CN1107860C - Making process of microvadose imitating model - Google Patents

Making process of microvadose imitating model Download PDF

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Publication number
CN1107860C
CN1107860C CN 00109777 CN00109777A CN1107860C CN 1107860 C CN1107860 C CN 1107860C CN 00109777 CN00109777 CN 00109777 CN 00109777 A CN00109777 A CN 00109777A CN 1107860 C CN1107860 C CN 1107860C
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China
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microvadose
making
transparent
model
imitating
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Expired - Fee Related
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CN 00109777
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Chinese (zh)
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CN1332368A (en
Inventor
胡雅仍
郭尚平
黄延章
周娟
马效武
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CHINA PETROLEUM GAS CORP
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CHINA PETROLEUM GAS CORP
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Abstract

The present invention relates to a making method of a seepage model for the research on underground fluids, such as petroleum, natural gas, etc., in porous media. The method is characterized in that a photochemical etching technology is adopted, the pore structures of natural core slices are accurately photoetched on a piece of plane optical glass, and the seepage model is formed by sintering at high temperature after hydrofluoric acid etching. The method has the advantages that the model is easy to observe, the model can be modified and regenerated as needed, and the wetting property of porous media and the diversity of the roughness can be truly reflected so that experiments and tests for fluids in stratums can become accurate.

