CN112525661A - Preparation method of natural gas hydrate simulated rock sample - Google Patents
Preparation method of natural gas hydrate simulated rock sample Download PDFInfo
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- CN112525661A CN112525661A CN202011030664.4A CN202011030664A CN112525661A CN 112525661 A CN112525661 A CN 112525661A CN 202011030664 A CN202011030664 A CN 202011030664A CN 112525661 A CN112525661 A CN 112525661A
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- rock sample
- refrigeration
- natural gas
- gas hydrate
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- 239000011435 rock Substances 0.000 title claims abstract description 109
- NMJORVOYSJLJGU-UHFFFAOYSA-N methane clathrate Chemical compound C.C.C.C.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O NMJORVOYSJLJGU-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000005057 refrigeration Methods 0.000 claims abstract description 53
- 238000000034 method Methods 0.000 claims abstract description 46
- 238000003825 pressing Methods 0.000 claims abstract description 20
- 229920006395 saturated elastomer Polymers 0.000 claims abstract description 19
- 239000007864 aqueous solution Substances 0.000 claims abstract description 13
- 239000011148 porous material Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000007710 freezing Methods 0.000 claims abstract description 11
- 230000008014 freezing Effects 0.000 claims abstract description 11
- 238000011065 in-situ storage Methods 0.000 claims description 8
- 238000002474 experimental method Methods 0.000 claims description 6
- 238000000748 compression moulding Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000009826 distribution Methods 0.000 claims description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 4
- 239000011707 mineral Substances 0.000 claims description 4
- 239000002689 soil Substances 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 4
- 238000000556 factor analysis Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 239000002734 clay mineral Substances 0.000 claims description 2
- 239000006185 dispersion Substances 0.000 claims description 2
- 238000012360 testing method Methods 0.000 abstract description 4
- 238000011160 research Methods 0.000 description 7
- 238000004088 simulation Methods 0.000 description 6
- 238000005065 mining Methods 0.000 description 4
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000012047 saturated solution Substances 0.000 description 2
- 238000000889 atomisation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000011549 displacement method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005243 fluidization Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000005464 sample preparation method Methods 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/42—Low-temperature sample treatment, e.g. cryofixation
Abstract
The invention relates to the technical field of natural gas hydrate experimental tests, in particular to a preparation method of a natural gas hydrate simulated rock sample. The preparation method comprises the following steps: (1) optimizing the artificial refrigeration freezing process and parameters; (2) pressing and forming a natural gas hydrate rock sample framework; (3) vacuumizing a rock sample framework to obtain a saturated aqueous solution; (4) and (5) freezing pore water in the saturated rock sample framework by refrigeration.
Description
Technical Field
The invention relates to the technical field of natural gas hydrate experimental tests, in particular to a preparation method of a natural gas hydrate simulated rock sample.
Background
The natural gas hydrate mining technology is still in the theoretical research and stope trial mining stage, and an economic and effective commercial mining mode is not formed yet, and the main mining methods comprise a depressurization method, a heat injection method, a chemical agent injection method, a CO2 displacement method, a solid fluidization method and the like. The commercial exploitation process of the natural gas hydrate still faces a plurality of key technical problems, the simulation research of the indoor experiment is a key basic link of the exploration and development of the natural gas hydrate, and a large amount of indoor simulation experiments are realized by corresponding stratum rock samples containing the natural gas hydrate. However, due to the difficulty and high cost of obtaining natural hydrate rock samples, most of related researchers at home and abroad adopt artificial natural gas hydrate rock samples to replace natural hydrate rock samples. At present, the natural gas hydrate experimental rock sample is prepared mainly by preparing a rock sample framework by pressurizing a high-pressure reaction kettle, and then inputting methane gas and water to generate a hydrate in a rock sample pore to obtain the natural gas hydrate experimental rock sample. In general, the natural gas hydrate experimental rock sample at the present stage has the defects of large difference of physical property parameters with the in-situ stratum, small size, poor uniformity of pores and the like, and the application accuracy of the research result is influenced.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of a natural gas hydrate simulated rock sample, which is characterized in that the simulated rock sample is formed by pressing a framework, a saturated solution and refrigerating and freezing to replace a natural gas hydrate in-situ rock sample, and an experimental rock sample is provided for the simulation of the mechanical properties of a natural gas hydrate reservoir rock and the research of related simulation experiments.
