CN105628560B - One kind measurement CO2The experimental provision of/salt solution/rock system contact angle - Google Patents

One kind measurement CO2The experimental provision of/salt solution/rock system contact angle Download PDF

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Publication number
CN105628560B
CN105628560B CN201510992562.3A CN201510992562A CN105628560B CN 105628560 B CN105628560 B CN 105628560B CN 201510992562 A CN201510992562 A CN 201510992562A CN 105628560 B CN105628560 B CN 105628560B
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high pressure
pressure kettle
high temperature
temperature
needle
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CN105628560A (en
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陈聪
叶自强
董波
张宁
李维仲
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Dalian University of Technology
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Dalian University of Technology
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N13/00Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects

Abstract

The invention provides one kind to measure CO2The experimental provision of/salt solution/rock system contact angle, belongs to greenhouse gases geological storage technical field.The experimental provision includes high temperature and high pressure kettle, heating tape, high-speed camera instrument, image analyzer, temperature control console, CO2Syringe, solution bottle, vavuum pump, pressure gauge, Temperature sampler and rock etc..The achievable Temperature sampler of the present invention has level regulation, the accurate temperature for measuring contact interface;Measure the contact angle of rock surface diverse location;Step-less adjustment CO2Bubble disengaging configuration and rock surface vertical range in salt solution, influence and measurement dynamic contact angle of the research bubble disengaging configuration to contact angle;The factors such as temperature, pressure, roughness of rock surface, salt solution constituent, ionic strength and Rock Species are studied to CO2The affecting laws of bubble and rock surface contact angle, are CO2Geological storage provides reliable experimental basis.

Description

One kind measurement CO2The experimental provision of/salt solution/rock system contact angle
Technical field
The invention belongs to greenhouse gases geological storage technical field, and in particular to one kind measurement CO2/ salt solution/rock system The experimental provision of contact angle.
Background technology
The whole world causes atmospheric greenhouse gas CO to the heavy dependence of fossil fuel2It is continuously increased, on Global Temperature continues Rise, trigger greenhouse effects.In order to alleviate greenhouse effects, various countries are one after another using carbon trapping and Plugging Technology Applied, by the CO of collection2With super In critical condition injection geologic structure, such as oil field, gas field, salt water layer and the colliery that can not be exploited, long-term geological storage is realized Purpose.
Under geological storage environment, CO2The contact angle of/salt solution/rock system is to influence CO2Migrate and advise in medium is sealed up for safekeeping Rule, capillary pressure, capillary seal efficiency, remaining capture ability, geological storage amount size and an important parameter of cap rock leakage up for safekeeping. Therefore, in order to ensure CO2The chronicity of geological storage, safety and stability, contrived experiment device is needed, simulate geological storage ring Border, measure CO2Boundary contact angle in/salt solution/rock system, understand contact angle changing rule.
Research shows:Influence contact angle factor it is a lot, such as temperature, pressure, roughness of rock surface, salt solution composition into Point, ionic strength and Rock Species etc..Existing measurement CO2The experimental provision of/salt solution/rock system contact angle, exist it is following not Foot:Experiment measurement temperature is high temperature and high pressure kettle wall temperature, can not measure the temperature of contact interface, due to internal brine temp field not Equal property, larger error be present with wall temperature to characterize the temperature of contact interface;Experimental provision can only measure connecing at rock center Feeler, the contact angle of rock surface diverse location can not be measured;In experimentation, CO can not be adjusted2Gas is pickled de- Off normal put with rock surface vertical range, influence of the bubble disengaging configuration to contact angle can not be studied, dynamic Contact can not be measured Angle.
The content of the invention
The purpose of the present invention is in order to solve above-mentioned the deficiencies in the prior art, there is provided one kind measurement CO2/ salt solution/rock The experimental provision of stone system contact angle.That realizes Temperature sampler has level regulation, the accurate temperature for measuring contact interface;Measure rock The contact angle of stone surface diverse location;Step-less adjustment CO2Bubble disengaging configuration and rock surface vertical range, research in salt solution Influence and measurement dynamic contact angle of the bubble disengaging configuration to contact angle.
