CN107024428A - A kind of experimental provision and its method of work for visualizing hydrate wall adhesion mechanics characteristic - Google Patents
A kind of experimental provision and its method of work for visualizing hydrate wall adhesion mechanics characteristic Download PDFInfo
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- CN107024428A CN107024428A CN201710272175.1A CN201710272175A CN107024428A CN 107024428 A CN107024428 A CN 107024428A CN 201710272175 A CN201710272175 A CN 201710272175A CN 107024428 A CN107024428 A CN 107024428A
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- hydrate
- wall
- normal pressure
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- suprasil
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N19/00—Investigating materials by mechanical methods
- G01N19/04—Measuring adhesive force between materials, e.g. of sealing tape, of coating
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/42—Low-temperature sample treatment, e.g. cryofixation
Abstract
The present invention relates to a kind of experimental provision and its method of work for visualizing hydrate wall adhesion mechanics characteristic, including cycle refrigeration system, test cell system, microtechnique system, microscopic observation system；Test cell system includes normal pressure visualization reaction unit, synthesis under normal pressure groove, liquid inlet, liquid outlet, test cell part, the side wall for visualizing reaction unit is provided with synthesis under normal pressure groove, connection is provided with liquid inlet, liquid outlet on the wall of side, visual windows are additionally provided with the wall of side, test cell part is provided with synthesis under normal pressure groove, test cell part includes solid metal block, suprasil frame, and solid metal block is provided with several suprasil frames.The present invention can be relatively good research and monitoring pentamethylene hydrate in the generation, growth and deposition conditions of wall, eliminate the condition limitation that hydrate must generate under hyperbaric environment, more accurate and visual measurement wall generates the adhesion of pentamethylene hydrate.
Description
Technical field
The present invention relates to a kind of experimental provision and its method of work for visualizing hydrate wall adhesion mechanics characteristic, belong to
Oil-gas mining technical field, more particularly to deep-sea oil gas exploitation field, are particularly suitable for use in hydrate wall in oil-gas pipeline and adhere to
Experiments of Machanics are studied.
Background technology
Hydrate is the cage structure that the molecular structure water connected by hydrogen bond is formed, and gas molecule is then in van der Waals interaction
Under be enclosed in lattice.The molecular structure hole of moisture is filled by some small molecules, and these small molecules play stable lattice
Effect.Small molecule includes the small hydrocarbon of relative molecular mass, such as methane, ethane, propane, and hydrogen and dioxy
Change carbon.During deep water gas field development, gathering line uses mixed transportation process mostly, be typically in pipeline high pressure low temperature environment and
There is the presence of Free water, therefore easily generate hydrate.The generation of hydrate in the duct, the pipeline that can result in blockage, reduction are natural
The harm such as the throughput rate of gas, the pressure difference for increasing pipeline, damage pipe fitting.And the repair after line clogging needs input substantial amounts of
Personnel and fund.Therefore it is to be badly in need of asking for solution at present to prevent Hydrate Plugging pipeline and the efficient de-plugging after generation is blocked
Topic.The basis for solving this problem is that deposition process and its related mechanical property expansion in-depth study are generated to hydrate.
Experimental provision research at present to hydrate mechanical property is considerably less, and research is to carry out in a kettle. mostly.
Chinese patent literature CN104406864A discloses a kind of gas hydrates mechanical property measurement apparatus, including data
Acquisition system, pumped vacuum systems, natural gas boosting gas handling system and hydrate reaction kettle, the hydrate reaction kettle include instead
Bottom seat, end cap, boosting-rod, reactor shell and reaction frame are answered, reactor shell and reactor base are bolted simultaneously
Sealed by sealing ring, end cap is connected by helical form stainless steel tubing with reactor base, boosting-rod is from reactor shell top
Portion penetrates and sealed with sealing ring, and end cap is withstood in boosting-rod one end, and the other end withstands and is provided with first import and export on reaction frame, end cap
And second import and export, reactor base be provided with the 3rd import and export and the 4th import and export, its boss having from reactor base
Center is through aforementioned four is imported and exported and is connected with pumped vacuum systems and natural gas boosting gas handling system.This measurement apparatus is by surveying
The parameters such as principal stress, confined pressure, temperature, deformation, top pressure, the base pressure of hydrate reaction Fu Zhong balancing gate pits are measured, water is obtained
The mechanical property of compound.
