CN106596348A - Testing method for rock surface static contact angle and rock surface wettability dynamic change testing method utilizing testing method for rock surface static contact angle - Google Patents
Testing method for rock surface static contact angle and rock surface wettability dynamic change testing method utilizing testing method for rock surface static contact angle Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
- G01N13/02—Investigating surface tension of liquids
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
- G01N13/02—Investigating surface tension of liquids
- G01N2013/0208—Investigating surface tension of liquids by measuring contact angle
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Abstract
The invention particularly relates to a testing method for a rock surface static contact angle and a rock surface wettability dynamic change testing method utilizing the testing method for the rock surface static contact angle. The testing method for the rock surface static contact angle includes the steps that the surface of a rock slice is cleaned and dried for use; by means of a surface/tension meter, a sample cell capable of ascending and descending is filled with to-be-tested liquid, and the rock slice for use is clamped and suspended below a micro balance; testing is carried out by means of an 'Interfacial tension' mode, the sample cell slowly ascends during testing till the liquid level just makes contact with the lower surface of the rock slice, reading numbers displayed by the micro balance are recorded, and the stress magnitude (F) of the rock slice is calculated; the contact angle (theta) of the to-be-tested liquid on the surface of rock is deduced and obtained according to the stress magnitude (F) of the rock slice, wherein theta is shown as the formula shown in the specification. The testing method is high in sensitivity, the micro balance can capture the micro change of surface stress of the rock slice, and the small contact angle and the micro change of the contact angle can be tested; the continuous testing time is long, and the rock surface wettability dynamic change rule can be recorded.
Description
Technical field
The invention belongs to surface chemistry, a kind of analysis in Instrumental Analysis field, e measurement technology, and in particular to a kind of rock table
The method of testing of face static contact angle and the wettability of rock surface dynamic change method of testing using it.
Background technology
Wetability is a key property of reservoir rockses, and it is affect oil, water to be distributed in blowhole, flow one
Individual principal element, while oil, water two-phase relative permeability, capillary force and oil recovery are directly govern, by effectively tune
Section wettability of rock surface can reduce the injection pressure of LOW PERMEABILITY RESERVOIR, improve sandstone, the water suction of clastic rock oil reservoir injection well and cut open
Face, effective Remaining Oil, so as to effectively improve the exploitation effect of sandstone, clastic rock oil reservoir.Therefore correct understanding oil reservoir wetting
Property, it is of great significance for correct understanding oil reservoir and exploration improve all tools such as recovery ratio method.
Wettability of rock surface is substantially the intermolecular forces property and the macro manifestations of size of liquid and rock surface, surveys
Determine the phase interaction that the dynamic change of wettability of rock surface contributes between deep understanding rock surface chemical group and hydrone
With and from molecular level recognize reservoir rockses moistened surface mechanism.
At present laboratory wettability evaluation method mainly have Spontaneous imbibition rate method, drop measurement contact angle method, Amott methods,
USBM methods, nuclear magnetic resonance relaxation method, permeability saturation curve method.These methods to less contact angle values indeterminacy, to contact angle
Minor variations it is insensitive, accurate perception is difficult with the dynamic change of time of contact to contact angle.
Therefore a kind of sensitivity height, the wetability characterizing method of continuance test time length are needed at present.
The content of the invention
An object of the present invention is to provide a kind of sensitivity height, the rock surface static contact angle of continuance test time length
Method of testing.
The method of testing of rock surface static contact angle provided by the present invention, comprises the steps:
(1) it is standby by the surface clean of Rock laminate, drying;
(2) using surface/tensiometer, testing liquid is contained in liftable sample cell, clips standby Rock laminate, and
Under being suspended on microbalance, as shown in Figure 1;Tested using " Interfacial tension " pattern, sample cell during test
Slow to rise, until liquid level just contacts Rock laminate lower surface, record microbalance shows reading, and the stress for calculating Rock laminate is big
Little (F);
(3) contact angle (θ) according to stress size (F) the Derivation testing liquid of Rock laminate on a rock surface;
Wherein, F=m × g, m are microbalance reading, and g is acceleration of gravity;
L and t are respectively Rock laminate width and thickness;γLIt is surface tension of liquid;
R is the internal diameter of sample cell.
In said method step (1), the Rock laminate can for it is following any one:Quartz plate, mica sheet, potassium feldspar, sodium are long
Stone, dolomite, calcite, illite and chlorite.
The surface compact of the Rock laminate is smooth, and chemical reaction does not occur with testing liquid.
For rough Rock laminate, rock surface can be processed by shot blasting using chemical mechanical polishing technology;
The cross section of the Rock laminate is regular oblong, and its width and thickness are respectively l, t, wherein l<60mm, t<
5mm。
In said method step (2), the surface/tensiometer concretely type surfaces of DCAT 21/tensiometer.
The testing liquid can for it is following any one:Redistilled water, salting liquid, aqueous slkali, surfactant solution.
In the sample cell, the height of testing liquid is not less than 2cm.
The climbing speed of the sample cell is 0.7 μm of s-1~500mmmin-1, concretely with 3mmmin-1。
The stress size (F) of Rock laminate is multiplied by acceleration of gravity (g) and is calculated by microbalance reading (m).
In step (3), calculative parameter includes meniscus gravity w, negative buoyancy force F suffered by Rock laminate in derivationb、
During test in sample cell liquid levels and quartz plate lower surface difference in height h.
By Rock laminate gravity automatic clear, the stress size (F) of the Rock laminate is equal to meniscus weight to instrument before test
Power (w) and negative buoyancy force (F suffered by Rock laminateb) sum, i.e. F=w+Fb;Wherein described meniscus gravity (w) calculates according to formula (a)
Obtain,
W=2 (l+t) γLcosθ (a)
In formula, l and t is respectively Rock laminate width and thickness;γLIt is surface tension of liquid;
γLIt is surface tension of liquid, this parameter represents liquid self character.For example under the conditions of 20 DEG C, the interface of pure water
Tension force is 72.75mN/m, and the surface tension of octane is 21.62mN/m, thus this parameter it doesn't matter with the moment.
Liquid levels are shown with the difference in height h computing formula such as formula (b) of Rock laminate lower surface in the sample cell, ρ in formula
It is testing liquid density, g is acceleration of gravity, and r is the internal diameter of sample cell;
Negative buoyancy force (F suffered by the Rock laminateb) shown in computing formula such as formula (c);
Fb=l × t × h × ρ × g (c)
Shown in contact angle (θ) computing formula such as formula (d) of the testing liquid on Rock laminate;
Wherein, F=m × g, m are microbalance reading, and g is acceleration of gravity.
Liquid level is parallel with the Rock laminate lower surface for having hung all the time in sample cell uphill process, and experiment table top keeps nothing to shake
It is dynamic.
This method Range of measuring temp is:- 10~130 DEG C, can be controlled in sample cell by heating refrigeration mode circulator bath
Testing liquid temperature.
Active force (F) test scope in this method:0.1 μ N~2.1N, measuring accuracy is ± 1 μ N.
It is a further object of the present invention to provide a kind of method of testing using above-mentioned rock surface static contact angle carries out rock
The method of testing of stone surface wettability dynamic change.
The method of testing of the wettability of rock surface dynamic change is:According to the survey of above-mentioned rock surface static contact angle
Method for testing, Rock laminate is fixed, and in different time points, reads microbalance reading, substitute into formula (d) calculate it is a series of with
The contact angle (θ) of time of contact change, draws Rock laminate surface stress size, contact angle and the relation curve of time of contact.
The beneficial effect comprise that:(1) this kind of method of testing sensitivity is high:Microbalance can catch Rock laminate table
The micro change of stress on face, so as to test out the micro change of less contact angle and contact angle;(2) this kind of method is continuous
Testing time is long, can with non-volatile recording contact angle with time of contact increase and occur minor variations, so as to contribute to from point
Sublayer face recognizes reservoir rockses moistened surface mechanism.
Description of the drawings
Fig. 1 is the type surfaces of DCAT 21/tensiometer test schematic diagram;Wherein, 1 is microbalance;2 is Rock laminate;3 is sample
Product pond;4 is testing liquid;5 is lifting platform;6 is circulating water outlet;7 are circulation water inlet.
Fig. 2 is Rock laminate force analysis in a liquid;Wherein, 8 is testing liquid;9 is sample cell;10 is micro day
It is flat;11 is Rock laminate clip;12 is Rock laminate;13 is liquid meniscus.
Fig. 3 is quartz plate surface stress size, contact angle and time of contact when quartz plate contacts the certain pH value aqueous solution
Relation curve;
The relation of quartz plate surface stress size, contact angle and pH value under Fig. 4 different pH conditions.
Specific embodiment
Below by specific embodiment, the present invention will be described, but the invention is not limited in this.
