CN114034725A - Method for observing generation process of tetrahydrofuran hydrate - Google Patents

Method for observing generation process of tetrahydrofuran hydrate Download PDF

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Publication number
CN114034725A
CN114034725A CN202111515669.0A CN202111515669A CN114034725A CN 114034725 A CN114034725 A CN 114034725A CN 202111515669 A CN202111515669 A CN 202111515669A CN 114034725 A CN114034725 A CN 114034725A
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China
Prior art keywords
reaction kettle
observation
tetrahydrofuran
solution
observing
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CN202111515669.0A
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夏富军
邓少贵
刘学锋
尼浩
魏宝君
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China University of Petroleum East China
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China University of Petroleum East China
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/02Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material
    • G01N23/04Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and forming images of the material
    • G01N23/046Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and forming images of the material using tomography, e.g. computed tomography [CT]
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q

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  • Health & Medical Sciences (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Pulmonology (AREA)
  • Radiology & Medical Imaging (AREA)
  • Theoretical Computer Science (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)

Abstract

The invention discloses an observation method for a tetrahydrofuran hydrate generation process, which comprises the steps of firstly preparing a tetrahydrofuran aqueous solution, then adding an inorganic salt developer into the tetrahydrofuran aqueous solution to obtain an observation solution, wherein the concentration of the inorganic salt developer in the observation solution is 10%, then adding sea sand into a reaction kettle, dripping the observation solution into the reaction kettle, carrying out cooling treatment on the reaction kettle after the sea sand and the observation solution are added, and carrying out X-ray CT scanning on the reaction kettle when the temperature in the reaction kettle is increased after the cooling treatment to obtain a CT scanning image; and carrying out image processing on the CT scanning image to obtain a processed image, and carrying out observation analysis on the processed image. The method provided by the invention can observe the slow growth of the hydrate even if a common CT scanning device is used, and realize the real-time observation of the growth process of the hydrate.