Chinese patent literature CN201749054U discloses a kind of experimental provision, more particularly to a kind of gas hydrates power
Learn experimental apparatus for capability.Gas hydrate mechanical property experiment test device of the present utility model, including triaxial apparatus, triaxial apparatus
It is arranged in thermostat, reative cell is provided with triaxial apparatus, top, the bottom of reative cell connect liquid injection system respectively；Reative cell
Bottom be connected with confined pressure system.The experiment synthesized by present apparatus system to gas hydrates and measure, can be contained
The mechanics parameter of natural gas hydrate deposits thing, probing and exploitation for gas hydrates provide very important basis ginseng
Number.The present apparatus obtains the mechanics spy such as stress and strain that hydrate is deposited by measuring the confined pressure of reative cell and deformation in triaxial apparatus
Property.
But above equipment is carried out all under the conditions of cryogenic high pressure, operation has certain danger, and visualization journey
Degree is low, it is impossible to the direct measurement of the data such as generation situation and adhesion of real-time monitored hydrate.
Hydrate tube wall deposition is to cause the key factor of line clogging and valve member failure, and hydrate is looked unfamiliar in duct wall
Length is one of basic model of hydrate tube wall deposition, however, the research for the pattern is also only at macro qualitative analysis at present
Awareness stage, related experiment test still explores rank with theoretical research in initial.
The content of the invention
In view of the shortcomings of the prior art, the invention provides a kind of experiment for visualizing hydrate wall adhesion mechanics characteristic
Device；
Present invention also offers a kind of method of work of said apparatus；
The present invention is using pentamethylene hydrate as model hydrate, and pentamethylene hydrate can be generated in atmospheric conditions, from
And the limitation of condition of high voltage is eliminated, and pentamethylene hydrate is II type structure hydrates, with being hydrated species generated in pipeline
Type is identical, therefore pentamethylene hydrate is the optimal selection of research hydrate adhesion mechanics characteristic in atmospheric pressure environment.
The present invention is simple in construction, and condition of normal pressure is operable, and visualization is high.
Sedimentation mechanism is grown present invention is disclosed hydrate tube wall, there is the risk management to hydrate important guidance to anticipate
Justice.
The technical scheme is that：
A kind of experimental provision for visualizing hydrate wall adhesion mechanics characteristic, including cycle refrigeration system, test cell
System, microtechnique system, microscopic observation system；
The cycle refrigeration system connects the test cell system, for providing constant for the test cell system
Temperature；
The microtechnique system connects the test cell system, raw in the test cell system for measuring in real time
Into hydrate adhesion；
The microscopic observation system connects the test cell system, for recording hydrate in test cell system in real time
Growing state, taken the photograph image is presented in real time, and carry out record storage；
The test cell system include normal pressure visualization reaction unit, synthesis under normal pressure groove, liquid inlet, liquid outlet,
Test cell part, the side wall of the visualization reaction unit is provided with to connect on the synthesis under normal pressure groove, the side wall and is provided with
It is additionally provided with the liquid inlet, the liquid outlet, the side wall in visual windows, the synthesis under normal pressure groove described in being provided with
Test cell part, the test cell part includes solid metal block, suprasil frame, and the solid metal block is provided with several
Suprasil frame.
Solid metal block generates the wall of hydrate to simulate in actual sea-bottom oil-gas pipeline, suprasil frame can be held
By minimum subzero 60 DEG C of temperature, the success tested under cryogenic conditions can be ensured to greatest extent.
According to currently preferred, one layer of stainless steel pitch cutting, the stainless steel pitch cutting are stained with the solid metal block
Several suprasil frames are set by neck.
The advantage designed herein is, the motion of suprasil frame is limited when playing fixed suprasil frame and measurement adhesion
The effect of track.
According to currently preferred, the suprasil frame is the square without top surface, without hollow out in the middle of bottom surface.
The advantage designed herein is, plays limitation hydrate generation area, assists measurement hydrate wall adhesion, sees
Examine the effect that hydrate generates form in wall.
