CN104132871A - Method for measuring surface contact angle between opaque liquid and solid - Google Patents

Method for measuring surface contact angle between opaque liquid and solid Download PDF

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Publication number
CN104132871A
CN104132871A CN201410395834.7A CN201410395834A CN104132871A CN 104132871 A CN104132871 A CN 104132871A CN 201410395834 A CN201410395834 A CN 201410395834A CN 104132871 A CN104132871 A CN 104132871A
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China
Prior art keywords
contact angle
opaque liquid
solid
surface contact
liquid
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Pending
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CN201410395834.7A
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Chinese (zh)
Inventor
蒋秀
屈定荣
刘小辉
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China Petroleum and Chemical Corp
Sinopec Qingdao Safety Engineering Institute
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China Petroleum and Chemical Corp
Sinopec Qingdao Safety Engineering Institute
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Priority to CN201410395834.7A priority Critical patent/CN104132871A/en
Publication of CN104132871A publication Critical patent/CN104132871A/en
Pending legal-status Critical Current

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Abstract

The invention relates to a method for measuring a surface contact angle between an opaque liquid and a solid, and mainly aims at solving the problem that the surface contact angle between the opaque liquid and the solid can not be measured in the prior art. The method for measuring the surface contact angle between the opaque liquid and the solid mainly comprises the following steps: (1), fixing a solid sample on a solid sample testing bracket in a testing container; (2), injecting a transparent medium in the testing container, wherein the height of the liquid level of the transparent medium is greater than that of the lower surface of the solid sample, and the density of the transparent medium is greater than that of the opaque liquid; (3), adjusting a video optical contact angle measuring instrument, the focal length of a light source and a shooting angle to ensure that a shot image is clear; (4), injecting liquid drops of the to-be-tested opaque liquid in the lower surface of the solid sample; and (5), shooting an opaque liquid drop image and calculating the contact angle. According to the technical scheme, the problem is well solved; and the method can be used in measurement of the surface contact angle between the opaque liquid and the solid.