Experimental technique used in following embodiments if no special instructions, is conventional method;Institute in following embodiments
Reagent, material etc., if no special instructions, commercially obtain.
A kind of method of testing of rock surface static contact angle provided by the present invention, can be by determining vertical hanging rock
The active force that flag surface applies to liquid is calculating contact angle of the liquid on Rock laminate surface.Comprise the steps:
(1) the smooth Rock laminate in surface is prepared, its surface clean is clean, and dried up with high pure nitrogen standby;(2) using DCAT 21
Type surface/tensiometer, contains testing liquid in liftable sample cell, and liquid height is not less than 2cm, clips standby rock
Piece, and be suspended under microbalance, as shown in figure 1, (lifting platform inner chamber the inside is empty, the water and constant temperature circulating of the inside in Fig. 1
Water in water-bath forms the temperature of water in circulation closed system, therefore the close thermostatical circulating water bath of lifting platform hull-skin temperature
Degree;There is a groove in the middle of in lifting platform profile, the external diameter of sample cell is just big as groove internal diameter, sample cell is contained and tested
It is put into after liquid in groove, therefore lifting platform outer surface can have heated constant temperature to act on liquid in sample cell, it is permanent by adjusting
Water temperature carrys out Control release test temperature in warm recirculated water bath), tested using " Interfacial tension " pattern,
Sample cell is with 3mmmin during test-1Speed slowly rise, until liquid level just contacts Rock laminate lower surface, record micro day
HUD shows reading, and the stress size (F) of Rock laminate is multiplied by acceleration of gravity (g) and is calculated by microbalance reading (m);(3)
According to the stress size Derivation liquid of Rock laminate contact angle (θ) on a rock surface,
Wherein, F=m × g, m are microbalance reading, and g is acceleration of gravity;
L and t are respectively Rock laminate width and thickness;γLIt is surface tension of liquid;
R is the internal diameter of sample cell.
Static contact angle method of testing of the invention, wherein, the Rock laminate includes that quartz plate, mica sheet, potassium are long
Stone, albite, dolomite, calcite, illite, chlorite,
Static contact angle method of testing of the invention, wherein, rock surface densification is smooth and liquid does not occur chemistry
The sample of reaction;
Static contact angle method of testing of the invention, wherein, for rough Rock laminate, using chemistry-
Mechanical polishing process is processed by shot blasting to rock surface;
Static contact angle method of testing of the invention, wherein, the cross section of Rock laminate is regular oblong, width and
Thickness is respectively l, t, wherein l<60mm, t<5mm;
In step (3), calculative parameter includes meniscus gravity w, negative buoyancy force F suffered by Rock laminate in derivationb、
During test in sample cell liquid levels and quartz plate lower surface difference in height h.
Static contact angle method of testing of the invention, wherein, front instrument is tested by Rock laminate gravity automatic clear, institute
The stress size (F) for stating Rock laminate is equal to meniscus gravity (w) and negative buoyancy force (F suffered by Rock laminateb) sum, i.e. F=w+Fb;Its
Described in meniscus gravity be calculated according to formula (a),
W=2 (l+t) γLcosθ (a)
In formula, l and t is respectively Rock laminate width and thickness;γLIt is surface tension of liquid;
Static contact angle method of testing of the invention, wherein, liquid levels and Rock laminate following table in the sample cell
Shown in the difference in height h computing formula such as formula (b) in face, ρ is fluid density in formula, and g is acceleration of gravity, and r is the internal diameter of sample cell;
Static contact angle method of testing of the invention, wherein, negative buoyancy force (F suffered by the Rock laminateb) computing formula
As shown in formula (c);
Fb=l × t × h × ρ × g (c)
Static contact angle method of testing of the invention, wherein, contact angle (θ) of the liquid on Rock laminate calculates public
Shown in formula such as formula (d);
Static contact angle method of testing of the invention, wherein, in uphill process liquid level all the time with the rock for having hung
Piece lower surface is parallel, and experiment table top keeps without friction.
Embodiment 1
Profit of the redistilled water on two kinds of various sizes of sheet glass (cover glass, quartz plate) is determined in the embodiment
It is moist.Redistilled water is put into into constant temperature 1h in clean sample cell before test;The clean sheet glass for drying up is clipped and is suspended on
Tested immediately on microbalance;Sample cell is with 3mmmin during test-1Speed slowly rise, until liquid level is just contacted
Sheet glass lower surface, liquid level is parallel with the sheet glass lower surface for having hung all the time in uphill process, and experiment table top keeps shockproof;
When liquid level just contacts sheet glass lower surface, because redistilled water is soaked to glass sheet surface, formed in glass sheet surface
Meniscus, redistilled water is applied active force by microbalance read-record sheet glass (F);Calculated by formula,
Obtain contact angle of the redistilled water in glass sheet surface.