According to currently preferred, the visual windows include white glass form, lucite form successively from inside to outside,
The white glass form, lucite form are lucite.
Course of reaction is shot by microscopic observation system as form equipped with white glass in synthesis under normal pressure front of the slot,
Real Time Observation record is carried out to hydrate wall generation growing state, it is main in the additional one layer of lucite form of white glass form
It is totally-enclosed in lucite form, full of dry air, due to the capacity of heat transmission of air if the principle based on double glazing
Difference, so as to avoid the generation of inside and outside form water smoke.
According to currently preferred, the cycle refrigeration system includes low temperature thermostat bath, circulation fluid entrance, circulation fluid and gone out
Mouthful, the circulation fluid entrance be connected by circulation conduit with the liquid outlet, the circulation fluid outlet pass through circulation conduit and
The liquid inlet connection.
Cycle refrigeration system and test cell system connectivity, by circulation fluid (main component is ethylene glycol) in two systems
Circulation so that keep normal pressure visualize reaction unit low temperature it is constant.
According to currently preferred, the microtechnique system includes digital display type pull and push dynamometer, cross slid platform, the digital display
Formula pull and push dynamometer is fixed on the cross slid platform, and crooked joint is provided with the top of the digital display type pull and push dynamometer, and the bending connects
Head is provided with stainless steel substrates, and the stainless steel substrates are fitted on the frame wall of the suprasil frame.
By slowly rotating the swingle of precise cross-shaped slide unit, make digital display type pull and push dynamometer to the hydration in suprasil frame
Nitride layer uniformly slowly applies push-and-pull, and digital display type pull and push dynamometer records added thrust in real time, when suprasil frame is moved along neck
When dynamic, digital display type pull and push dynamometer records the adhesion that greatest measure is hydrate.Its digital display type tensiometer will survey adhesion
Power is accurate to after decimal point four.
According to currently preferred, the microscopic observation system includes computer, ccd image sensor, even becomes camera lens, hair
One end on optical diode LED intense light sources, microscope crossbeam, main vertical rod, light source control box, base, the ccd image sensor
Connection is described even to become camera lens, for implementing the growthform of observation and record hydrate in metal wall, the ccd image sensing
Device, the camera lens that even becomes are each attached on the micro- crossbeam, the ccd image sensor, described even become camera lens, described micro-
Crossbeam is fixed in the main vertical rod by the sliding recess in the main vertical rod, and the main vertical rod is vertically fixed on the base
On, the LED intense light source is fixed on the leading portion for even becoming camera lens, for being carried into the test cell system
For light source, the light source control box is used to adjusting the brightness of LED intense light source, the ccd image sensor it is another
One end connects computer by data wire；
Ccd image sensor is connected with even becoming camera lens, is fixed and is moved by microscope crossbeam, main vertical rod, base,
Make even to become the double-deck observation window that camera lens is directed at synthesis under normal pressure groove in test cell system all the time, in real time in record synthesis under normal pressure groove
The growing state of hydrate, meanwhile, ccd image sensor one end is connected with computer, and taken the photograph image is presented on into calculating in real time
In machine screen, and carry out record storage.