Description

Method for observing generation process of tetrahydrofuran hydrate
Technical Field
The invention relates to the technical field of petroleum engineering, in particular to a method for observing a generation process of tetrahydrofuran hydrate.
Background
Compared with an oil gas reservoir, the natural gas hydrate reservoir is more complex in distribution form in pores, so that the difference of macroscopic resistivity and acoustic wave characteristics is caused, the acoustic-electric characteristics of the natural gas hydrate reservoir are the basis for evaluating the porosity and the saturation, the change rule of microscopic characteristics and macroscopic response of the natural gas hydrate reservoir is quantitatively researched, and the evaluation precision of the reservoir is improved.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for observing the formation process of tetrahydrofuran hydrate, which can reduce the formation rate of hydrate in a simulation experiment of tetrahydrofuran aqueous solution.
In order to achieve the above purpose, the solution of the invention is:
a method for observing a generation process of a tetrahydrofuran hydrate is characterized by comprising the following steps:
the method comprises the following steps: preparing tetrahydrofuran aqueous solution;
step two: adding an inorganic salt developer into the tetrahydrofuran aqueous solution in the step one, wherein the inorganic salt developer is potassium iodide or sodium iodide to obtain an observation solution, and the concentration of the inorganic salt developer in the observation solution is 10%;
step three: adding sea sand into a reaction kettle, and dripping into an observation solution;
step four: cooling the reaction kettle;
step five: when the temperature in the reaction kettle rises, carrying out X-ray CT scanning on the reaction kettle to obtain a CT scanning image;
step six: and (4) carrying out image processing on the CT scanning image obtained in the fourth step to obtain a processed image, and carrying out observation analysis on the processed image.
Further, in the second step, the developer is in a solution state or a solid state.
Further, in the fourth step, the frequency of the X-ray CT scan is 4 times/min.
Further, in the second step, the tetrahydrofuran concentration in the observation solution is greater than 30%.
Further, in the third step, the sea sand is 20-40 meshes.
Further, the reaction kettle is a sealable reaction kettle, and the reaction kettle is firstly sealed in the fourth step.
The invention has the following beneficial effects: the concentration of the inorganic salt developer in the observation solution used was 10%, and the inorganic salt developer at this concentration had an inhibitory effect on hydrate formation. As hydrates are formed, the amount of free water in the system decreases, resulting in a gradual increase in the concentration of inorganic salt developer in solution. The increase of the concentration of the inorganic salt developer causes the growth process of the hydrate to be inhibited and the growth process to be slowed down. In the process, the inorganic salt developer with the concentration plays a role in developing and inhibiting the generation of the hydrate, and the slow growth of the hydrate can be observed even if a common CT scanning device is used by using the method provided by the invention, so that the real-time observation of the growth process of the hydrate is realized.
Drawings
FIG. 1 is a schematic flow chart of the present invention
Detailed Description
In order to further explain the technical solution of the present invention, the present invention is explained in detail by the following specific examples.
The embodiment provides a method for observing a generation process of a tetrahydrofuran hydrate, wherein the flow is shown as a figure 1, and the method comprises the following steps:
a method for observing a generation process of a tetrahydrofuran hydrate is characterized by comprising the following steps:
the method comprises the following steps: preparing tetrahydrofuran aqueous solution.
Step two: and (2) adding an inorganic salt developer into the tetrahydrofuran aqueous solution in the step one, wherein the inorganic salt developer is potassium iodide or sodium iodide, so as to obtain an observation solution, the concentration of the inorganic salt developer in the observation solution is 10%, and the value range of the tetrahydrofuran concentration in the observation solution is more than 30%. And is less than or equal to the saturation concentration.
Step three: the method comprises the steps of adding sea sand into a reaction kettle, and dripping into an observation solution, wherein the reaction kettle is provided with a cylindrical accommodating cavity with the cross section diameter of 1cm and the height of 1cm, the sea sand is placed in the accommodating cavity, the added sea sand is about 2g, and the dripped observation solution just submerges the surface of the sea sand in the reaction kettle.
Step four: and carrying out air cooling continuous cooling treatment on the reaction kettle, wherein the used air cooling equipment is conventional technology.
Step five: when the temperature in the reaction kettle rises, generating hydrate in the reaction kettle, continuously performing air cooling continuous cooling treatment on the reaction kettle, and performing X-ray CT scanning on the reaction kettle to obtain a CT scanning image;
step six: and (4) carrying out image processing on the CT scanning image obtained in the fourth step to obtain a processed image, and carrying out observation analysis on the processed image.
Preferably, in the second step, the developer is in a solution state or a solid state.
Preferably, in the fourth step, the frequency of the X-ray CT scan is 4 times/min.
Preferably, in the third step, the sea sand is 20-40 meshes.
Preferably, the reaction kettle is a sealable reaction kettle, and the reaction kettle is firstly sealed in the fourth step.
The invention has the following beneficial effects: the concentration of the inorganic salt developer in the observation solution used was 10%, and the inorganic salt developer at this concentration had an inhibitory effect on hydrate formation. As hydrates are formed, the amount of free water in the system decreases, resulting in a gradual increase in the concentration of inorganic salt developer in solution. The increase of the concentration of the inorganic salt developer causes the growth process of the hydrate to be inhibited and the growth process to be slowed down. In the process, the inorganic salt developer with the concentration plays a role in developing and inhibiting the generation of the hydrate, and the slow growth of the hydrate can be observed even if a common CT scanning device is used by using the method provided by the invention, so that the real-time observation of the growth process of the hydrate is realized.
Although illustrative embodiments of the present invention have been described above to facilitate the understanding of the present invention by those skilled in the art, it should be understood that the present invention is not limited to the scope of the embodiments, and various changes may be made apparent to those skilled in the art as long as they are within the spirit and scope of the present invention as defined and defined by the appended claims, and all matters of the invention which utilize the inventive concepts are protected.

