CN106596348B - Rock surface static contact angle and its wetability dynamic change test method - Google Patents
Rock surface static contact angle and its wetability dynamic change test method Download PDFInfo
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- CN106596348B CN106596348B CN201611203555.1A CN201611203555A CN106596348B CN 106596348 B CN106596348 B CN 106596348B CN 201611203555 A CN201611203555 A CN 201611203555A CN 106596348 B CN106596348 B CN 106596348B
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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
Abstract
Present invention relates particularly to a kind of test method of rock surface static contact angle and utilize its wettability of rock surface dynamic change test method.The test method of rock surface static contact angle, comprising: spare by the surface clean of Rock laminate, drying;Using surface/tensiometer, testing liquid is contained in liftable sample cell, clips spare Rock laminate, and be suspended under microbalance;It is tested using " Interfacial tension " mode, sample cell slowly rises when test, and until liquid level just contacts Rock laminate lower surface, record microbalance display reading calculates the stress size (F) of Rock laminate;According to the contact angle (θ) of stress size (F) the Derivation testing liquid of Rock laminate on a rock surface;
Description
Technical field
The invention belongs to surface chemistries, a kind of analysis of instrument analysis field, measuring technique, and in particular to a kind of rock table
The test method of face static contact angle and the wettability of rock surface dynamic change test method for utilizing it.
Background technique
Wetability is a key property of reservoir rocks, it is to influence oil, one that water is distributed in blowhole, flows
A principal element, while oil, water two-phase relative permeability, capillary force and oil recovery are directly restrict, by effectively adjusting
Section wettability of rock surface can reduce the injection pressure of LOW PERMEABILITY RESERVOIR, and the water suction for improving sandstone, clastic rock oil reservoir injection well is cutd open
Face, effective Remaining Oil, to effectively improve the exploitation effect of sandstone, clastic rock oil reservoir.Therefore correct understanding oil reservoir wetting
Property, it improves recovery ratio method etc. for correctly recognizing oil reservoir and exploration and all has a very important significance.
Wettability of rock surface is substantially the macro manifestations of active force property and size between liquid and rock surface, is surveyed
The dynamic change for determining wettability of rock surface facilitates the phase interaction goed deep between understanding rock surface chemical group and hydrone
Reservoir rocks moistened surface mechanism is recognized with and from molecular level.
At present laboratory wettability evaluation method mainly have Spontaneous imbibition rate method, drop measurement contact angle method, Amott method,
USBM method, nuclear magnetic resonance relaxation method, permeability saturation curve method.These methods are to smaller contact angle values indeterminacy, to contact angle
Minor change it is insensitive, accurate perception is difficult with the dynamic change of time of contact to contact angle.
Therefore the wetability characterizing method for needing a kind of high sensitivity, continuance test time long at present.
Summary of the invention
An object of the present invention is to provide a kind of high sensitivity, continuance test time long rock surface static contact angle
Test method.
The test method of rock surface static contact angle provided by the present invention, includes the following steps:
(1) spare by the surface clean of Rock laminate, drying;
(2) surface/tensiometer is used, testing liquid is contained in liftable sample cell, clips spare Rock laminate, and
It is suspended under microbalance, as shown in Figure 1;It is tested using " Interfacial tension " mode, sample cell when test
Slowly rise, until liquid level just contacts Rock laminate lower surface, record microbalance display is read, and the stress for calculating Rock laminate is big
Small (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 is Rock laminate width and thickness respectively;γLIt is surface tension of liquid;
R is the internal diameter of sample cell.
In above method step (1), the Rock laminate can be following any: 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 does not chemically react with testing liquid.
For rough Rock laminate, chemical mechanical polishing technology can be used, rock surface is processed by shot blasting;
The cross section of the Rock laminate is regular oblong, and width and thickness is respectively l, t, wherein l < 60mm, t <
5mm。
In above method step (2), the surface/tensiometer concretely 21 type surface DCAT/tensiometer.
The testing liquid can be following any: secondary distilled 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 calculated by microbalance reading (m) multiplied by acceleration of gravity (g).
In step (3), calculative parameter includes meniscus gravity w, negative buoyancy force F suffered by Rock laminate in derivation processb、
When test in sample cell liquid levels and quartz plate lower surface difference in height h.
For instrument by Rock laminate gravity automatic clear, the stress size (F) of the Rock laminate is equal to meniscus weight before testing
Negative buoyancy force (F suffered by power (w) and Rock laminatebThe sum of), i.e. F=w+Fb;Wherein the meniscus gravity (w) calculates according to formula (a)
It obtains,
W=2 (l+t) γLcosθ (a)
In formula, l and t are Rock laminate width and thickness respectively;γLIt is surface tension of liquid;
γLIt is surface tension of liquid, this parameter represents liquid self character.Such as under the conditions of 20 DEG C, the interface of pure water
Tension is 72.75mN/m, and the surface tension of octane is 21.62mN/m, therefore this parameter and moment are not related.
Liquid levels and the difference in height h calculation formula such as formula (b) of Rock laminate lower surface are shown 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 calculation formula such as formula (c);
Fb=l × t × h × ρ × g (c)
Shown in contact angle (θ) calculation 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 hung always in sample cell uphill process, and experiment table top is kept without vibration
It is dynamic.
This method Range of measuring temp are as follows: -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 are ± 1 μ N.
It is a further object of the present invention to provide a kind of test methods using above-mentioned rock surface static contact angle to carry out rock
The test method of stone surface wettability dynamic change.
The test method of the wettability of rock surface dynamic change are as follows: according to the survey of above-mentioned rock surface static contact angle
Method for testing fixes Rock laminate, in different times point, read microbalance reading, substitute into formula (d) calculate it is a series of with
The contact angle (θ) of time of contact variation, draws the relation curve of Rock laminate surface stress size, contact angle and time of contact.
The beneficial effect comprise that: (1) such test method high sensitivity: microbalance can capture Rock laminate table
The micro variation of stress on face, so as to test out the micro change of lesser contact angle and contact angle;(2) such method is continuous
Testing time is long, can with non-volatile recording contact angle with time of contact increase and occur minor change, thus facilitate from point
Sublayer face recognizes reservoir rocks moistened surface mechanism.
Detailed description of the invention
Fig. 1 is the 21 type surface DCAT/tensiometer test schematic diagram;Wherein, 1 is microbalance;2 be Rock laminate;3 be sample
Product pond;4 be testing liquid;5 be lifting platform;6 be circulating water outlet;7 be circulation water inlet.
Fig. 2 is the force analysis of Rock laminate in a liquid;Wherein, 8 be testing liquid;9 be sample cell;10 be micro day
It is flat;11 be Rock laminate clip;12 be Rock laminate;13 be liquid meniscus.
Fig. 3 is quartz plate surface stress size, contact angle and time of contact when quartz plate contacts certain pH value aqueous solution
Relation curve;
Quartz plate surface stress size, the relationship of contact angle and pH value under Fig. 4 different pH condition.
Specific embodiment
The present invention will be described below by way of specific embodiments, but the present invention is not limited thereto.
Experimental method used in following embodiments is conventional method unless otherwise specified;Institute in following embodiments
Reagent, material etc., are commercially available unless otherwise specified.
A kind of test method of rock surface static contact angle provided by the present invention can pass through measurement vertical hanging rock
Contact angle of the liquid on Rock laminate surface is calculated in active force that flag surface applies liquid.Include the following steps:
(1) the smooth Rock laminate in preparation surface is clean by its surface clean and spare with high pure nitrogen drying;(2) DCAT 21 is used
Type surface/tensiometer, contains testing liquid in liftable sample cell, and liquid height is not less than 2cm, clips spare rock
Piece, and be suspended under microbalance, as shown in Figure 1, (lifting platform inner cavity the inside is empty, the water and constant temperature circulating of the inside in Fig. 1
Water in water-bath forms circulation closed system, therefore lifting platform hull-skin temperature is close to the temperature of water in thermostatical circulating water bath
Degree;Intermediate in lifting platform shape to have a groove, the outer diameter of sample cell is just big as groove internal diameter, and sample cell is contained and tested
It is put into groove after liquid, therefore lifting platform outer surface can have heated constant temperature effect to liquid in sample cell, it is permanent by adjusting
Water temperature tests test temperature to control in warm recirculated water bath), it is tested using " Interfacial tension " mode,
Sample cell is when test with 3mmmin-1Rate slowly rise, until liquid level just contacts Rock laminate lower surface, record micro day
Head up display shows reading, and the stress size (F) of Rock laminate is calculated by microbalance reading (m) multiplied by acceleration of gravity (g);(3)
According to the contact angle (θ) of the stress size Derivation 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 is Rock laminate width and thickness respectively;γLIt is surface tension of liquid;
R is the internal diameter of sample cell.
Static contact angle test method according to the present invention, wherein the Rock laminate includes that quartz plate, mica sheet, potassium are long
Stone, albite, dolomite, calcite, illite, chlorite,
Static contact angle test method according to the present invention, wherein rock surface densification is smooth, chemistry does not occur with liquid
The sample of reaction;
Static contact angle test method according to the present invention, wherein for rough Rock laminate, using chemistry-
Mechanical polishing process is processed by shot blasting rock surface;
Static contact angle test method according to the present invention, wherein the cross section of Rock laminate be 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 derivation processb、
When test in sample cell liquid levels and quartz plate lower surface difference in height h.
Static contact angle test method according to the present invention, wherein test preceding instrument for Rock laminate gravity automatic clear, institute
The stress size (F) for stating Rock laminate is equal to negative buoyancy force (F suffered by meniscus gravity (w) and Rock laminatebThe sum of), 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 are Rock laminate width and thickness respectively;γLIt is surface tension of liquid;
Static contact angle test method according to the present invention, wherein liquid levels and Rock laminate following table in the sample cell
Shown in the difference in height h calculation 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 test method according to the present invention, wherein negative buoyancy force (F suffered by the Rock laminateb) calculation formula
As shown in formula (c);
Fb=l × t × h × ρ × g (c)
Static contact angle test method according to the present invention, wherein contact angle (θ) of the liquid on Rock laminate is calculated public
Shown in formula such as formula (d);
Static contact angle test method according to the present invention, wherein in uphill process liquid level always with the rock that has hung
Piece lower surface is parallel, and experiment table top keeps without friction.
Embodiment 1
Profit of the secondary distilled water on two kinds of various sizes of sheet glass (coverslip, quartz plate) is determined in the embodiment
It is moist.Secondary distilled water is put into constant temperature 1h in clean sample cell before test;The sheet glass of clean drying is clipped and is suspended on
It is tested immediately on microbalance;Sample cell is when test with 3mmmin-1Rate slowly rise, until liquid level just contacts
Sheet glass lower surface, liquid level is parallel with the sheet glass lower surface hung always in uphill process, and experiment table top keeps shockproof;
When liquid level just contacts sheet glass lower surface, since secondary distilled water soaks glass sheet surface, formed in glass sheet surface
Meniscus, the active force that secondary distilled water is applied by microbalance read-record sheet glass (F);It is calculated by formula,
Obtain contact angle of the secondary distilled water in glass sheet surface.
Coverslip 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 7:3 (volume ratio) mixed solution) is in 90 DEG C of conditions in Piranha solution
It is lower to impregnate 1 hour;With secondary distilled water repeated flushing glass sheet surface, liquid pH value is rinsed with the test of pH test paper, until
Until the liquid shows neutral rinsed.
The sheet glass cleaned in the embodiment is dried up using high pure nitrogen, is tested immediately after;
Pay attention to guaranteeing that sheet glass is vertical when hanging sheet glass in the embodiment, while guaranteeing the liquid in lower surface and sample cell
Face is parallel;
Contact angle θ calculation formula is as follows in the embodiment:
F indicates sheet glass stress size when test in formula, and l and t are sheet glass width and thickness respectively, are shown in Table 1;γLIt is
Surface tension of liquid, r are the internal diameter of sample cell, r=32.70mm.According to formula (a), (b), (c), (d), calculating acquires curved liquid
Negative buoyancy force (F suffered by the difference in height h, Rock laminate of liquid levels and Rock laminate lower surface in face gravity (w), sample cellb) and liquid
Contact angle (θ) on Rock laminate, calculated result is shown in Table 1.
Table 1
As shown in table 1, contact angle of the secondary distilled 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 bigger.