The method of said apparatus acquisition visualization hydrate wall generation form and wall adhesion, including step are as follows：
(1) to normal pressure visualization reaction unit injection circulation fluid ethylene glycol；
(2) start cycle refrigeration system, the temperature in the normal pressure visualization reaction unit is adjusted to T1, (- 10) DEG C<T1<
(-2)℃；
(3) poured into the synthesis under normal pressure grooveThe pentamethylene of volume, cools down 20-40min；
(4) solid metal block is immersed in liquid nitrogen and cooled down, after after solid metal block completely cooling, using distilling water vapour
Condensation solid metal block wall after the cooling period generate one layer of snowy white ice film, several described suprasil frames are led to
Cross the neck to be arranged in the solid metal block, the solid metal block provided with suprasil frame several described is put into institute
State in the pentamethylene in synthesis under normal pressure groove；
(5) cycle refrigeration system is adjusted, with 0.5-1.5 DEG C/min programming rate, cycle refrigeration system temperature is improved, directly
To (- 0.5) DEG C -0.5 DEG C, and more than 30min is maintained in this temperature, continue, with 0.2-1.2 DEG C/min programming rate, to improve
Cycle refrigeration system temperature, until T2, (- 1) DEG C<T2<7℃；
(6) in step (1)-step (5), the microscopic observation system Real Time Observation, the generation shape of record hydrate are passed through
State, and every 20-40min syringes into the synthesis under normal pressure groove plus 0.05-0.15ml water, every 2h to the normal pressure
Reactive tank adds 4-6ml pentamethylene；
(7) refrigeration system temperature to be recycled reaches T2Afterwards, continue to test 5-10h, rotate cross slid platform digital display type push-and-pull
Power meter is moved forward, and promotes the suprasil frame to be moved along stainless steel neck, and the wall of the suprasil inframe is hydrated
Thing is peeled off, and the maximum of digital display type pull and push dynamometer record is hydrate wall adhesion；
(8) repeat to test several times according to step (1)-step (7), take several hydrate walls drawn under similarity condition
Face adhesion, averages as final hydrate wall adhesion.
Beneficial effects of the present invention are：
The present invention can be relatively good research and monitoring pentamethylene hydrate wall generation, growth and deposition conditions,
The condition limitation that hydrate must be generated under hyperbaric environment is eliminated, different affecting factors are intuitively observed, such as：Wall material
Matter, wall roughness, temperature, hydrate inhibitor etc. to pentamethylene hydrate wall grow and its mechanical characteristic influence,
The adhesion of measurement wall generation pentamethylene hydrate that simultaneously can be more accurate and visual.
Brief description of the drawings
Fig. 1 visualizes the structural representation of the experimental provision of hydrate wall adhesion mechanics characteristic for the present invention；
Fig. 2 is the structural representation that normal pressure of the present invention visualizes reaction unit；
Fig. 3 is the structural representation of test cell part of the present invention；
A series of generation aspect graph for hydrates that Fig. 4 is obtained for the present invention by microscope；
1st, computer, 2, data wire, 3, ccd image sensor, 4, even become camera lens, 5, LED intense light source, 6,
Base, 7, circulation conduit, 8, normal pressure visualization reaction unit, 9, low temperature thermostat bath, 10, cross slid platform, 11, digital display type push-pull effort
Meter, 12, microscope crossbeam, 13, main vertical rod, 14, visual windows, 15, synthesis under normal pressure groove, 16, test cell part, 17, transparent stone
English frame, 18, neck, 19, solid metal block, 20, liquid inlet, 21, liquid outlet.
Embodiment
The present invention is further qualified with reference to Figure of description and embodiment, but not limited to this.
Embodiment 1
A kind of experimental provision for visualizing hydrate wall adhesion mechanics characteristic, as shown in figure 1, including circularly cooling system
System, test cell system, microtechnique system, microscopic observation system；Cycle refrigeration system connecting test cellular system, for for
Test cell system provides steady temperature；Microtechnique system connecting test cellular system, for measuring test cell system in real time
Generation hydrate adhesion in system；Microscopic observation system connecting test cellular system, for recording in real time in test cell system
The growing state of hydrate, taken the photograph image is presented in real time, and carries out record storage；
Test cell system includes normal pressure visualization reaction unit 8, synthesis under normal pressure groove 15, liquid inlet 20, liquid outlet
21st, test cell part 16, visualization reaction unit 8 is processed using 316L stainless steels, for long 170mm, width 170mm, height
70mm hollow structures, the side wall of visualization reaction unit 8 is provided with synthesis under normal pressure groove 15, reaction flute length 50mm, width 40mm, depth
Connection is provided with liquid inlet 20, liquid outlet 21, side wall and is additionally provided with visual windows 14, synthesis under normal pressure groove 15 on 67mm, side wall
Test cell part 16 is inside provided with, test cell part 16 is included in solid metal block 19, suprasil frame 17, solid metal block 19
Provided with 4 suprasil frames 17.Adhesion wall of the solid metal block 19 to provide hydrate generation, its material and sea-bottom oil-gas
Pipeline is identical, generates the wall of hydrate, the length of solid metal block 19 difference in actual sea-bottom oil-gas pipeline to simulate
For 40mm, 37mm, 25mm, suprasil frame 17 can bear minimum subzero 60 DEG C of temperature, can ensure low temperature to greatest extent
Under the conditions of the success tested.The structural representation of normal pressure visualization reaction unit is as shown in Figure 2.