The invention relates to a preparation method of a natural gas hydrate simulated rock sample, which comprises the following steps:
(1) optimizing the artificial refrigeration freezing process and parameters;
(2) pressing and forming a natural gas hydrate rock sample framework;
(3) vacuumizing a rock sample framework to obtain a saturated aqueous solution;
(4) and (5) freezing pore water in the saturated rock sample framework by refrigeration.
According to the preparation method of the natural gas hydrate simulated rock sample, the artificial refrigeration freezing process and parameters are optimized in the step (1), the balance refrigeration process is preferably adopted according to the mechanical parameters of the pure natural gas hydrate rock sample, the relation between factors such as the refrigeration speed, the refrigeration temperature and the refrigeration time and the mechanical parameters of frozen ice is established through a single-factor analysis method, the artificial refrigeration parameters are optimized, and the mechanical parameters of frozen ice and the mechanical parameters of natural gas hydrate are consistent.
The mechanical parameters of the rock sample comprise key parameters such as compressive strength, shear strength, Young modulus, Poisson's ratio and the like.
The balanced refrigeration process refers to a process capable of realizing balanced refrigeration of a rock sample from inside to outside;
the refrigeration rate refers to the reduction rate of the ambient temperature in the refrigeration process adopted by the balanced refrigeration process;
the refrigeration temperature refers to the initial and final refrigeration ambient temperatures adopted by the balanced refrigeration process;
the refrigeration time refers to the refrigeration time adopted by the equilibrium refrigeration process.
According to the preparation method of the natural gas hydrate simulated rock sample, the natural gas hydrate rock sample framework is pressed and formed in the step (2), rock and soil with the same mineral components, the same particle size composition and the same distribution as those of the actual reservoir rock framework are adopted, and the rock sample framework is pressed and formed by adopting a proper pressing process and parameters according to the shape required by an experiment after humidification treatment.
The rock sample framework is characterized in that the collapse is not generated after the compression molding.
The rock sample pressing process comprises pressing pressure, pressing time and the like.
The porosity of the rock sample framework is basically equivalent to the porosity of the in-situ hydrate reservoir framework.
According to the preparation method of the natural gas hydrate substitute rock sample, the natural gas hydrate rock sample framework is pressed and formed in the step (3), rock and soil with the same mineral components, the same particle size composition and the same distribution as those of the actual reservoir rock framework are adopted, and the rock sample framework is pressed and formed by adopting a proper pressing process and parameters according to the shape required by an experiment after humidification treatment.
The rock sample framework is characterized in that the collapse is not generated after the compression molding.
The rock sample pressing process comprises pressing pressure, pressing time and the like.
The porosity of the rock sample framework is basically equivalent to the porosity of an in-situ hydrate reservoir.
The preparation method of the natural gas hydrate simulated rock sample comprises the steps of (3) vacuumizing a rock sample framework to saturate aqueous solution, placing the rock sample framework formed in the step (2) in a vacuum container, and saturating the aqueous solution under a certain saturation condition to prepare a saturated rock sample containing a certain aqueous solution saturation degree.
The aqueous solution needs to meet the condition that clay mineral expansion and dispersion do not occur on the rock sample framework.
The rock sample can be protected by a sponge block, and collapse of the rock sample in the saturation process is avoided.
The certain saturation condition refers to a specific vacuum degree and saturation time.
And the ice saturation formed after the pore water in the saturated rock sample is refrigerated and frozen is equivalent to the natural gas hydrate saturation in the required simulated natural gas hydrate reservoir.
According to the preparation method of the natural gas hydrate simulated rock sample, the pore water in the saturated rock sample framework is frozen in the step (4) in a refrigerating manner, the saturated rock sample is refrigerated by adopting the artificial refrigerating process and the refrigerating parameters in the step (1) on the basis of the step (3), and the water solution in the pore is frozen to finally form the simulated rock sample.