Description

The measuring method of opaque liquid and solid surface contact angle
Technical field
The measuring method that the present invention relates to a kind of opaque liquid and solid surface contact angle, is particularly useful for the measurement of crude oil and solid surface contact angle.
Background technology
The contact angle of liquid on solid material surface, is to weigh the important parameter of this liquid to material surface wettability, can obtain the relevant information of solid-liquid, solid-atmosphere interaction to the measurement of contact angle.Contact Angle Measurement Technique has important application in fields such as petroleum industry, medical material, chip industry, the nontoxic anti-fouling material of low-surface-energy, cosmetics, agricultural chemicals, printing and dyeing, papermaking, sprayings.
When liquid partly soaks solid surface, liquid forms drop at solid surface, and solid is larger to the contact angle of liquid, shows that the wetting state of this liquid effects on surface is poorer.
In Crude Oil Transportation process, former W/O is in the bottom of pipeline deposition, and the Korrosionsmedium in water and water may cause corrosion to pipeline, and crude oil self does not have corrosivity.Because crude oil and water are the flowing of pipe interior, under certain fluidised form, crude oil may intermittent contact duct bottom surface, contributes to suppress corrosive pipeline.But crude oil is relevant in factors such as the wetting state of pipe surface and former oil properties and pipe surface states, therefore, measures crude oil wetting state to solid surface in water environment, and contact angle, very necessary, but crude oil is generally opaque, and this has increased the difficulty of measuring.
At present the measurement of effects on surface contact angle is more be for transparency liquid in transparent gas or transparency liquid environment, as water at air or water the Surface Contact angular measurement at clean oil.CN201110342914.2 discloses a kind of detecting method of hydrophobic static contact angle, first gathers globule image, then globule image is analyzed, and to the globule under different condition, selects the algorithm of appointment to analyze, and finally tries to achieve contact angle.CN201110343828.3 provides a kind of detection method of static contact angle of hydrophilic water bead, comprising: obtain globule image; Select circle fitting algorithm or ellipse fitting algorithm to calculate the estimated value of globule static contact angle; According to globule volume and the estimated value that calculates globule static contact angle, select circle fitting algorithm or ellipse fitting algorithm to calculate the exact value of globule static contact angle.
Because light can not see through opaque liquid, therefore, said method is not suitable for opaque liquid to be measured at the contact angle of solid surface, especially when opaque transparent liquid phase density is lower than the density of another transparent liquid phase, and cannot measurement for opaque liquid phase and the contact angle of solid phase.
The present invention has solved this problem targetedly.
Summary of the invention
Technical matters to be solved by this invention is cannot measurement for opaque liquid in prior art and the problem of solid surface contact angle, and the measuring method of a kind of new opaque liquid and solid surface contact angle is provided.The method is for the measurement of crude oil and solid surface contact angle, and having advantages of can measurement for opaque liquid and solid surface contact angle.
For addressing the above problem, the technical solution used in the present invention is as follows: the measuring method of a kind of opaque liquid and solid surface contact angle, mainly comprises the following steps: (1) is fixed on solid sample on the solid sample test bracket in test container; (2) in test container, inject transparent medium, the liquid level of transparent medium is greater than the lower surface height of solid sample, and density is greater than the density of opaque liquid; (3) adjust video optics contact angle measurement, light source focal length, shooting angle, make photographic images clear; (4) opaque liquid drop to be tested is injected into the lower surface of solid sample; (5) take opaque liquid drop image and calculate contact angle.
In technique scheme, preferably, by entry needle, opaque liquid drop is injected into the lower surface of solid sample.
In technique scheme, preferably, described test container is made by transparent materials such as being selected from polycarbonate, optical glass, colourless transparent resin glass.
In technique scheme, preferably, described test container top cross-section is circular, and adopts O-ring seal sealing.
In technique scheme, preferably, the top seal of described test container covers and is provided with draft tube, escape pipe and pH meter, by draft tube and escape pipe, in transparent medium, passes into the object that gas reaches deoxygenation or passes into experimental gas, and the test lead of pH meter inserts below the liquid level of transparent medium.
In technique scheme, preferably, on described test container sidewall, have the aperture that entry needle enters on solid sample test bracket.If entry needle is elbow pin, from the pH meter mouth at test container top, insert entry needle, opaque transparent liquid is dripped to the lower surface that is filled into solid sample.
In technique scheme, preferably, perforate respectively on the chamber wall being irradiated by light source on test container and relative wall, and camera plane is installed, avoid scattering of light to affect test result, light by camera plane in the imaging of crude oil drop surface and by camera.
In technique scheme, preferably, opaque liquid is crude oil, and transparent medium is water.
When the contact angle that adopts method of the present invention to carry out opaque liquid (as crude oil) and solid surface is measured, owing to having injected water in test container, the density of the density ratio crude oil of water is large, so crude oil will form oil droplet on the lower surface of solid sample, adopt the camera in the video optics contact angle measurement of German Dataphysics instrument company to carry out clear shooting, by image, carry out the calculating of contact angle.
Adopt method of the present invention, by described proving installation, can realize opaque liquid and measure at the contact angle of solid surface, as the measurement of the contact angle of the solid surface of crude oil in water environment, simple and direct-viewing operation, measurement result is accurate, has obtained good technique effect.
Accompanying drawing explanation
Fig. 1 is the structural representation of the proving installation of the method for the invention employing;
In Fig. 1,1 is container; 2 is oil droplet; 3 is solid sample support; 4 is solid sample; 5 is the aperture on solid sample support 3; 6 is aperture and the sealing-plug on container 1; 7 is transparent shooting mouthful; 8 is O-ring seal; 9 is gland bonnet; 10 is draft tube; 11 is escape pipe; 12 is pH meter.
Fig. 2 is the contact angle schematic diagram of opaque liquid and solid surface;
In Fig. 2,13 lower surfaces that are solid sample; 14 is opaque liquid drop; θ is contact angle.
Below by embodiment, the invention will be further elaborated, but be not limited only to the present embodiment.
Embodiment
[embodiment 1]
On device as shown in Figure 1, adopt method of the present invention to carry out the measurement of crude oil and solid sample contact angle, test container is transparent, for columniform, material is optical glass, adopts O-ring seal sealing, and test container top and gland bonnet seal by O-ring seal and screw.Top seal covers and is provided with draft tube, escape pipe and pH meter, by draft tube and escape pipe, in transparent medium, passes into the object that gas reaches deoxygenation or passes into experimental gas, and the test lead of pH meter inserts below the water surface.
Video optics contact angle measurement adopts German Dataphysics instrument company, towards the vessel surface of charge-coupled image sensor (CCD) camera lens and the parallel side of container of video optics contact angle instrument device, is partly plane, and no marking.
Respectively perforate on the chamber wall being irradiated by light source on test container and relative wall, and camera plane is installed, avoids scattering of light affect test result, light by camera plane in the surperficial imaging of crude oil drop and by camera.
On the sample stage of video optics contact angle instrument device, place test container, pack water in container into, the height of water is higher than the lower surface of solid sample, by solid sample support fixed solid sample.By draft tube, to passing into gas in container, carried out deoxygenation and be filled with experimental gas, escape pipe is got rid of oxygen or other gas, measures the pH value of solution by pH meter.Solid sample support need guarantee can be positioned at the reflected image of oil droplet upper surface CCD camera and the observation the video optics contact angle instrument device of test container opposite side from CCD camera lens light out.Regulate light source focal length to make the clear picture of entry needle, by the aperture on the aperture on test container sidewall and solid sample support, the crude oil in syringe is expelled to the lower surface of solid sample; If entry needle is elbow pin, can insert entry needle from the pH meter mouth at test container top, opaque transparent liquid is dripped to the lower surface that is filled into solid sample.Due to the density of the crude oil density lower than water, crude oil will form oil droplet on the lower surface of solid sample, takes oil droplet image and also according to shown in Fig. 2, calculates contact angle.
[embodiment 2]
According to method and the step shown in embodiment 1, just test container is square column, and water-tight equipment is not established at top, does not set out tracheae, draft tube and pH meter yet, and the material of test container is colourless transparent resin glass.