Description

The method for making of microvadose imitating model
The present invention relates to making, modification and the regeneration techniques of percolation model, is a kind of method for making of microvadose imitating model.
The research Seepage problems of fluid in porous medium has crucial meaning for the antiseepage of exploitation, ground surface works and the river dykes and dams of underground fluid resources such as petroleum gas etc.But for a long time, adopt the method for macroscopic view for the research of Seepage problems in the porous medium more, with natural core or artificial geologic model is research object, can only infer the situation of seepage flow core or the model from parameters such as the pressure reduction of measuring turnover core or model two ends fluid, flows, and can not observe directly the concrete situation of fluid motion in the porous system and the details such as interaction of fluid and pore surface.For simulate and observe microscopic seepage in the porous medium dynamically, nineteen fifty-two Chatenever[AIME, V.192 (1952)] develop single-glass pearl model, and immiscible two-phase seepage flow is observed; [Oil and GasJ., No.42 (1961)] such as Mattax developed microtriche managed network model in 1961, and observed the oil-water seepage state; Donaldson[SPE of AIME in 1971,46 Th.Fall Meeting Vol.2 (1971)] announced a kind of silica sand sandwich mould, be used for studying the distribution of oil in the wet structure of water.The advantage of these models is transparent, can be by the detail of the inner seepage flow of observation instrument Direct observation models such as microscope.But all these artificial models' pore texture all is Utopian design, can not reflect pore texture complicated and changeable in the real porous medium, as the situation of mesoporosity, stratum structure; Simultaneously these artificial models' wetting state and roughness also are changeless, can not reflect the diversity of wetting state and roughness in the true porous medium equally; And when these models of application are studied the seepage flow of such complicated component of image-stone oil and viscous fluid, owing to reasons such as absorption, viscous, being easy to stop up the seepage channel of model inside, and don't easy cleaning, just can not use again afterwards to cause these models often to use once.
The objective of the invention is to overcome above-mentioned the deficiencies in the prior art, a kind of easy observation, correctability and regeneration are provided, can truly reflect the method for making of the multifarious microvadose imitating model of wetting state and roughness in the porous medium.
Technical solution of the present invention is as follows:
Adopt the photochemical etching technical matters, the accurate photoetching of pore texture of natural core section is on glass to plane optics, and the high temperature sintering moulding is made after hydrofluoric acid etch.
Its detailed process is:
A. natural core is cut into thin slice and extracting oven dry, inject the thermosetting plastics of dyeing under vacuum condition, pressurization is also ground;
B. use the positive film to the pore passage structure photomicrograph in the core, carry out micro photography with negative film again and become film;
C. the one side at two blocks of glass plates metal film, coats photoresist; Film is covered on glass and photoetching under ultraviolet light behind the plated film;
D. and then with the another side of glass plate after the photoetching coat antiseptic wax, put into the hydrofluorite etching;
E. the one side that glass plate is had indentation is overlapping relatively, puts sinter molding in the high temperature furnace into.
The present invention also provides following technical scheme:
Sintering temperature is at 500 ℃~600 ℃ in the high temperature furnace.
The concentration of hydrofluorite is controlled at 20%~50%, can add phosphoric acid as corrosion inhibiter when hydrofluoric acid etch.
The model of sinter molding immersion treatment in solution of silane, the concentration of solution of silane are 0.3%~1.5%, and the model of sinter molding soak time in solution of silane is 15~25 minutes.
Model can be regenerated with sherwood oil cleaning, high-temperature baking, alkaline soak.
The high-temperature baking temperature of model regeneration is 500 ℃~600 ℃, and the time is 9 hours.
The invention has the advantages that: model is easy to observe, and modification and regeneration as required may truly reflect the diversity of wetting state and roughness in the porous medium, and it is more accurate with test to make the experiment of stratum inner fluid.
Embodiment of the invention process is as follows:
Make the core thin slice: natural core is cut into thin slice, after the extracting oven dry, inject the thermosetting plastics of dyeing under vacuum condition, pressurization, moulding, grinding stick on the glass sheet with Arabic gum;
The positive film is to the photomicrograph of core thin slice, and the splicing photo is depicted in the pore passage structure in the core (being that coloured plastics plants oneself) in the tracing paper, carries out micro photography with the negative film film with certain multiple again, with stand-by behind the film rinsing;
The planar optics glass plate of two identical sizes of system belongs to film in its one side plated with gold respectively, coats photoresist; Processed film is covered on the glass plate with photoresist one side, under ultraviolet light, carry out photoetching, and then the another side of the glass plate that photoetching, burn into clean, oven dry is good is coated antiseptic wax, put into the hydrofluorite etching;
Glass plate is taken out flushing, airing from hydrofluorite, the one side that will have indentation overlaps relatively, puts sinter molding in the high temperature furnace in the lump into, temperature is controlled at about 550 ℃ in the stove, too high possibility molten glass plate makes indentation make up, crosses to hang down two blocks of glass are combined into one.
In order to change the roughness of this microvadose imitating model, make it to reflect the diversity of true porous medium mesoporosity roughness, the present invention is controlled at 20%~50% with the concentration of hydrofluorite in the modelling process, can add an amount of phosphoric acid as corrosion inhibiter.Can change the hole roughness by control hydrofluoric acid concentration, the time of corrosion, the consumption of phosphoric acid.As hydrofluoric acid concentration 40%, 1~3 minute time of corrosion, can generate the imbricated texture surface, at 1 minute with the interior smooth surface that generates.
The microvadose imitating model of sinter molding, the wetting state of itself is hydrophilic, the lipophilicity or the neutral situation that exist in the true porous medium for model can be reflected, the present invention adopts the principle of silane and glass bonding, model is carried out immersion treatment, with the difference of silane concentration, model can present different wetting states, shows neutral or inclined to one side lipophilicity.As soaking 20 minutes, silane concentration 0.7% shows neutral, greater than 0.7% apparent lipophilicity, shows water wettability less than 0.7%.
Silane of the present invention can adopt dimethyldichlorosilane, diphenyl dichlorosilane, trichlorine dodecyl silane, trimethyl chlorinated silane, and the solvent of employing can be used benzene.
But the present invention's model adopts alkaline soak or sherwood oil to clean, and adopts the method for high-temperature baking can recover the virgin state of model again, and baking temperature should be controlled at 500 ℃~600 ℃, and the time is 9 hours.Through the model that this method was handled, can reuse.