Cover glass and quartz plate surface in the present embodiment is smooth;
Sheet glass cleaning method in the present embodiment is as follows:
(98% concentrated sulfuric acid and 30% hydrogen peroxide 7 in Piranha solution:3 (volume ratio) mixed solutions) in 90 DEG C of conditions
Lower immersion 1 hour;Glass sheet surface is rinsed repeatedly with redistilled water, is got off liquid pH value with the test flushing of pH test paper, until
Till the liquid shows neutral for rinsing.
The sheet glass cleaned in the embodiment is dried up using high pure nitrogen, is tested immediately after;
Note ensureing that sheet glass is vertical when sheet glass is hung in the embodiment, while ensureing lower surface and the liquid in sample cell
Face is parallel;
Contact angle θ computing formula are as follows in the embodiment:
Sheet glass stress size when F represents test in formula, l and t is respectively sheet glass width and thickness, is shown in Table 1;γLIt is
Surface tension of liquid, r is the internal diameter of sample cell, r=32.70mm.According to formula (a), (b), (c), (d), curved liquid is tried to achieve in calculating
Negative buoyancy force (F suffered by difference in height h of liquid levels and Rock laminate lower surface, Rock laminate in face gravity (w), sample cellb) and liquid
Contact angle (θ) on Rock laminate, result of calculation is shown in Table 1.
Table 1
As shown in table 1, contact angle of the redistilled water on two kinds of sheet glass is respectively 2.2 °, 2.9 °.With sheet glass
Larger, Rock laminate meniscus quality w is bigger, then the negative buoyancy force that liquid level falling head h and sheet glass are subject in sample cell
FbAlso it is bigger.
Contact angle very little of the redistilled water on two kinds of sheet glass, illustrates the static contact angle method of testing spirit of the present invention
Sensitivity is high, can measure the contact angle of very little.There is larger difference, but redistilled water two in the size of two kinds of sheet glass
The contact angle experiments result planted on sheet glass is close, illustrates that the method for testing is reappeared for the different size Rock laminate of material of the same race
Property preferably, while considering the necessity of negative buoyancy force in illustrating the computational methods of static contact angle;Forefathers experimental results demonstrate pure water
Contact angle is nearly equal to 0 on clean glass surface, and experimental result is very close with forefathers' experimental result in this embodiment, says
Clear the inventive method has reliability.
Embodiment 2
The Changing Pattern that the static contact angle on quartz surfaces extends with time of contact is tested by the method for example 1.
The reading that microbalance is recorded is multiplied by into acceleration of gravity (g=9.8N/kg) and obtains quartz plate stress size F, led to
Cross method in example 1 and ask for contact angle θ of the aqueous solution on quartz plate surface under the conditions of different times of contact, quartz plate stress is big
The contact angle of little F and the aqueous solution on quartz plate is as shown in Figure 3 with the relation curve of time of contact.
Fig. 3 shows that quartz plate stress F and contact angle θ extend the micro change for occurring with time of contact, illustrates this test
Method sensitivity is high, can record the micro change of contact angle, contributes to recognizing wettability of rock surface dynamic rule.With
Time of contact is elongated, and quartz plate stress F increase, aqueous solution contact angle θ on the glass sheet reduces, final balance.This be due to
As quartz plate is elongated with aqueous solution time of contact, part electroneutral silanol groups (≡ Si-OH) constantly dissociate on quartz surfaces
Into elecrtonegativity silanol groups (≡ Si-O-), the hydrophily of quartz surfaces strengthens, therefore quartz plate stress increases, and the aqueous solution is in stone
Contact angle θ on English piece reduces.
Embodiment 3
By contact angle of the method test different pH value of example 2 on quartz surfaces.By the side introduced in example 2
Method asks for the relation of contact angle θ of the different pH value aqueous solution on quartz plate and pH value, as shown in Figure 4.
