|
邹遂丰;郭正斌;王珏;骆青松;: "井筒内超临界多元热流体注入过程的数值模拟", 科学技术与工程, no. 19, 8 July 2020 (2020-07-08), pages 96 - 103 * |
黄祖杰等: "超临界多元热流体提高稠油采收率机理研究", 工程热物理学报, vol. 43, no. 4, 30 April 2022 (2022-04-30), pages 1 * |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN101520962B (en) | Hydrocarbon source rock formation pore heat-pressing hydrocarbon-generation simulator and use method thereof | |
CN104849172B (en) | Oil content of oil shale experimental apparatus for testing and its method of testing | |
CN104777057A (en) | Supercritical CO2 injection and coalbed methane enhanced displacement simulation test device | |
CN108730760B (en) | Hydrogen storage tank fills hydrogen filling performance detecting system | |
CN108072751B (en) | Fracturing fluid and reservoir interaction simulation experiment system and experiment method | |
CN109781579A (en) | A kind of hydrogen storage material cycle life auto testing instrument and test method | |
CN113324889B (en) | Device for evaluating shale oil in-situ pyrolysis exploitation displacement efficiency and testing method | |
CN111855377A (en) | Supercritical CO2Test device and method for producing methane by extracting coal coupling biological reaction | |
CN115582085A (en) | System and method for preparing supercritical multi-element thermal fluid in laboratory | |
CN208013210U (en) | A kind of fracturing fluid and reservoir interact experimental system for simulating | |
CN109238794A (en) | A kind of automatic sampling apparatus of shock tube pyrolysis product | |
CN112345732A (en) | Deep geothermal reservoir transformation and seepage heat transfer simulation device | |
CN108414391A (en) | A kind of experimental provision and experimental method of high temperature and high pressure steam pyrolytic reaction | |
CN210015106U (en) | Gas reservoir drives gas experimental apparatus | |
CN208765930U (en) | Supercritical CO2Jet stream feedway and jet stream experimental system | |
CN219104675U (en) | Water-doped supercritical carbon dioxide corrosion test device | |
CN206740583U (en) | A kind of carbon dioxide dry method fracturing fluid rheological property evaluating apparatus | |
CN106770396B (en) | Method for measuring hydrogen storage material hydrogen discharge reaction thermodynamic parameter | |
CN213955679U (en) | Test device for measuring performance of supercritical carbon dioxide heat exchanger and material | |
CN107315025A (en) | The pressure compensation and bleeder of HTHP thermal insulation test process | |
CN203732526U (en) | Test device for carbon dioxide-hot dry rock powder reaction | |
CN107315029A (en) | The pressure compensation and drainage method of HTHP thermal insulation test process | |
CN103869044B (en) | Testing device and testing method for reaction of carbon dioxide and hot dry rock powder | |
CN208921655U (en) | Carbon and hydrogen isotope oil-free valve analysis system for mineral fluid inclusion | |
CN110243672B (en) | CO (carbon monoxide)2Supercharging metering system and using method |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination |