CN1085834C - Selection of solution agent in electron nicroscope cryosolution method of crude petroleum system - Google Patents
Selection of solution agent in electron nicroscope cryosolution method of crude petroleum system Download PDFInfo
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- CN1085834C CN1085834C CN 98115390 CN98115390A CN1085834C CN 1085834 C CN1085834 C CN 1085834C CN 98115390 CN98115390 CN 98115390 CN 98115390 A CN98115390 A CN 98115390A CN 1085834 C CN1085834 C CN 1085834C
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Abstract
The present invention relates to selection of a solvent etching agent for a freezing solvent etching method of an electron microscope in a crude oil system. According to different sample characteristics, different organic solvents are selected to serve as the solvent etching agents to carry out solvent etching. After the spraying process is finished, the post processing is carried out on a copper net. The freezing solvent etching method of the electron microscope is applied to the crude oil system and other systems with high organic content. After the method is adopted, the clearness of the observation surfaces and the photographs is enhanced, the reproducibility of the microstructure is good, and the method can be used for the structure observation on systems of emulsification, emulsion breakage, etc. in tertiary oil recovery.
Description
The present invention relates to a kind of system of selection to corrosion agent in the electron microscope freezing and dissolving corrosion method of crude oil system
Combination flooding is the generally good method of people in the present intensified oil reduction, and it is low that it has a cost, and the characteristics that oil displacement efficiency is high are near the on-the-spot practical stage.But people lack understanding to the structure of matter form that exists in the composite displacement system, and its main cause is because it belongs to fluid sample, is dynamic system, and mass exchange speed is very fast in the system, and general means are difficult to observe.Therefore, Chinese patent 91105525.8 has at first been set up the freezing and dissolving corrosion technology of electron microscope, and it is used for the observation of pure system, has obtained effect preferably.But effect was undesirable when this patented technology observation contained crude oil sample.The present invention is directed to the problem of existence, and, develop a kind of system of selection at corrosion agent in the electron microscope freezing and dissolving corrosion method of crude oil system through a large amount of tests.
The system of selection of corrosion agent in the electron microscope freezing and dissolving corrosion method of the crude oil system that the objective of the invention is to develop, the difference that is characteristics per sample selects for use different organic solvents as corrosion agent corrosion, after spraying plating finishes again to copper mesh aftertreatment in addition, this method has reduced the pollution of crude oil, but increased sightingpiston, make the microcosmic of sample examine clear in structure ground and reproduce, same sample also has good structure repeatability when getting different parallel sample.This method can be used for crude oil, the complex system when kerosene is oil phase simultaneously, and different profits is when shown agent content alive and all can not used simultaneously, and sample making technology also is suitable for the oil and the water of other dark many components and the electron microscopic observation of the colloidal dispersion of the agent formation of showing to live.The establishing of this method helps the structure of matter form that forms behind the oil displacement agent and water effect in the deep understanding tertiary oil recovery, also helps deeply to be familiar with breakdown of emulsion mechanism on structure.
System of selection at corrosion agent in the electron microscope freezing and dissolving corrosion method of crude oil system of the present invention, select for use the little solvent of organic solvent-normal hexane, cyclohexane, normal heptane, dioxane, phenixin polarity in any two kinds of mixing of ratio in 1: 1 as the corrosion agent, with the sample freezing and dissolving corrosion, spraying plating platinum and carbon film then, be replicated on the copper mesh, mix the back washing with certain two kinds of material in 30-60 ℃ sherwood oil or ether or sherwood oil, ether and three kinds of materials of acetone by 1: 1 ratio again, again with the distilled water washing, dry and get final product.
Referring to accompanying drawing
Fig. 1 is that crude oil of the present invention, kerosin are the Electronic Speculum figure of oil phase
Fig. 2 is the Electronic Speculum figure of reverse microemulsion system of the present invention
Fig. 3 is the Electronic Speculum figure of oil phase with kerosene for the present invention
Further describe below in conjunction with accompanying drawing
Embodiment 1,
With the kerosin that contains 5% crude oil is oil phase, the lauryl sodium sulfate of 3% concentration is table agent alive, 6% normal butyl alcohol, isopropyl alcohol mixture is for helping table agent alive, table agent alive is that 2: 1 (weight ratio) is 20.05% o'clock preparation middle phase micro-emulsified liquid in salinity with helping table agent ratio alive, get the freezing sample preparation of 5 μ l samples during 25 ℃ of constant temperature, use normal hexane, after the corrosion agent corrosion of cyclohexane in 1: 1 ratio preparation, spraying plating platinum and carbon film, be replicated on the copper mesh, to the copper mesh petroleum ether, carry out going up after the washing and drying sem observation with redistilled water again and can obtain oil, the bicontinuous structure of the small block of water.
Embodiment 2,
With normal octane TX-100, hexanol preparation reverse microemulsion liquid system, it is freezing to get 5 μ l samples during 25 ℃ of constant temperature, with the corrosion agent corrosion of normal heptane, dioxane in 1: 1 ratio preparation, spraying plating platinum and carbon film, be replicated on the copper mesh, copper mesh is washed with ether, wash with redistilled water, the oven dry back local order that promptly can be observed surfactant on show is arranged and the nuclear of water wherein.
Embodiment 3,
With kerosene is oil phase, the lauryl sodium sulfate of 3% concentration is table agent alive, 6% normal butyl alcohol, isopropyl alcohol mixture is for helping table agent alive, table agent alive is 2: 1 (weight ratio) with helping table agent ratio alive, in salinity is 18.75% o'clock preparation middle phase micro-emulsified liquid, get the freezing sample preparation of 5 μ l samples during 25 ℃ of constant temperature, use dioxane, after the corrosion agent corrosion of phenixin in 1: 1 ratio preparation, spraying plating platinum and carbon film, be replicated on the copper mesh, to the copper mesh ether, sherwood oil mixes the back washing in 1: 1 ratio, washs with redistilled water again, and sem observation is gone up in the oven dry back can obtain the vesica structure.
Embodiment 4,
With normal octane TX-100, hexanol preparation reverse microemulsion liquid system, it is freezing to get 5 μ l samples during 25 ℃ of constant temperature, with the corrosion agent corrosion of normal heptane, cyclohexane in 1: 1 ratio preparation, spraying plating platinum and carbon film, be replicated on the copper mesh, copper mesh acetone, ether are mixed the back washing in 1: 1 ratio, wash with redistilled water, the oven dry back local order that promptly can be observed surfactant on show is arranged and the nuclear of water wherein.
Claims (1)
1, a kind of system of selection at corrosion agent in the electron microscope freezing and dissolving corrosion method of crude oil system, it is characterized in that selecting for use the little solvent of organic solvent-normal hexane, cyclohexane, normal heptane, dioxane, phenixin polarity in any two kinds of mixing of ratio in 1: 1 as the corrosion agent, with the sample freezing and dissolving corrosion, spraying plating platinum and carbon film then, be replicated on the copper mesh, mix the back washing with certain two kinds of material in sherwood oil or ether or sherwood oil, ether and three kinds of materials of acetone in 1: 1 ratio again, get final product with distilled water washing, oven dry again.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 98115390 CN1085834C (en) | 1998-07-16 | 1998-07-16 | Selection of solution agent in electron nicroscope cryosolution method of crude petroleum system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 98115390 CN1085834C (en) | 1998-07-16 | 1998-07-16 | Selection of solution agent in electron nicroscope cryosolution method of crude petroleum system |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1242515A CN1242515A (en) | 2000-01-26 |
| CN1085834C true CN1085834C (en) | 2002-05-29 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 98115390 Expired - Fee Related CN1085834C (en) | 1998-07-16 | 1998-07-16 | Selection of solution agent in electron nicroscope cryosolution method of crude petroleum system |
Country Status (1)
| Country | Link |
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| CN (1) | CN1085834C (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106681398B (en) * | 2017-02-15 | 2019-07-19 | 益和电气集团股份有限公司 | Temprature control method, system and the chamber of high low temperature cycles test case |
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1998
- 1998-07-16 CN CN 98115390 patent/CN1085834C/en not_active Expired - Fee Related
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| Publication number | Publication date |
|---|---|
| CN1242515A (en) | 2000-01-26 |
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