Contact angle very little of the secondary distilled water on two kinds of sheet glass illustrates static contact angle test method spirit of the invention
Sensitivity is high, can measure the contact angle of very little.There are larger differences for the size of two kinds of sheet glass, but secondary distilled water is two
Contact angle experiments result on kind sheet glass is close, illustrates that the test method reappears the different size Rock laminates of material of the same race
Property it is preferable, while illustrating the necessity that negative buoyancy force is considered in the calculation method of static contact angle;Experimental results demonstrate pure water by forefathers
Contact angle is nearly equal to 0 on clean glass surface, and experimental result and forefathers' experimental result are very close in this embodiment, says
The method of the present invention, which is illustrated, has reliability.
Embodiment 2
The static contact angle on quartz surfaces is tested with time of contact extended changing rule by the method for example 1.
The reading that microbalance records is obtained into quartz plate stress size F multiplied by acceleration of gravity (g=9.8N/kg), is led to
It crosses method in example 1 and seeks 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 relation curve of the contact angle and time of contact of small F and aqueous solution on quartz plate is as shown in Figure 3.
Fig. 3 shows that quartz plate stress F and contact angle θ extend the micro variation occurred with time of contact, illustrates this test
Method high sensitivity can record the micro change of contact angle, help to recognize wettability of rock surface dynamic rule.With
Time of contact is elongated, and quartz plate stress F increases, and the contact angle θ of aqueous solution on the glass sheet reduces, final to balance.This is because
As quartz plate and aqueous solution time of contact are elongated, part electroneutral silanol groups (≡ Si-OH) are constantly dissociated on quartz surfaces
At elecrtonegativity silanol groups (≡ Si-O-), the hydrophily enhancing of quartz surfaces, therefore quartz plate stress increases, aqueous solution is in stone
The contact angle θ of English on piece reduces.
Embodiment 3
By contact angle of the method test different pH value of example 2 on quartz surfaces.Pass through the side introduced in example 2
Method seeks the relationship of different pH value aqueous solution the contact angle θ 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 value.As pH > 2.3, with molten
Liquid pH value increases, and more electroneutral silanol groups dissociation generate elecrtonegativity silanol groups, therefore quartz surfaces on quartz surfaces
Stress increases, hydrophily enhancing;As pH < 2.3, due to H in solution+It is dense, the electroneutral silicon of part on quartz surfaces
Alcohol groups are converted into the stronger electropositive silanol groups of hydrophily, so that the increase of quartz surfaces stress is showed, hydrophily enhancing.Knot
Fruit illustrates this method high sensitivity, can test out the micro change of contact angle, to help to understand solution composition to rock table
The Regulation Mechanism of face wetability.
Claims (7)
1. a kind of test method of rock surface static contact angle, includes the following steps:
(1) spare by the surface clean of Rock laminate, drying;
(2) surface/tensiometer is used, testing liquid is contained in liftable sample cell, clips spare Rock laminate, and hang
Under microbalance, to be tested using " Interfacial tension " mode, sample cell slowly rises when test, until
Liquid level just contacts Rock laminate lower surface, and record microbalance display 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 is Rock laminate width and thickness respectively;γLIt is surface tension of liquid;
R is the internal diameter of sample cell.
2. according to the method described in claim 1, it is characterized by: the Rock laminate is following any: stone in step (1)
English piece, mica sheet, potassium feldspar, albite, dolomite, calcite, illite and chlorite;
The cross section of the Rock laminate is regular oblong, and width and thickness is respectively l, t, wherein 10mm < l < 30mm, t <
5mm。
3. method according to claim 1 or 2, it is characterised in that: in step (2), the testing liquid is following any
Kind: secondary distilled 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 calculated by microbalance reading (m) multiplied by acceleration of gravity (g).
4. method according to claim 1 or 2, it is characterised in that: in sample cell uphill process liquid level always with suspension
Good Rock laminate lower surface is parallel, and experiment table top keeps without friction.
5. method according to claim 1 or 2, it is characterised in that: the method Range of measuring temp are as follows: -10~130
℃。
6. method according to claim 1 or 2, it is characterised in that: active force (F) test scope in the method: 0.1 μ N
~2.1N, measuring accuracy are ± 1 μ N.
7. a kind of test method of wettability of rock surface dynamic change, comprising: according to of any of claims 1-6
The test method of rock surface static contact angle, first fixes Rock laminate, in different times point, 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 and contacting
Between relation curve.
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