One layer of stainless steel pitch cutting is stained with solid metal block 19,4 necks will be formed on the surface of solid metal block 19,
It is all suprasil frames of the 10mm without top and bottom that a length, width and height are respectively placed in four necks.The advantage designed herein is, rises
The effect of the movement locus of suprasil frame 17 is limited during to fixed suprasil frame 17 and measurement adhesion.The knot of test cell part
Structure schematic diagram is as shown in Figure 3.
Suprasil frame 17 is the square without top surface, without hollow out in the middle of bottom surface, and the length of side is 10mm, the advantage designed herein
It is, plays limitation hydrate generation area, assists measurement hydrate wall adhesion, observation hydrate to generate form in wall
Effect.The structural representation of test cell part 16 is as shown in Figure 3.
Visual windows 14 include white glass form, lucite form, white glass form, lucite successively from inside to outside
Form is lucite.Identical dimensional thickness is installed additional before the long 70mm of white glass form, width 70mm, thickness 3mm, white glass form
For 5mm lucite form, two form spacing 15mm are insulated with the thick lucite of 5mm, so as to avoid the life of water smoke
Into.
Course of reaction is clapped by microscopic observation system as form equipped with white glass in the front end of synthesis under normal pressure groove 15
Take the photograph, Real Time Observation record is carried out to hydrate wall generation growing state, in the additional one layer of lucite form of white glass form,
Be mainly based upon in the principle of double glazing, lucite form it is totally-enclosed, full of dry air, due to the capacity of heat transmission of air
Difference, so as to avoid the generation of inside and outside form water smoke.
Cycle refrigeration system includes low temperature thermostat bath 9 and (is purchased from Ningbo Xin Zhi biotechnologies instrument plant, model DC-
2006), circulation fluid entrance, circulation fluid outlet, circulation fluid entrance are connected by circulation conduit 7 with liquid outlet 21, and circulation fluid goes out
Mouth is connected by circulation conduit 7 with liquid inlet 20.Cycle refrigeration system and test cell system connectivity, it is (main by circulation fluid
It is ethylene glycol to want composition) circulation in two systems so that keep normal pressure visualize reaction unit 8 low temperature it is constant.
Microtechnique system includes digital display type pull and push dynamometer 11 (being purchased from Wenzhou Shan Du instrument companies, model SH-50), ten
Word slide unit 10, digital display type pull and push dynamometer 11 is fixed on cross slid platform 10 by six M4 nuts, and the material of cross slid platform 10 is
316L stainless steels, the top of digital display type pull and push dynamometer 11 is provided with crooked joint, and crooked joint is provided with stainless steel substrates, stainless steel substrates patch
Close on the frame wall of suprasil frame 17.By slowly rotating the swingle of precise cross-shaped slide unit 10, make digital display type pull and push dynamometer
Hydrate layer in 11 pairs of suprasil frames 17 uniformly slowly applies push-and-pull, and digital display type pull and push dynamometer 11 is pushed away added by record in real time
Power, when suprasil frame 17 is moved along neck 18, it is hydrate that digital display type pull and push dynamometer 11, which records greatest measure,
Adhesion.Surveyed adhesion is accurate to after decimal point four by its digital display type tensiometer 11.
Microscopic observation system includes computer 1, ccd image sensor 3, even becomes camera lens 4 (14-90 times of amplification), luminous two
One end on pole pipe LED intense light sources 5, microscope crossbeam 12, main vertical rod 13, light source control box, base 6, ccd image sensor 3
Connection is described even to become camera lens 4, for implementing observation and record hydrate in the growthform of metal wall, ccd image sensor
3rd, even become camera lens 4 to be each attached on the micro- crossbeam 12, ccd image sensor 3, even change camera lens 4, micro- crossbeam 12 pass through master
Sliding recess in vertical rod 13 is fixed in main vertical rod 13, and main vertical rod 13 is vertically fixed on base 6, and LED is strong
The company of being fixed on of light source 5 becomes the leading portion of camera lens 4, for providing light source into test cell system, and light source control box, which is used to adjust, to be sent out
The brightness of optical diode LED intense light sources 5, the other end of ccd image sensor 3 connects computer 1 by data wire 2.