The present invention is achieved through the following technical solutions:
One kind measurement CO2The experimental provision of/salt solution/rock system contact angle, including light source, end socket, high temperature and high pressure kettle, ring Shape Teflon sealing ring, sapphire visor, annular red copper pad, heating tape, high-speed camera instrument, image analyzer, temperature control Platform, CO2Gas cylinder, CO2Pump, flow control valve, CO2Syringe, conic connector, drainage valve, solution bottle, vavuum pump, dual-handle threeway Needle-valve, pressure gauge, micro slide, slot, Temperature sampler and rock.
It is horizontal cylindrical cavity inside described high temperature and high pressure kettle, welds slot inside cavity vertical direction 2/3, insert Groove location is horizontal, is distributed with stepped hole at left and right sides of cavity, is female thread structure at the port of high temperature and high pressure kettle both sides;High temperature is high Press and four screwed holes are distributed on the symmetrical section of kettle, respectively positioned at the top of high temperature and high pressure kettle, bottom, front lower place and rear.
Described Temperature sampler includes plug, clamp nut, thermocouple and cutting ferrule;Cutting ferrule is used to fix thermocouple, Gu It is unadjustable to determine position;Cutting ferrule is pressed in plug by clamp nut, and plug and the screwed hole at high temperature and high pressure kettle rear are connected; Thermocouple is stretched into high temperature and high pressure kettle cavity through plug, its front end;Plug length is 3 series, and length difference is followed successively by 3mm, by changing different length plug, there is level movement position of the thermocouple front end in high temperature and high pressure kettle cavity, realizes Temperature sampler has level regulation, the accurate temperature for measuring contact interface.
Described CO2Syringe includes syringe needle, annular Teflon sealing ring, barrel, boss, screw rod handle and needle tubing.Syringe needle Installed in needle tubing front end, boss is welded in the middle part of needle tubing, and needle tubing front end passes through barrel, and boss is inserted in barrel;Screw rod from Needle tubing end is inserted in, and the external screw thread of screw rod handle connects with the screw-internal thread fit of barrel, and the front end of screw rod handle is headed in the middle part of needle tubing Boss, rotary screw handle, boss move up and down, and drive syringe needle to move up and down, realize step-less adjustment CO2Bubble departs from salt solution Position and rock surface vertical range;Syringe needle is stretched into high temperature and high pressure kettle cavity, external screw thread and the high temperature and high pressure kettle bottom of barrel Screwed hole is connected, and annular Teflon sealing ring is pressed in the screwed hole of high temperature and high pressure kettle bottom, realizes sealing;Syringe needle For straight type syringe needle or the curved syringe needle of eccentric throw, eccentric throw is 3mm or 6mm.
Rock is pasted onto micro slide lower surface, and micro slide is stuck in the slot of high temperature and high pressure kettle, for fixing rock;Annular Teflon sealing ring is located at the side of sapphire visor, and the end socket with through hole is nibbled with internal thread at the port of high temperature and high pressure kettle both sides Connection is closed, and the sapphire visor that annular red copper pad and side are cased with to annular Teflon sealing ring successively is pressed in HTHP In the stepped hole of kettle, annular red copper pad realizes high temperature and high pressure kettle both sides port between end surface of step hole and sapphire visor Sealing;The lower port of dual-handle threeway needle-valve is connected by conic connector with high temperature and high pressure kettle screw top hole, dual-handle threeway The upper left port of needle-valve is connected with vavuum pump, and the upper right output port of dual-handle threeway needle-valve is sequentially connected pressure gauge and flow control valve Afterwards, with CO2The outlet connection of pump;CO2The needle tubing of syringe passes through flow control valve and CO2The outlet connection of pump;CO2Pump enters Mouth is sequentially connected flow control valve and CO2Gas cylinder;Solution bottle is connected with flow control valve, and separates two branch roads, a branch road It is connected by conic connector with high temperature and high pressure kettle front lower place screwed hole, with fluid injection;Another branch road connects drainage valve, with drainage; Thermocouple tip of the temperature control console respectively with heating tape and Temperature sampler is connected, and heating tape is wrapped in outside high temperature and high pressure kettle Wall, with heating;Light source and high-speed camera instrument are placed at left and right sides of high temperature and high pressure kettle at end socket, and light source, high-speed camera and high temperature are high The central axis of pressure kettle is located in same horizontal line, and high-speed camera instrument is connected with image analyzer, and to handle image, measurement connects Feeler.