Claims (6)

1. A method for observing a generation process of a tetrahydrofuran hydrate is characterized by comprising the following steps:
the method comprises the following steps: preparing tetrahydrofuran aqueous solution;
step two: adding an inorganic salt developer into the tetrahydrofuran aqueous solution in the step one, wherein the inorganic salt developer is potassium iodide or sodium iodide to obtain an observation solution, and the concentration of the inorganic salt developer in the observation solution is 10%;
step three: adding sea sand into a reaction kettle, and dripping into an observation solution;
step four: cooling the reaction kettle;
step five: when the temperature in the reaction kettle rises, carrying out X-ray CT scanning on the reaction kettle to obtain a CT scanning image;
step six: and (4) carrying out image processing on the CT scanning image obtained in the fourth step to obtain a processed image, and carrying out observation analysis on the processed image.
2. The method for observing a formation process of a tetrahydrofuran hydrate according to claim 1, wherein: in the second step, the developer is in a solution state or a solid state.
3. The method for observing a formation process of a tetrahydrofuran hydrate according to claim 1, wherein: in the fourth step, the frequency of the X-ray CT scan is 4 times/min.
4. The method for observing a formation process of a tetrahydrofuran hydrate according to claim 1, wherein: in the second step, the tetrahydrofuran concentration in the observation solution is more than 30%.
5. The method for observing a formation process of a tetrahydrofuran hydrate according to claim 1, wherein: in the third step, the sea sand is 20-40 meshes.
6. The method for observing a formation process of a tetrahydrofuran hydrate according to claim 1, wherein: the reaction kettle is a sealable reaction kettle, and the reaction kettle is firstly sealed in the fourth step.
CN202111515669.0A 2021-12-13 2021-12-13 Method for observing generation process of tetrahydrofuran hydrate Pending CN114034725A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004002754A (en) * 2002-03-28 2004-01-08 Mitsui Eng & Shipbuild Co Ltd Gas hydrate, method for producing the same and agent for suppressing decomposition of gas hydrate
CN105866144A (en) * 2016-05-26 2016-08-17 大连理工大学 Method for distinguishing aquo-complex phase from water phase through CT scanning
CN109406551A (en) * 2018-12-11 2019-03-01 吉林大学 A kind of analysis method for testing asphalt internal structure feature
WO2021003996A1 (en) * 2019-07-05 2021-01-14 中国矿业大学 Experimentation apparatus and method utilizing x-ray for measuring content and distribution of water in coal rock
CN113533676A (en) * 2021-07-23 2021-10-22 中国石油大学(华东) Laboratory simulation method for determining generation efficiency of natural gas hydrate in deep sea bottom

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004002754A (en) * 2002-03-28 2004-01-08 Mitsui Eng & Shipbuild Co Ltd Gas hydrate, method for producing the same and agent for suppressing decomposition of gas hydrate
CN105866144A (en) * 2016-05-26 2016-08-17 大连理工大学 Method for distinguishing aquo-complex phase from water phase through CT scanning
CN109406551A (en) * 2018-12-11 2019-03-01 吉林大学 A kind of analysis method for testing asphalt internal structure feature
WO2021003996A1 (en) * 2019-07-05 2021-01-14 中国矿业大学 Experimentation apparatus and method utilizing x-ray for measuring content and distribution of water in coal rock
CN113533676A (en) * 2021-07-23 2021-10-22 中国石油大学(华东) Laboratory simulation method for determining generation efficiency of natural gas hydrate in deep sea bottom

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
LIANG LEI等: "Pore-Scale Visualization of Methane Hydrate-Bearing Sediments With Micro-CT", 《GEOPHYSICAL RESEARCH LETTERS》, vol. 45, no. 11, pages 5419 - 5421 *
吴迪: "水合物生成分解过程相分辨和渗流特性研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》, pages 33 - 34 *
马应海;苟兰涛;何晓霞;刘芙蓉;: "四氢呋喃水合物零度以上生成动力学研究", 天然气地球科学, no. 02 *

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Application publication date: 20220211