Compared with the prior art, the invention has the beneficial effects that: according to the preparation method of the natural gas hydrate simulated rock sample, the simulated rock sample is formed by pressing the framework, the saturated solution and refrigerating and freezing to replace the natural gas hydrate in-situ rock sample, so that the experimental rock sample is provided for the mechanical property simulation of the natural gas hydrate reservoir rock and the related simulation experiment research, the requirement of the indoor experiment research on a large number of hydrate rock samples is met, the consumption of a large amount of manpower, material resources and financial resources required by the natural gas hydrate reservoir in-situ heat preservation and pressure maintaining coring is greatly reduced, and a reasonable and feasible rock sample preparation method is provided for the natural gas hydrate indoor experiment research.
Drawings
FIG. 1 is a diagram of the preparation method of the natural gas hydrate simulated rock sample of the invention.
Detailed Description
The following detailed description of embodiments of the present invention is provided in connection with the accompanying drawings and examples. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example, as shown in fig. 1:
firstly, carrying out mechanical parameter test on an artificially synthesized natural gas hydrate rock sample to obtain the mechanical parameters (compressive strength, shear strength, Young modulus, Poisson ratio and the like) of the artificially synthesized natural gas hydrate rock sample; and secondly, adopting a balanced refrigeration process, controlling the water solution to be uniformly solidified, controlling the refrigeration rate to slowly reduce the initial environmental temperature to the refrigeration termination temperature, and realizing balanced refrigeration. And analyzing the ice strength under the conditions influenced by factors such as different refrigeration rates, refrigeration temperatures, refrigeration time and the like by adopting a single-factor analysis method, optimizing the refrigeration parameters, and realizing consistency of the mechanical parameters of the frozen ice and the mechanical parameters of the natural gas hydrate.
And (2) adopting rock and soil with the same mineral components, the same grain size composition and the same distribution as those of the actual reservoir rock framework, performing atomization and humidification treatment, performing compression molding on the natural gas hydrate rock framework, testing the porosity of the natural gas hydrate rock framework, adjusting the compression process to ensure that the porosity of the rock sample is basically equivalent to that of the in-situ hydrate reservoir, and preventing the rock sample framework from collapsing after compression molding. And finally, forming the rock sample framework by adopting the pressing process.
And (3) in order to avoid collapse of the rock sample in the saturation process, wrapping the rock sample skeleton in the step (2) by using a sponge block, placing the rock sample skeleton into a vacuum container, adding an aqueous solution with good compatibility with the rock sample, and adjusting the vacuum degree and the saturation time to form the saturated rock sample with a certain aqueous solution saturation degree.
And (4) on the basis of the step (3), refrigerating the saturated rock sample by adopting the artificial refrigeration process and the refrigeration parameters in the step (1), and freezing the water solution in the pores to finally form the simulated rock sample.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (5)
1. A preparation method of a natural gas hydrate simulated rock sample is characterized by comprising the following steps:
(1) optimizing the artificial refrigeration freezing process and parameters;
(2) pressing and forming a natural gas hydrate rock sample framework;
(3) vacuumizing a rock sample framework to obtain a saturated aqueous solution;
(4) and (5) freezing pore water in the saturated rock sample framework by refrigeration.
2. The method for preparing the natural gas hydrate simulated rock sample according to claim 1, wherein the artificial refrigeration freezing process and parameters are optimized in the step (1), and the relationship between factors such as the refrigeration speed, the refrigeration temperature and the refrigeration time and the mechanical parameters of the frozen ice is established according to the mechanical parameters of the pure natural gas hydrate rock sample, preferably by adopting an equilibrium refrigeration process, through a single-factor analysis method, so that the artificial refrigeration parameters are optimized, and the mechanical parameters of the frozen ice are consistent with the mechanical parameters of the natural gas hydrate.
The mechanical parameters of the rock sample comprise key parameters such as compressive strength, shear strength, Young modulus, Poisson's ratio and the like.
The balanced refrigeration process refers to a process capable of realizing balanced refrigeration of a rock sample from inside to outside;
the refrigeration rate refers to the reduction rate of the ambient temperature in the refrigeration process adopted by the balanced refrigeration process;
the refrigeration temperature refers to the initial and final refrigeration ambient temperatures adopted by the balanced refrigeration process;
the refrigeration time refers to the refrigeration time adopted by the equilibrium refrigeration process.