Claims (8)

1. a measuring method for opaque liquid and solid surface contact angle, mainly comprises the following steps:
(1) solid sample is fixed on the solid sample test bracket in test container;
(2) in test container, inject transparent medium, the liquid level of transparent medium is greater than the lower surface height of solid sample, and density is greater than the density of opaque liquid;
(3) adjust video optics contact angle measurement, light source focal length, shooting angle, make photographic images clear;
(4) opaque liquid drop to be tested is injected into the lower surface of solid sample;
(5) take opaque liquid drop image and calculate contact angle.
2. the measuring method of opaque liquid and solid surface contact angle according to claim 1, is characterized in that by entry needle, opaque liquid drop being injected into the lower surface of solid sample.
3. the measuring method of opaque liquid and solid surface contact angle according to claim 1, is characterized in that described test container made by transparent materials such as being selected from polycarbonate, optical glass, colourless transparent resin glass.
4. the measuring method of opaque liquid and solid surface contact angle according to claim 1, is characterized in that described test container top cross-section is for circular, and adopts O-ring seal sealing.
5. the measuring method of opaque liquid and solid surface contact angle according to claim 1, the top seal that it is characterized in that described test container covers and is provided with draft tube, escape pipe and pH meter, by draft tube and escape pipe, in transparent medium, pass into the object that gas reaches deoxygenation or passes into experimental gas, the test lead of pH meter inserts below the liquid level of transparent medium.
6. the measuring method of opaque liquid and solid surface contact angle according to claim 1, is characterized in that on described test container sidewall, on solid sample test bracket, has the aperture that entry needle enters.If entry needle is elbow pin, from the pH meter mouth at test container top, insert entry needle, opaque transparent liquid is dripped to the lower surface that is filled into solid sample.
7. the measuring method of opaque liquid and solid surface contact angle according to claim 1, it is characterized in that perforate respectively on the chamber wall that irradiated by light source and relative wall on test container, and camera plane is installed, avoid scattering of light to affect test result, light by camera plane in the imaging of crude oil drop surface and by camera.
8. the measuring method of opaque liquid and solid surface contact angle according to claim 1, is characterized in that opaque liquid is crude oil, and transparent medium is water.
CN201410395834.7A 2014-05-30 2014-08-12 Method for measuring surface contact angle between opaque liquid and solid Pending CN104132871A (en)

