CN105628577B - Large scale simulation model of microscopic production method - Google Patents

Large scale simulation model of microscopic production method Download PDF

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CN105628577B
CN105628577B CN201410638167.0A CN201410638167A CN105628577B CN 105628577 B CN105628577 B CN 105628577B CN 201410638167 A CN201410638167 A CN 201410638167A CN 105628577 B CN105628577 B CN 105628577B
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large scale
microscopic
simulation model
etching
scale simulation
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CN105628577A (en
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陈霆
陈亚宁
耿建梅
王曦
马炳杰
范菲
杨海博
苏法卿
刘津
姚风英
王磊
李继山
张玉利
刘丽
孟小海
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China Petroleum and Chemical Corp
Sinopec Shengli Geological Scientific Reserch Institute
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China Petroleum and Chemical Corp
Sinopec Shengli Geological Scientific Reserch Institute
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Abstract

The present invention provides a kind of large scale simulation model of microscopic production method, which includes according to research needs, and setting technique index makes the negative of large scale simulation model of microscopic;Photoetching, development and cleaning are carried out to large scale finished product chromium plate using negative;According to technical requirement, suitable corrosion reagent is selected, the chromium plate after development is performed etching;The good chromium plate of preliminary etching, then carries out punch operation, makes the import and export needed for experiment;The chromium plate of the large scale simulation model of microscopic prepared is cleaned repeatedly, ensures cleannes;Large scale simulation model of microscopic is subjected to high-temperature heating bonding.The large scale simulation model of microscopic production method solves the problems, such as that the effective coverage of model in current microscopic simulation test is too small, greatly improves the Research Ability of this experimental technique.