The present invention function and beneficial effect be:
(1) plug of different length series is changed, there is level movement thermocouple front end position in high temperature and high pressure kettle, real Existing Temperature sampler has level regulation, the accurate temperature for measuring contact interface.
(2) syringe needle type is changed, measures the contact angle of rock surface diverse location.Using straight type syringe needle, measure in rock Contact angle at the heart;Using the curved syringe needle of eccentric throw, rotate needle tubing, drive the curved syringe needle of eccentric throw to do circumference operation, measure with Centered on rock core, radius is the contact angle on the circumference of eccentric throw.
(3) rotary screw handle, step-less adjustment CO2The pickled disengaging configuration of gas and rock surface vertical range, grind Study carefully influence of the bubble disengaging configuration to contact angle, and measurement dynamic contact angle.
(4) using the present invention, temperature, pressure, roughness of rock surface, salt solution constituent, ionic strength can be studied With the factor such as Rock Species to CO2The affecting laws of bubble and rock surface contact angle, are CO2Geological storage provides reliable real Test foundation.
Brief description of the drawings
Fig. 1 is a kind of measurement CO of the invention2The experimental provision structural representation of/salt solution/rock system contact angle.
Fig. 2 is the Temperature sampler structural representation of the present invention.
Fig. 3 is the CO of the present invention2Syringe construction schematic diagram.
Fig. 4 is the straight type needle head structure schematic diagram of the present invention.
Fig. 5 is the curved needle head structure schematic diagram of eccentric throw of the present invention.
In figure:1 light source;2 end sockets;3 high temperature and high pressure kettles;4 annular Teflon sealing rings;5 sapphire visors;6 annular red coppers Pad;7 heating tapes;8 high-speed camera instrument;9 image analyzers;10 temperature control consoles;11CO2Gas cylinder;12CO2Pump;13 flows control Valve;14CO2Syringe;15 conic connectors;16 drainage valves;17 solution bottles;18 vavuum pumps;19 dual-handle threeway needle-valves;20 pressure Table;21 micro slides;22 slots;23 Temperature samplers;24 rocks;25 plugs;26 clamp nuts;27 thermocouples;28 cutting ferrules;29 Syringe needle;30 barrels;31 boss;32 screw rod handles;33 needle tubings;34 straight type syringe needles;The curved syringe needle of 35 eccentric throws.
Embodiment
Explanation is described in further detail to the present invention with technical scheme below in conjunction with the accompanying drawings.
A kind of measurement CO of the invention2The experimental provision of/salt solution/rock system contact angle, as shown in figure 1, by light source 1, envelope First 2, high temperature and high pressure kettle 3, annular Teflon sealing ring 4, sapphire visor 5, annular red copper pad 6, heating tape 7, high-speed camera Instrument 8, image analyzer 9, temperature control console 10, CO2Gas cylinder 11, CO2Pump 12, flow control valve 13, CO2Syringe 14, the conical surface Joint 15, drainage valve 16, solution bottle 17, vavuum pump 18, dual-handle threeway needle-valve 19, pressure gauge 20, micro slide 21, slot 22, Temperature sampler 23 and rock 24 form.
Described Temperature sampler, as shown in Fig. 2 being made up of plug 25, clamp nut 26, thermocouple 27 and cutting ferrule 28.
Described CO2Syringe, as shown in figure 3, by syringe needle 29, annular Teflon sealing ring 4, barrel 30, boss 31, Screw rod forms 32 and needle tubing 33.
Specific experiment device installation steps:
(1) Temperature sampler 23 is installed.According to shown in Fig. 2, cutting ferrule 28 fixes thermocouple 27, and clamp nut 26 is by cutting ferrule 28 It is pressed in plug 25, plug 25 is connected with the rear screwed hole of high temperature and high pressure kettle 3, and high temperature and high pressure kettle is stretched into the front end of thermocouple 27 In 3 cavitys.