Claims (10)

1. the method for making of a transparent microvadose imitating model is characterized in that: adopt the photochemical etching technical matters, the accurate photoetching of pore texture of natural core section is on glass to plane optics, and the high temperature sintering moulding is made after hydrofluoric acid etch.
2. the method for making of transparent microvadose imitating model according to claim 1, its detailed process is:
A. natural core is cut into thin slice and extracting oven dry, inject the thermosetting plastics of dyeing under vacuum condition, pressurization is also ground;
B. use the positive film to the pore passage structure photomicrograph in the core, carry out micro photography with negative film again and become film;
C. the one side at two blocks of glass plates metal film, coats photoresist; Again film is covered the on glass of metal-coated membrane and photoetching under ultraviolet light;
D. and then with the another side of glass plate after the photoetching coat antiseptic wax, put into the hydrofluorite etching;
E. the one side that glass plate is had indentation is overlapping relatively, puts sinter molding in the high temperature furnace into.
3. the method for making of transparent microvadose imitating model according to claim 1, it is characterized in that: the high temperature sintering forming temperature is at 500 ℃~600 ℃.
4. the method for making of transparent microvadose imitating model according to claim 1, it is characterized in that: the concentration of hydrofluorite is controlled at 20%~50%.
5. according to the method for making of claim 1 or 4 described transparent microvadose imitating models, it is characterized in that: when hydrofluoric acid etch, can add phosphoric acid as corrosion inhibiter.
6. the method for making of transparent microvadose imitating model according to claim 1 is characterized in that: the model of sinter molding immersion treatment in solution of silane.
7. the method for making of transparent microvadose imitating model according to claim 6, it is characterized in that: the concentration of solution of silane is 0.3%~1.5%.
8. the method for making of transparent microvadose imitating model according to claim 6, it is characterized in that: the model of sinter molding soak time in solution of silane is 15~25 minutes.
9. the method for making of transparent microvadose imitating model according to claim 1 is characterized in that: model can be with sherwood oil cleaning, high-temperature baking, alkaline soak regeneration.
10. the method for making of transparent microvadose imitating model according to claim 9 is characterized in that: the high-temperature baking temperature of model regeneration is 500 ℃~600 ℃, and the time is 9 hours.
CN 00109777 2000-07-07 2000-07-07 Making process of microvadose imitating model Expired - Fee Related CN1107860C (en)

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Application Number Priority Date Filing Date Title
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US7496488B2 (en) * 2003-03-06 2009-02-24 Schlumberger Technology Company Multi-scale finite-volume method for use in subsurface flow simulation
CN101105120B (en) * 2007-04-20 2010-12-22 大庆石油学院 Three-dimensional glass porous media model for microcosmic oil drive and manufacturing method thereof
CN102031965B (en) * 2010-06-30 2013-08-21 中国石油大学(北京) Oil-gas reservoir physical simulation wellbore radius processing method
CN102768812B (en) * 2011-05-06 2015-02-11 中国科学院理化技术研究所 Visual microscopic model of real core and manufacturing method thereof
CN102494972B (en) * 2011-11-21 2014-03-26 北京科技大学 Manufacturing method of wwo-dimensional heat curing porous medium model for microscopic oil displacement
CN103471882B (en) * 2013-08-20 2015-08-05 中国石油天然气股份有限公司 Manufacturing method of visual totally-enclosed real core model and core model
CN105626005B (en) * 2014-10-30 2019-03-08 中国科学院地质与地球物理研究所 Visualization plane glass model and preparation method thereof
CN105628577B (en) * 2014-11-07 2018-10-30 中国石油化工股份有限公司 Large scale simulation model of microscopic production method
CN104502253A (en) * 2015-01-22 2015-04-08 中国石油大学(华东) Capillary tube microcosmic inhalation oil displacement image collection device and work method thereof
CN105869496A (en) * 2016-06-02 2016-08-17 北京科技大学 Visual micro-pore structure simulation physical model and manufacturing method thereof
CN110563340B (en) * 2019-08-26 2022-01-11 中国石油化工股份有限公司 Manufacturing method of micro glass model with middle-permeation core
CN114011478B (en) * 2021-02-20 2023-06-02 中国海洋石油集团有限公司 Multifunctional microfluidic chip and manufacturing method thereof
CN114575799A (en) * 2022-03-08 2022-06-03 西南石油大学 Experimental device based on nanometer-micro-nano pore structure displacement process

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