Description

Large scale simulation model of microscopic production method
Technical field
The present invention relates to oil field development technical fields, especially relate to a kind of large scale simulation model of microscopic making side Method.
Background technology
Currently, petroleum industry laboratory experiment improves the micromodel master used in the microcosmic Simulation technology of reservoir sweep of recovery ratio field There are two classes:Microvadose imitating model (the patent No.:) and true reservoir rock micro pore model and its system ZL00109777.6 Make the technology (patent No.:ZL93105170.3).Two class simulation model of microscopic are small-scale models, and effective area is in 1.5cm2Extremely 4cm2Between, small-scale model applies in microcosmic Simulation oil displacement experiment that there are following main problems:
1, Research Ability is limited
In the range of 4cm2, many experimental phenomenas are not obvious, and the experimental result contrast difference under the same terms is small, grinds It is weak to study carefully ability.For example, in the binary combination flooding experiment of research different formulations, need different under comparative analysis same experimental conditions The experimental result of binary system formula.It is tested in mini Mod, since the change of divergence is small, some experimental results can be caused to be neglected Slightly.And large scale micro-model test is utilized, the quantity and degree of variation are significantly larger than mini Mod, and Experimental comparison results are more clear Clear, research level is more deep.
2, stronger convincingness is lacked to the Study on Microcosmic Mechanism of oil displacement system sweep efficiency
The Study on Microcosmic Mechanism of oil displacement system sweep efficiency is to improve the important link of recovery efficiency technique, related by micro- During the special topic for seeing simulation experiment study sweep efficiency mechanism of oil displacement is reported and discussed, many experts and scholar are to microscopic simulation test Research involves problem and queries, and how the variation that problem concentrates on tens holes reflects and involve how people to be allowed to convince?Example Such as, in part Experiment under the conditions of mini Mod, wetability strong hydrophilicity, the initial waterline of water drive has involved all effective of mini Mod Region, further with experimental result go analysis involve problem really some reluctantly.And it is real to apply large scale micromodel to carry out It tests, whole pore area and hole quantity are to being significantly increased, and the distance of waterline migration increases, and the variation involved is more notable, gram The problem of water filling initial stage model is all involved is taken, undoubtedly, the mechanism study that involves microcosmic to oil displacement system has more convincingness.
Thus we have invented a kind of new large scale simulation model of microscopic production method, solves the above technical problem.
Invention content
The object of the present invention is to provide one kind on the basis of following glass etching basic principle, to its processing technology, sets The large scale simulation model of microscopic production method that standby flow and expansion using three levels improve and innovate.
The purpose of the present invention can be achieved by the following technical measures:
Large scale simulation model of microscopic production method, the large scale simulation model of microscopic production method include:Step 1, root It needs according to the study, setting technique index, makes the negative of large scale simulation model of microscopic;Step 2, using negative to large scale at Product chromium plate carries out photoetching, development and cleaning;Step 3, according to technical requirement, suitable corrosion reagent is selected, after development Chromium plate perform etching;Step 4, the good chromium plate of preliminary etching, then carries out punch operation, make needed for experiment into, Outlet;Step 5, the chromium plate of the large scale simulation model of microscopic prepared is cleaned repeatedly, ensures cleannes;Step 6, will Large scale simulation model of microscopic carries out high-temperature heating bonding.
The purpose of the present invention can be also achieved by the following technical measures:
In step 1, the material for making the negative of large scale simulation model of microscopic is quartz glass or pyrex 7740 Glass.
In step 3, when needing to carry out deep etching, capillary etching, with HF and NH4The mixed liquor of F is that etching is tried Agent, HF:NH4F=0.5-0.75:0.5-0.75 molar ratios, Clean after every time are 20h.
In step 3, when needing to carry out capillary etching, with HF and HNO3Mixed liquor be etching reagent, HF:HNO3 =0.5-0.75:0.5 molar ratio, Clean after every time are 20h.
In step 3, in needing to carry out when deep etching, capillary etching, with HF, NH4F and HN03Mixed liquor be Etch reagent, HF:NH4F:HNO3=0.75-1:0.5:0.5 molar ratio, Clean after every time are 20h.
In step 3, when needing to carry out deep etching, with HF, NH4The mixed liquor of F and HCL is etching reagent, HF: NH4F:HCL=0.75:0.5:0.5 molar ratio, Clean after every time are 20h.
In step 3, ranging from 20-50 DEG C of etching temperature.
In step 6, large scale simulation model of microscopic is horizontally arranged on large scale simulation model of microscopic dedicated platform, Large scale simulation model of microscopic platform and model are put into together in numerical control high temperature furnace, high-temperature heating bonding is carried out;Hyposmosis mould Type uses 690 DEG C, fires adhesive bonding method three times;Thief zone model uses 698 DEG C, fires adhesive bonding method twice;The large scale is micro- Simulation model dedicated platform surface smoothness is seen within 3 μm, and indeformable in 800 DEG C of high temperature.
The large scale simulation model of microscopic production method further includes, and after step 6, is burnt in large scale simulation model of microscopic After the completion of system, the etching quality of venturi is observed under the microscope.
The present invention relates to the underground fluids such as the petroleum gas big ruler that percolation law research institute applies in porous media The production method of very little microscopic glass simulation model is that petroleum industry in-house laboratory investigation improves microcosmic Simulation drive in recovery ratio field The core of oil tech.The present invention is the effective dimensions of microscopic glass model by original 4cm2Within be expanded to 10cm2, solution It has determined the too small problem in effective coverage of model in current microscopic simulation test, has greatly improved the research energy of this experimental technique Power, present invention is particularly suitable for the special items to oil displacement system sweep efficiency microcosmic mechanism, and experiment effect is more obvious, achievement More convincingness.The manufacturing technology of the present invention is on the basis of following glass etching basic principle, to its processing technology, equipment Flow and expansion are improved and have been innovated using three levels.Present invention is mainly used for the microcosmic Simulation displacement of reservoir oils in petroleum industry room Experiment, the research of be suitable for the mechanism of oil displacement of the oil displacement systems such as water drive and variety classes chemical flooding and improve recovery ratio etc., The present invention improves the research level and Research Ability of microcosmic Simulation oil displacement experiment technology so that result of study has more convincingness.
Description of the drawings
Fig. 1 is the flow chart of a specific embodiment of the large scale simulation model of microscopic production method of the present invention.
Specific implementation mode
For enable the present invention above and other objects, features and advantages be clearer and more comprehensible, it is cited below particularly go out preferable implementation Example, and coordinate institute's accompanying drawings, it is described in detail below.
As shown in FIG. 1, FIG. 1 is the flow charts of the large scale simulation model of microscopic production method of the present invention.In step 101, According to research needs, setting technique index (high and low permeability etc.) makes the negative of large scale simulation model of microscopic.Due to Glass has preferable chemical stability, large-scale spectrum penetrability, good thermal insulation and insulating properties, lower light absorption The base material of the advantages that coefficient, large scale simulation model of microscopic are 7740 glass of quartz glass or pyrex.Flow enters To step 102.
In step 102, according to the traditional machining processes of etching glass, using negative to large scale finished product chromium plate (by glass Substrate adds chromium film to constitute) carry out photoetching, development and cleaning.Flow enters step 103.
Suitable corrosion reagent is selected according to technical requirement in step 103, the chromium plate after development is performed etching, Pay attention to the control of temperature and time.The main method of glass etching is cleaning, gluing, photoetching, development and corrodes repeatedly.Glass is carved Generally using 46% hydrofluoric acid as etching agent, etching speed is higher for erosion, but glass surface quality is bad after etching, and Etching agent is serious to protection damage layer.Inevitable problem in side corrosion and etching and processing, influences the factor of side corrosion very It is more, such as:(1) selection of etchant;(2) the Clean after every time;(3) selection etc. of etching mode (equipment).
In the manufacturing process of large scale simulation model of microscopic, these contradictions become more prominent.It is difficult if processing is bad To obtain the microcosmic etching model for meeting experimental technique requirement.For example, making the hypotonic model and 120 microns that depth is 50 microns Hypertonic model, it is necessary to use different etching agent prescription and application method.
By testing repeatedly, the selection of etching reagent and its use for making large scale simulation model of microscopic can be wanted according to technology It asks and is carried out according to the following table, to obtain the higher product of quality.
Table 1 etches agent prescription and its scope of application
For etching the application method of reagent, following item is paid attention to.
(1)NH4F is conducive to improve etch rate as additive, but etching surface is of low quality.
(2)HNO3Ideal surface quality can be obtained as additive, but etch rate is not high, and had to layers of chrome relatively strong Destruction.
(3) HCI and HNO3It compares, etching surface quality is almost the same, but HCI small to the destruction of layers of chrome.
It (4) can be by NH4F、HNO3, HCI configure by a certain percentage, to obtain higher etch rate and preferable simultaneously Surface quality.
(5) etching temperature range is generally 20-50 DEG C, and etch rate increases with the raising of temperature.
Flow enters step 104.
In step 104, then the good model chromium plate of preliminary etching carries out punch operation, make needed for experiment into, Outlet.Flow enters step 105.
In step 105, the chromium plate of the large scale simulation model of microscopic prepared is cleaned repeatedly, ensures cleannes. In one embodiment, first heating being carried out with alcohol to clean, then being cleaned repeatedly with deionized water, glass is clear after guarantee etching Cleanliness.Flow enters step 106.
In step 106, model level is placed on large scale simulation model of microscopic dedicated platform, platform and model one It rises and is put into numerical control high temperature furnace, be accurately positioned, carry out high-temperature heating bonding.
In order to ensure the quality of large scale simulation model of microscopic, during the roughness on glass corrosion surface is modelling Need the key point strictly handled.In corrosion process, some insoluble matters are will produce, when insoluble matter deposits on the glass surface When, local mask will be formed, corrosion rate is on the one hand reduced, on the other hand increases the roughness of corrosion surface.
High temperature adhesives technology is to overcome a kind of effective ways of the roughness of glass surface, and by test, hyposmosis model is adopted With 690 DEG C, adhesive bonding method is fired three times;Thief zone model uses 698 DEG C, and better quality can be obtained by firing adhesive bonding method twice Simulation model of microscopic.
The large scale microscopic glass model dedicated platform surface of independent research needs to reach flatness and tool within 3 μm Hold the indeformable ability of resistance to 800 DEG C of high temperature.In one embodiment, testing to a variety of heat-resisting materials, the results are shown in Table 2.
The different heat-resisting materials of table 2 test table
According to test result, materials of the ceramic tile #3 as the dedicated platform of large scale simulation model of microscopic is determined.Flow into Enter to step 107.
In step 107, after the completion of large scale simulation model of microscopic is fired, the etching quality of venturi is observed under the microscope, Passed examination is completed spare.
The active porosity area of large and small size micromodel is by 4cm2Within be expanded to 10cm2.It is micro- using large scale one In the example for seeing the influence that Study on Simulation Model gravity migrate to remaining oil, model place vertically 10 days it is forward and backward compared, reality The influence situation of change that result explicitly reflects gravity to different types of remaining oils such as shape in flakes, island shape, cecum shapes is tested, And variation of experiment under the conditions of small size micromodel is very little, experimental analysis does not satisfy the requirements.The example is fully said Application value of the present invention in scientific research is illustrated.

Claims (6)

1. large scale simulation model of microscopic production method, which is characterized in that the large scale simulation model of microscopic production method includes:
Step 1, according to research needs, setting technique index makes the negative of large scale simulation model of microscopic;
Step 2, photoetching, development and cleaning are carried out to large scale finished product chromium plate using negative;
Step 3, according to technical requirement, suitable corrosion reagent is selected, the chromium plate after development is performed etching;
Step 4, then the good chromium plate of preliminary etching carries out punch operation, make the import and export needed for experiment;
Step 5, the chromium plate of the large scale simulation model of microscopic prepared is cleaned repeatedly, ensures cleannes;
Step 6, large scale simulation model of microscopic is subjected to high-temperature heating bonding;
In step 1, the material for making the negative of large scale simulation model of microscopic is 7740 glass of quartz glass or pyrex;
In step 3, when needing to carry out deep etching, capillary etching, with HF and NH4The mixed liquor of F is etching reagent, HF: NH4F=0.5-0.75:0.5-0.75 molar ratios, Clean after every time are 20h;
In step 6, large scale simulation model of microscopic is horizontally arranged on large scale simulation model of microscopic dedicated platform, big Size simulation model of microscopic platform and model are put into together in numerical control high temperature furnace, carry out high-temperature heating bonding;Hyposmosis model is adopted With 690 DEG C, adhesive bonding method is fired three times;Thief zone model uses 698 DEG C, fires adhesive bonding method twice;The large scale is microcosmic imitative True mode dedicated platform surface smoothness is and indeformable in 800 DEG C of high temperature within 3 μm.
2. large scale simulation model of microscopic production method according to claim 1, which is characterized in that in step 3, when need When carrying out capillary etching, with HF and HNO3Mixed liquor be etching reagent, HF:HNO3=0.5-0.75:0.5 molar ratio, clearly It is 20h to wash interval time.
3. large scale simulation model of microscopic production method according to claim 1, which is characterized in that in step 3, when need In carrying out when deep etching, capillary etching, with HF, NH4F and HN03Mixed liquor be etching reagent, HF:NH4F:HNO3= 0.75-1:0.5:0.5 molar ratio, Clean after every time are 20h.
4. large scale simulation model of microscopic production method according to claim 1, which is characterized in that in step 3, when need When carrying out deep etching, with HF, NH4The mixed liquor of F and HCL is etching reagent, HF:NH4F:HCL=0.75:0.5:0.5 rubs That ratio, Clean after every time are 20h.
5. large scale simulation model of microscopic production method according to claim 1, which is characterized in that in step 3, etching Temperature range is 20-50 DEG C.
6. large scale simulation model of microscopic production method according to claim 1, which is characterized in that the large scale is microcosmic imitative True mode production method further includes, and after step 6, after the completion of large scale simulation model of microscopic is fired, sees under the microscope Examine the etching quality of venturi.
CN201410638167.0A 2014-11-07 2014-11-07 Large scale simulation model of microscopic production method Expired - Fee Related CN105628577B (en)

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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
CN107831102B (en) * 2017-05-11 2020-06-16 中国石油化工股份有限公司 Method for simulating water film on rough surface of rock particles of oil reservoir
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

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1320818A (en) * 2001-04-23 2001-11-07 清华大学 Process for preparing capillary electrophoresis chip used in chemical analysis
CN1332368A (en) * 2000-07-07 2002-01-23 中国石油天然气总公司中国科学院渗流流体力学研究所 Making process of microvadose imitating model
CN101105120A (en) * 2007-04-20 2008-01-16 大庆石油学院 three-dimensional glass porous media model for microcosmic oil drive and manufacturing method thereof
CN102979516A (en) * 2012-11-29 2013-03-20 西南石油大学 Workmanship of indoor microscopic oil displacement model
CN203515528U (en) * 2013-10-09 2014-04-02 中国石油大学(华东) Glass model used for displacement micro-experiments

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1332368A (en) * 2000-07-07 2002-01-23 中国石油天然气总公司中国科学院渗流流体力学研究所 Making process of microvadose imitating model
CN1320818A (en) * 2001-04-23 2001-11-07 清华大学 Process for preparing capillary electrophoresis chip used in chemical analysis
CN101105120A (en) * 2007-04-20 2008-01-16 大庆石油学院 three-dimensional glass porous media model for microcosmic oil drive and manufacturing method thereof
CN102979516A (en) * 2012-11-29 2013-03-20 西南石油大学 Workmanship of indoor microscopic oil displacement model
CN203515528U (en) * 2013-10-09 2014-04-02 中国石油大学(华东) Glass model used for displacement micro-experiments

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
中高渗砂岩油藏水驱油效果及波及规律研究;李奋;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20100315(第3期);第1章、第4章 *

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