Ccd image sensor 3 is connected with even becoming camera lens 4, is fixed by microscope crossbeam 12, main vertical rod 13, base 6
And movement, make even to become the double-deck observation window that camera lens 4 is directed at synthesis under normal pressure groove 15 in test cell system all the time, record is normal in real time
The growing state of hydrate in reactive tank 15 is pressed, meanwhile, the one end of ccd image sensor 3 is connected with computer 1, by taken the photograph image
In real time it is presented in the screen of computer 1, and carry out record storage.
Embodiment 2
The described device of embodiment 1 obtains visualization hydrate wall generation form and the method for wall adhesion, including step
It is rapid as follows：
(1) to the normal pressure visualization injection circulation fluid ethylene glycol of reaction unit 8；
(2) start cycle refrigeration system, the temperature that normal pressure is visualized in reaction unit 8 is adjusted to T1, T1=-3 DEG C；
(3) poured into synthesis under normal pressure groove 15The pentamethylene of volume, cools down 30min；
(4) solid metal block 19 is immersed in liquid nitrogen and cools down 5min, after after solid metal block 19 completely cooling, utilize steaming
The wall of solid metal block 19 of the condensation of distilled water steam after the cooling period generates one layer of snowy white ice film, by 4 suprasils
Frame 17 is arranged in solid metal block 19 by neck 18, and the solid metal block 19 provided with 4 suprasil frames 17 is put into often
Press in the pentamethylene in reactive tank 19；
(5) cycle refrigeration system is adjusted, with 1 DEG C/min programming rate, cycle refrigeration system temperature is improved, until to 0
DEG C, and more than 30min is maintained in this temperature, continue, with 0.2 DEG C/min programming rate, to improve cycle refrigeration system temperature, directly
To T2, T2=2 DEG C；
(6) in step (1)-step (5), by microscopic observation system Real Time Observation, the generation form of record hydrate,
And add 0.1ml water into synthesis under normal pressure groove 15 every 30min syringes, add 5ml ring to synthesis under normal pressure groove 15 every 2h
Pentane；In the generation aspect graph such as Fig. 4 of the hydrate that experiment is obtained when just starting shown in (a), experiment carries out acquisition during 30min
In the generation aspect graph such as Fig. 4 of hydrate shown in (b), experiment carries out generation aspect graph such as Fig. 4 of the hydrate of acquisition during 60min
In shown in (c), experiment is carried out in generation aspect graph such as Fig. 4 of the hydrate of acquisition during 90min shown in (d), experiment progress
In the generation aspect graph such as Fig. 4 of the hydrate obtained during 260min shown in (e), experiment carries out the hydrate of acquisition during 280min
Generate in aspect graph such as Fig. 4 shown in (f), (g) institute in the generation aspect graph such as Fig. 4 of the hydrate of acquisition during experiment progress 340min
Show, during experiment progress 350min in the generation aspect graph such as Fig. 4 of the hydrate of acquisition shown in (h), experiment obtained during 400min
In the generation aspect graph such as Fig. 4 of the hydrate taken shown in (i).
(7) refrigeration system temperature to be recycled reaches T2Afterwards, continue to test 5-10h, rotate cross slid platform 10 and digital display type is pushed away
Tensiometer 11 is moved forward, and promotes suprasil frame 17 to be moved along neck 18, and the wall hydrate in suprasil frame 17 is shelled
From the maximum that digital display type pull and push dynamometer 11 is recorded is hydrate wall adhesion；
(8) repeat to test several times according to step (1)-step (7), take several hydrate walls drawn under similarity condition
Face adhesion, averages as final hydrate wall adhesion.