(2) CO is installed2Syringe 14.According to shown in Fig. 3, syringe needle 29 is arranged on the front end of needle tubing 33, and the front end of needle tubing 33 passes through Barrel 30, and boss 31 is inserted in barrel 30;Screw rod is inserted in 32 from the end of needle tubing 33, using in external screw thread and barrel 30 Screw thread is connected, and front end heads on boss 31;Barrel 30 is connected using external screw thread with the bottom thread hole of high temperature and high pressure kettle 3, and will Annular Teflon sealing ring 4 is pressed in the bottom thread hole of high temperature and high pressure kettle 3, and syringe needle 29 is stretched into the cavity of high temperature and high pressure kettle 3.
(3) according to shown in Fig. 1, connecting components.Rock 24 is pasted onto the lower surface of micro slide 21, and the edge card of micro slide 21 exists In slot 22;Annular Teflon sealing ring 4 is enclosed on the side of sapphire visor 5, end socket 2 with the both sides port of high temperature and high pressure kettle 3 Internal thread engagement connection, and the sapphire that annular red copper pad 6 and side are cased with to annular Teflon sealing ring 4 successively regards Mirror 5 is pressed in the stepped hole of high temperature and high pressure kettle 3, and annular red copper pad 6 is between end surface of step hole and sapphire visor 5;It is double The lower port of handle threeway needle-valve 19 is connected by conic connector 15 with the screw top hole of high temperature and high pressure kettle 3, upper left port with it is true Empty pump 18 connects, after upper right output port is sequentially connected pressure gauge 20 and flow control valve 13, with CO2The outlet connection of pump 12;CO2Note The needle tubing 33 of emitter 14 passes through flow control valve 13 and CO2The outlet connection of pump 12;CO2The entrance of pump 12 is sequentially connected flow control Valve 13 and CO processed2Gas cylinder 11;Solution bottle 17 is connected with flow control valve 13, and separates two branch roads, and a branch road passes through the conical surface Joint 15 is connected with the front lower place screwed hole of high temperature and high pressure kettle 3;Another branch road connects drainage valve 16;Temperature control console 10 respectively with Heating tape 7 is connected with the end of thermocouple 27 of Temperature sampler 23, and heating tape 7 is wrapped in the outer wall of high temperature and high pressure kettle 3;The He of light source 1 High-speed camera instrument 8 is placed at the left and right sides end socket 2 of high temperature and high pressure kettle 3, and central axis is located in same horizontal line, high-speed camera instrument 8 are connected with image analyzer 9.
Specific Contact-angle measurement step:
(1) all valves, verifying attachment sealing are closed.
(2) left port on dual-handle threeway needle-valve 19 is opened, using vavuum pump 18, extracts air in high temperature and high pressure kettle 3 out, Left port in closing.
(3) flow control valve 13 being connected with solution bottle 17 is opened, injects salt solution into the cavity of high temperature and high pressure kettle 3, until Rock 24 is submerged, is turned off.
(4) heating tape 7 is opened, high temperature and high pressure kettle 3 is heated, reaches set temperature value, insulation is set.
(5) open right output port on dual-handle threeway needle-valve 19, the flow control valve 13 being connected with pressure gauge 20 and with CO2The flow control valve 13 that gas cylinder 11 connects, CO is filled with into high temperature and high pressure kettle 32, pressure reaches setting value, keeps small half When, close the flow control valve 13 being connected with pressure gauge 20.
(6) flow control valve 13 being connected with needle tubing 33 is finely tuned, CO is injected into salt solution2Bubble, CO2Bubble departs from syringe needle 29, rise in salt solution, be attached to the lower surface of rock 24, by the shooting image of high-speed camera instrument 8, input picture analyzer 9, measurement Contact angle.
(7) 32, front end heads on boss 31 and moved up and down in barrel 30 rotary screw, drives syringe needle 29 in salt solution Move up and down, repeat experimental procedure (6), measure CO2Contact angle of the bubble in salt solution during different disengaging configurations.