As shown in Figure 4:As pH=2.3, quartz plate stress is minimum, and contact angle is maximum.Work as pH>When 2.3, with molten
Liquid pH value increases, and more electroneutral silanol groups dissociation on quartz surfaces generate elecrtonegativity silanol groups, therefore quartz surfaces
Stress increases, and hydrophily strengthens;Work as pH<When 2.3, due to H in solution+It is dense, the electroneutral silicon of part on quartz surfaces
Alcohol groups are converted into the higher electropositive silanol groups of hydrophily, and so as to show the increase of quartz surfaces stress, hydrophily strengthens.Knot
Fruit explanation the method sensitivity is high, the micro change of contact angle can be tested out, so as to contribute to understanding solution composition to rock table
The Regulation Mechanism of face wetability.
Claims (7)
1. a kind of method of testing of rock surface static contact angle, comprises the steps:
(1) it is standby by the surface clean of Rock laminate, drying;
(2) using surface/tensiometer, testing liquid is contained in liftable sample cell, clips standby Rock laminate, and hung
Under microbalance, tested using " Interfacial tension " pattern, sample cell slowly rises during test, until
Liquid level just contacts Rock laminate lower surface, and record microbalance shows reading, calculates the stress size (F) of Rock laminate;
(3) contact angle (θ) according to stress size (F) the Derivation testing liquid of Rock laminate on a rock surface;
Wherein, F=m × g, m are microbalance reading, and g is acceleration of gravity;
L and t are respectively Rock laminate width and thickness;γLIt is surface tension of liquid;
R is the internal diameter of sample cell.
2. method according to claim 1, it is characterised in that:In step (1), the Rock laminate for it is following any one:Stone
English piece, mica sheet, potassium feldspar, albite, dolomite, calcite, illite and chlorite;
The cross section of the Rock laminate is regular oblong, and its width and thickness are respectively l, t, wherein 10mm<l<30mm, t<
5mm。
3. method according to claim 1 and 2, it is characterised in that:In step (2), the testing liquid is following arbitrary
Kind:Redistilled water, salting liquid, aqueous slkali, surfactant solution;
In the sample cell, the height of testing liquid is not less than 2cm;
The climbing speed of the sample cell is 0.7 μm of s-1~500mmmin-1;
The stress size (F) of Rock laminate is multiplied by acceleration of gravity (g) and is calculated by microbalance reading (m).
4. the method according to any one of claim 1-3, it is characterised in that:Liquid level is all the time in sample cell uphill process
Parallel with the Rock laminate lower surface for having hung, experiment table top keeps without friction.
5. the method according to any one of claim 1-4, it is characterised in that:Methods described Range of measuring temp is:-10
~130 DEG C.
6. the method according to any one of claim 1-5, it is characterised in that:Active force (F) test model in methods described
Enclose:0.1 μ N~2.1N, measuring accuracy is ± 1 μ N.
7. a kind of method of testing of wettability of rock surface dynamic change, including:According to any one of claim 1-6
The method of testing of rock surface static contact angle, first fixes Rock laminate, in different time points, reads microbalance and reads
Number, calculates a series of contact angle θ changed with time of contact, when drawing Rock laminate surface stress size, contact angle with contacting
Between relation curve.
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CN107796737A (en) * | 2017-09-15 | 2018-03-13 | 深圳大学 | Metal bath soaks test device and the method for testing of substrate wettability |
CN107966403A (en) * | 2017-11-23 | 2018-04-27 | 中国工程物理研究院化工材料研究所 | A kind of apparatus and method for testing the micro- adhesion of non-infiltration solid-liquid interface |
CN109724898A (en) * | 2019-01-30 | 2019-05-07 | 湖北中烟工业有限责任公司 | A kind of detection method of cigarette tipping paper surface wettability |
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CN110411901A (en) * | 2018-04-26 | 2019-11-05 | 国家能源投资集团有限责任公司 | The evaluating apparatus of the wetting factor of the evaluation method and measurement electrode of liquid flow cell material of the wetting factor of electrode of liquid flow cell material |
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CN109991130A (en) * | 2019-04-17 | 2019-07-09 | 中国海洋石油集团有限公司 | The evaluation method of wettability of rock surface in a kind of rock-aqueous solution-crude oil system |
CN109991130B (en) * | 2019-04-17 | 2021-09-17 | 中国海洋石油集团有限公司 | Method for evaluating rock surface wettability in rock-water solution-crude oil system |
CN114062199A (en) * | 2020-07-31 | 2022-02-18 | 中国石油化工股份有限公司 | Method and device for testing surface energy of solid material |
CN112268840A (en) * | 2020-11-05 | 2021-01-26 | 山东电力研究院 | Test device and method for testing anti-wettability of coating |
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