The present embodiment can be relatively good research and monitoring pentamethylene hydrate wall generation, growth and deposition feelings
Condition, eliminates the condition limitation that hydrate must be generated under hyperbaric environment, intuitively observes different affecting factors, such as：Wall
Material, wall roughness, temperature, hydrate inhibitor etc. are to pentamethylene hydrate in wall growth and its shadow of mechanical characteristic
Ring, while measurement wall that can be more accurate and visual generates the adhesion of pentamethylene hydrate.
Embodiment 3
The described device of embodiment 1 obtains visualization hydrate wall generation form and the method for wall adhesion, including step
It is rapid as follows：
(1) to the normal pressure visualization injection circulation fluid ethylene glycol of reaction unit 8；
(2) start cycle refrigeration system, the temperature that normal pressure is visualized in reaction unit 8 is adjusted to T1, T1=-10 DEG C；
(3) poured into synthesis under normal pressure groove 15The pentamethylene of volume, cools down 20min；
(4) solid metal block 19 is immersed in liquid nitrogen and cools down 5min, after after solid metal block 19 completely cooling, utilize steaming
The wall of solid metal block 19 of the condensation of distilled water steam after the cooling period generates one layer of snowy white ice film, by 4 suprasils
Frame 17 is arranged in solid metal block 19 by neck 18, and the solid metal block 19 provided with 4 suprasil frames 17 is put into often
Press in the pentamethylene in reactive tank 19；
(5) cycle refrigeration system is adjusted, with 1 DEG C/min programming rate, cycle refrigeration system temperature is improved, until to 0
DEG C, and more than 30min is maintained in this temperature, continue, with 0.2 DEG C/min programming rate, to improve cycle refrigeration system temperature, directly
To T2, T2=4 DEG C；
(6) in step (1)-step (5), by microscopic observation system Real Time Observation, the generation form of record hydrate,
And add 0.05ml water into synthesis under normal pressure groove 15 every 20min syringes, add 6ml ring to synthesis under normal pressure groove 15 every 2h
Pentane；
(7) refrigeration system temperature to be recycled reaches T2Afterwards, continue to test 5-10h, rotate cross slid platform 10 and digital display type is pushed away
Tensiometer 11 is moved forward, and promotes suprasil frame 17 to be moved along neck 18, and the wall hydrate in suprasil frame 17 is shelled
From the maximum that digital display type pull and push dynamometer 11 is recorded is hydrate wall adhesion；
(8) repeat to test several times according to step (1)-step (7), take several hydrate walls drawn under similarity condition
Face adhesion, averages as final hydrate wall adhesion.
Embodiment 4
The described device of embodiment 1 obtains visualization hydrate wall generation form and the method for wall adhesion, including step
It is rapid as follows：
(1) to the normal pressure visualization injection circulation fluid ethylene glycol of reaction unit 8；
(2) start cycle refrigeration system, the temperature that normal pressure is visualized in reaction unit 8 is adjusted to T1, T1=-2 DEG C；
(3) poured into synthesis under normal pressure groove 15The pentamethylene of volume, cools down 40min；
(4) solid metal block 19 is immersed in liquid nitrogen and cools down 5min, after after solid metal block 19 completely cooling, utilize steaming
The wall of solid metal block 19 of the condensation of distilled water steam after the cooling period generates one layer of snowy white ice film, by 4 suprasils
Frame 17 is arranged in solid metal block 19 by neck 18, and the solid metal block 19 provided with 4 suprasil frames 17 is put into often
Press in the pentamethylene in reactive tank 19；
(5) cycle refrigeration system is adjusted, with 0.5 DEG C/min programming rate, cycle refrigeration system temperature is improved, until arriving
0 DEG C, and more than 30min is maintained in this temperature, continue, with 0.5 DEG C/min programming rate, to improve cycle refrigeration system temperature, directly
To T2, T2=5 DEG C；
(6) in step (1)-step (5), by microscopic observation system Real Time Observation, the generation form of record hydrate,
And add 0.15ml water into synthesis under normal pressure groove 15 every 40min syringes, add 6ml ring to synthesis under normal pressure groove 15 every 2h
Pentane；
(7) refrigeration system temperature to be recycled reaches T2Afterwards, continue to test 5-10h, rotate cross slid platform 10 and digital display type is pushed away
Tensiometer 11 is moved forward, and promotes suprasil frame 17 to be moved along neck 18, and the wall hydrate in suprasil frame 17 is shelled
From the maximum that digital display type pull and push dynamometer 11 is recorded is hydrate wall adhesion；
(8) repeat to test several times according to step (1)-step (7), take several hydrate walls drawn under similarity condition
Face adhesion, averages as final hydrate wall adhesion.