(8) when syringe needle 29 rises to certain position, CO2Bubble also without departing from syringe needle 29, is just attached to the following table of rock 24 Face, the flow control valve 13 being connected with needle tubing 33 is finely tuned, continue to inject CO2, air bubble growth procedure chart is shot by high-speed camera instrument 8 Picture, input picture analyzer 9, measure dynamic contact angle.
(9) all valves and heating tape 7 are closed, after the cooling of high temperature and high pressure kettle 3, vavuum pump 18 is dismantled, from dual-handle three Left port pressure release on cleansing pin valve 19, from the drainage of drainage valve 16, and clean high temperature and high pressure kettle.
(10) CO is dismantled2Syringe 14, change the different curved syringe needles 35 of eccentric throw;Dismantle Temperature sampler 23, replacing pair Answer the plug 25 of length series;Reinstall CO2Syringe 14, Temperature sampler 23, vavuum pump 18.Repeat experimental procedure (1) ~(8), in experimentation, needle tubing 33 is rotated, drives the curved syringe needle 35 of eccentric throw to be moved in a circle in salt solution.Accurate measurement The temperature of contact interface and contact angle, the dynamic contact angle of rock diverse location.
(11) after the completion of testing, cooling, pressure release, drainage, dismounting laboratory apparatus, cleaning experiment device.

Claims (2)

1. one kind measurement CO2The experimental provision of/salt solution/rock system contact angle, it is characterised in that the experimental provision include light source, End socket, high temperature and high pressure kettle, annular Teflon sealing ring, sapphire visor, annular red copper pad, heating tape, high-speed camera instrument, figure As analyzer, temperature control console, CO2Gas cylinder, CO2Pump, flow control valve, CO2Syringe, conic connector, drainage valve, solution bottle, Vavuum pump, dual-handle threeway needle-valve, pressure gauge, micro slide, slot, Temperature sampler and rock;
It is horizontal cylindrical cavity inside described high temperature and high pressure kettle, slot, slot position is welded inside cavity vertical direction 2/3 Level is put, stepped hole is distributed with left and right sides of cavity, is female thread structure at the port of high temperature and high pressure kettle both sides;High temperature and high pressure kettle Four screwed holes are distributed on symmetrical section, respectively positioned at the top of high temperature and high pressure kettle, bottom, front lower place and rear;
Described Temperature sampler includes plug, clamp nut, thermocouple and cutting ferrule;Cutting ferrule is used to fix thermocouple, fixed part Position is unadjustable;Cutting ferrule is pressed in plug by clamp nut, and plug and the screwed hole at high temperature and high pressure kettle rear are connected;Thermoelectricity It is even to be stretched into through plug, its front end in high temperature and high pressure kettle cavity;Plug length is 3 series, and length difference is followed successively by 3mm, is led to Replacing different length plug is crossed, there is level movement position of the thermocouple front end in high temperature and high pressure kettle cavity, realizes that temperature is adopted Storage has level regulation, the accurate temperature for measuring contact interface;
Described CO2Syringe includes syringe needle, annular Teflon sealing ring, barrel, boss, screw rod handle and needle tubing;Syringe needle is arranged on Needle tubing front end, boss are welded in the middle part of needle tubing, and needle tubing front end passes through barrel, and boss is inserted in barrel;Screw rod is last from needle tubing End is inserted in, and the external screw thread of screw rod handle connects with the screw-internal thread fit of barrel, and the front end of screw rod handle heads on the boss in the middle part of needle tubing, rotation Turn screw rod handle, boss moves up and down, and drives syringe needle to move up and down, realizes step-less adjustment CO2Bubble in salt solution disengaging configuration with Rock surface vertical range;Syringe needle is stretched into high temperature and high pressure kettle cavity, external screw thread and the high temperature and high pressure kettle bottom thread hole of barrel It is connected, and annular Teflon sealing ring is pressed in the screwed hole of high temperature and high pressure kettle bottom, realizes sealing;Syringe needle is straight type Syringe needle or the curved syringe needle of eccentric throw, eccentric throw are 3mm or 6mm;