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CN201410241130.4 2014-05-30
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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104914018A (en) * 2015-05-06 2015-09-16 上海梭伦信息科技有限公司 3D contact angle testing device and testing method
CN105043936A (en) * 2015-07-08 2015-11-11 中国石油天然气股份有限公司 Device and method for measurement of contact angle and interfacial tension under simulative oil reservoir conditions
CN106442227A (en) * 2016-12-08 2017-02-22 南京航空航天大学 Testing device and method for ice removing performance of solid surface under action of simulated external field
JP2017096685A (en) * 2015-11-19 2017-06-01 国立大学法人 岡山大学 Needle, and injection needle equipped with the same
CN107589218A (en) * 2017-08-22 2018-01-16 北京理工大学 A kind of measuring method of fluid molecule potential parameter and molecule distance parameter
CN111665171A (en) * 2020-07-14 2020-09-15 上海梭伦信息科技有限公司 Wet contact angle measuring device and testing method thereof
CN112557259A (en) * 2020-12-30 2021-03-26 中国石油大学(北京) Rock wettability measuring device and method under stratum water environment
CN113029871A (en) * 2021-03-12 2021-06-25 西安石油大学 Device and method for measuring contact angle in multi-medium environment under high-temperature and high-pressure conditions
CN113203662A (en) * 2021-05-11 2021-08-03 厦门理工学院 Contact angle measuring device

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CN101892040A (en) * 2010-07-12 2010-11-24 孙安顺 Wetting agent and application thereof in binary compound flooding tertiary oil recovery
CN102914490A (en) * 2012-10-10 2013-02-06 中国科学院苏州纳米技术与纳米仿生研究所 Solid-liquid contact angle measuring method in non-transparent or sealed space

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CN102914490A (en) * 2012-10-10 2013-02-06 中国科学院苏州纳米技术与纳米仿生研究所 Solid-liquid contact angle measuring method in non-transparent or sealed space

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104914018A (en) * 2015-05-06 2015-09-16 上海梭伦信息科技有限公司 3D contact angle testing device and testing method
CN105043936A (en) * 2015-07-08 2015-11-11 中国石油天然气股份有限公司 Device and method for measurement of contact angle and interfacial tension under simulative oil reservoir conditions
CN105043936B (en) * 2015-07-08 2017-12-01 中国石油天然气股份有限公司 It is a kind of to simulate oil reservoir conditioned measurement contact angle and the device and method of interfacial tension
JP2017096685A (en) * 2015-11-19 2017-06-01 国立大学法人 岡山大学 Needle, and injection needle equipped with the same
CN106442227A (en) * 2016-12-08 2017-02-22 南京航空航天大学 Testing device and method for ice removing performance of solid surface under action of simulated external field
CN107589218A (en) * 2017-08-22 2018-01-16 北京理工大学 A kind of measuring method of fluid molecule potential parameter and molecule distance parameter
CN111665171A (en) * 2020-07-14 2020-09-15 上海梭伦信息科技有限公司 Wet contact angle measuring device and testing method thereof
CN111665171B (en) * 2020-07-14 2023-03-03 上海梭伦信息科技有限公司 Wet contact angle measuring device and testing method thereof
CN112557259A (en) * 2020-12-30 2021-03-26 中国石油大学(北京) Rock wettability measuring device and method under stratum water environment
CN113029871A (en) * 2021-03-12 2021-06-25 西安石油大学 Device and method for measuring contact angle in multi-medium environment under high-temperature and high-pressure conditions
CN113203662A (en) * 2021-05-11 2021-08-03 厦门理工学院 Contact angle measuring device

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Application publication date: 20141105