3. The method for preparing a natural gas hydrate simulated rock sample according to claim 1, wherein the natural gas hydrate rock sample skeleton molded in the step (2) is formed by pressing the rock sample skeleton according to the shape required by the experiment and by adopting a proper pressing process and parameters after humidification treatment by using rock and soil with the same mineral composition, the same particle size composition and the same distribution as those of the actual reservoir rock skeleton.
The rock sample framework is characterized in that the collapse is not generated after the compression molding.
The rock sample pressing process comprises pressing pressure, pressing time and the like.
The porosity of the rock sample framework is basically equivalent to the porosity of the in-situ hydrate reservoir framework.
4. The method for preparing the natural gas hydrate simulated rock sample as claimed in claim 1, wherein the rock sample framework in the step (3) is vacuumized to obtain the saturated aqueous solution, the rock sample framework formed by pressing in the step (2) is placed in a vacuum container, and the aqueous solution is saturated under a certain saturation condition to prepare the saturated rock sample of the saturated aqueous solution.
The aqueous solution needs to meet the condition that clay mineral expansion and dispersion do not occur on the rock sample framework.
The rock sample can be protected by a sponge block, and collapse of the rock sample in the saturation process is avoided.
The certain saturation condition refers to a specific vacuum degree and saturation time.
And the ice saturation formed after the pore water in the saturated rock sample is refrigerated and frozen is equivalent to the natural gas hydrate saturation in the required simulated natural gas hydrate reservoir.
5. The method for preparing the natural gas hydrate simulated rock sample as claimed in claim 1, wherein the pore water in the skeleton of the saturated rock sample is frozen by refrigeration in the step (4), and on the basis of the step (3), the saturated rock sample is refrigerated by adopting the artificial refrigeration process and the refrigeration parameters in the step (1), so that the water solution in the pore is frozen, and the simulated rock sample is finally formed.
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| CN104198243A (en) * | 2014-08-29 | 2014-12-10 | 中国石油天然气股份有限公司 | Preparation method of artificial rock core for simulating permafrost region hydrate stratum skeleton |
| CN104949870A (en) * | 2015-06-16 | 2015-09-30 | 青岛海洋地质研究所 | Pressing method for methane hydrate containing rock core sample |
| CN107238521A (en) * | 2017-06-07 | 2017-10-10 | 中国石油大学(华东) | A kind of preparation method of tundra hydrate rock core |
| CN107526892A (en) * | 2017-08-30 | 2017-12-29 | 广州海洋地质调查局 | A kind of stability assessment method of ocean gas hydrate pilot production reservoir |
| CN107576562A (en) * | 2017-10-19 | 2018-01-12 | 南京泰克奥科技有限公司 | A kind of multi- scenarios method true triaxial test system and its test method |
| CN109212162A (en) * | 2018-08-17 | 2019-01-15 | 西南石油大学 | A method of estimation diagenesis gas hydrates reservoir mechanics parameter |
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2020
- 2020-09-27 CN CN202011030664.4A patent/CN112525661B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104198243A (en) * | 2014-08-29 | 2014-12-10 | 中国石油天然气股份有限公司 | Preparation method of artificial rock core for simulating permafrost region hydrate stratum skeleton |
| CN104949870A (en) * | 2015-06-16 | 2015-09-30 | 青岛海洋地质研究所 | Pressing method for methane hydrate containing rock core sample |
| CN107238521A (en) * | 2017-06-07 | 2017-10-10 | 中国石油大学(华东) | A kind of preparation method of tundra hydrate rock core |
| CN107526892A (en) * | 2017-08-30 | 2017-12-29 | 广州海洋地质调查局 | A kind of stability assessment method of ocean gas hydrate pilot production reservoir |
| CN107576562A (en) * | 2017-10-19 | 2018-01-12 | 南京泰克奥科技有限公司 | A kind of multi- scenarios method true triaxial test system and its test method |
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Non-Patent Citations (4)
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| JUN-WEI HUANG: "Application of conditional simulation of heterogeneous rock properties to seismic scattering and attenuation analysis in gas hydrate reservoirs", 《JOURNAL OF APPLIED GEOPHYSICS》 * |
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