Rock is pasted onto micro slide lower surface, and micro slide is stuck in the slot of high temperature and high pressure kettle, for fixing rock;Annular Teflon Imperial sealing ring is located at the side of sapphire visor, and the end socket with through hole engages company with internal thread at the port of high temperature and high pressure kettle both sides Connect, and the sapphire visor that annular red copper pad and side are cased with to annular Teflon sealing ring successively is pressed in high temperature and high pressure kettle In stepped hole, annular red copper pad realizes high temperature and high pressure kettle both sides port sealing between end surface of step hole and sapphire visor; The lower port of dual-handle threeway needle-valve is connected by conic connector with high temperature and high pressure kettle screw top hole, dual-handle threeway needle-valve Upper left port is connected with vavuum pump, after the upper right output port of dual-handle threeway needle-valve is sequentially connected pressure gauge and flow control valve, with CO2The outlet connection of pump;CO2The needle tubing of syringe passes through flow control valve and CO2The outlet connection of pump;CO2The entrance of pump is successively Connection traffic control valve and CO2Gas cylinder;Solution bottle is connected with flow control valve, and separates two branch roads, and a branch road passes through cone Plane tie is connected with high temperature and high pressure kettle front lower place screwed hole, with fluid injection;Another branch road connects drainage valve, with drainage;Temperature control Thermocouple tip of the platform processed respectively with heating tape and Temperature sampler is connected, and heating tape is wrapped in high temperature and high pressure kettle outer wall, to add Heat;Light source and high-speed camera instrument are placed at left and right sides of high temperature and high pressure kettle at end socket, in light source, high-speed camera and high temperature and high pressure kettle Mandrel line is located in same horizontal line, and high-speed camera instrument is connected with image analyzer, to handle image, measures contact angle.
2. the method for Contact-angle measurement is carried out with the experimental provision described in claim 1, it is characterised in that step is as follows:
(1) all valves, verifying attachment sealing are closed;
(2) left port on dual-handle threeway needle-valve is opened, using vavuum pump, extracts air in high temperature and high pressure kettle out, left end in closing Mouthful;
(3) flow control valve being connected with solution bottle is opened, injects salt solution into high temperature and high pressure kettle cavity, until submergence rock, It is turned off;
(4) heating tape is opened, high temperature and high pressure kettle is heated, reaches set temperature value, insulation is set;
(5) right output port on dual-handle threeway needle-valve, the flow control valve and and CO that are connected with pressure gauge are opened2Gas cylinder connection Flow control valve, CO is filled with into high temperature and high pressure kettle2, pressure reaches setting value, kept for half an hour, and closing is connected with pressure gauge Flow control valve;
(6) flow control valve being connected with needle tubing is finely tuned, CO is injected into salt solution2Bubble, CO2Bubble departs from syringe needle, in salt solution Rise, be attached to rock lower surface, by high-speed camera instrument shooting image, input picture analyzer, measure contact angle;
(7) rotary screw handle, front end head on boss and moved up and down in barrel, drive syringe needle to be moved up and down in salt solution, repeat Step (6), measure CO2Contact angle of the bubble in salt solution during different disengaging configurations;
(8) when syringe needle rises to CO2Bubble also without departing from syringe needle, is just attached to rock lower surface, finely tunes the flow being connected with needle tubing Control valve, continue to inject CO2, air bubble growth procedural image, input picture analyzer are shot by high-speed camera instrument, measurement dynamic connects Feeler;
(9) all valves and heating tape are closed, after high temperature and high pressure kettle cooling, vavuum pump is dismantled, from dual-handle threeway needle-valve Left port pressure release, from drainage valve drainage, and clean high temperature and high pressure kettle;
(10) CO is dismantled2Syringe, change the different curved syringe needles of eccentric throw;Temperature sampler is dismantled, changes corresponding length series Plug;Reinstall CO2Syringe, Temperature sampler and vavuum pump;Experimental procedure (1)-(8) are repeated, in experimentation, rotation Rotating the needle pipe, the curved syringe needle of eccentric throw is driven to be moved in a circle in salt solution;The temperature and rock of accurate measurement contact interface are not Contact angle, dynamic contact angle with position.
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CN109632580B (en) * 2019-01-21 2020-04-17 浙江大学 Experimental system and method for measuring dynamic contact angle in high-temperature and high-pressure environment
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