Claims (8)
1. it is a kind of visualize hydrate wall adhesion mechanics characteristic experimental provision, it is characterised in that including cycle refrigeration system,
Test cell system, microtechnique system, microscopic observation system；
The cycle refrigeration system connects the test cell system, for providing constant temperature for the test cell system
Degree；The microtechnique system connects the test cell system, and water is generated for measuring in real time in the test cell system
Compound adhesion；The microscopic observation system connects the test cell system, for recording water in test cell system in real time
The growing state of compound, taken the photograph image is presented in real time, and carries out record storage；
The test cell system includes normal pressure visualization reaction unit, synthesis under normal pressure groove, liquid inlet, liquid outlet, test
Unit piece, the side wall of the visualization reaction unit is provided with connection on the synthesis under normal pressure groove, the side wall and is provided with described
It is additionally provided with liquid inlet, the liquid outlet, the side wall in visual windows, the synthesis under normal pressure groove and is provided with the test
Unit piece, the test cell part includes solid metal block, suprasil frame, and the solid metal block is transparent provided with several
Quartzy frame.
2. a kind of experimental provision for visualizing hydrate wall adhesion mechanics characteristic according to claim 1, its feature exists
In being stained with one layer of stainless steel pitch cutting in the solid metal block, the stainless steel pitch cutting is set described in several by neck
Suprasil frame.
3. a kind of experimental provision for visualizing hydrate wall adhesion mechanics characteristic according to claim 2, its feature exists
In the suprasil frame is the square without top surface, without hollow out in the middle of bottom surface.
4. a kind of experimental provision for visualizing hydrate wall adhesion mechanics characteristic according to claim 1, its feature exists
In the visual windows include white glass form, lucite form, the white glass form, organic glass successively from inside to outside
Glass form is lucite.
5. a kind of experimental provision for visualizing hydrate wall adhesion mechanics characteristic according to claim 1, its feature exists
In the cycle refrigeration system includes low temperature thermostat bath, circulation fluid entrance, circulation fluid outlet, and the circulation fluid entrance is by following
Ring conduit is connected with the liquid outlet, and the circulation fluid outlet is connected by circulation conduit with the liquid inlet.
6. a kind of experimental provision for visualizing hydrate wall adhesion mechanics characteristic according to claim 1, its feature exists
In the microtechnique system includes digital display type pull and push dynamometer, cross slid platform, and the digital display type pull and push dynamometer is fixed on described ten
On word slide unit, be provided with crooked joint at the top of the digital display type pull and push dynamometer, the crooked joint is provided with stainless steel substrates, it is described not
Rust steel disc is fitted on the frame wall of the suprasil frame.
7. a kind of experimental provision for visualizing hydrate wall adhesion mechanics characteristic according to claim 1, its feature exists
In, the microscopic observation system include computer, ccd image sensor, even become camera lens, it is LED intense light source, micro-
One end connection even change camera lens on mirror crossbeam, main vertical rod, light source control box, base, the ccd image sensor, is used for
Implement the growthform of observation and record hydrate in metal wall, the ccd image sensor, the camera lens that even becomes are fixed
On the micro- crossbeam, the ccd image sensor, the camera lens, the micro- crossbeam of even becoming pass through in the main vertical rod
Sliding recess be fixed in the main vertical rod, the main vertical rod is vertically fixed on the base, the LED
Intense light source is fixed on the leading portion for even becoming camera lens, for providing light source, the light source control into the test cell system
Box is used for the brightness for adjusting LED intense light source, and the other end of the ccd image sensor is connected by data wire to be counted
Calculation machine.
8. a kind of experimental provision of visualization hydrate wall adhesion mechanics characteristic described in claim 6 obtains visualization hydration
Thing wall generates form and the method for wall adhesion, it is characterised in that as follows including step：
(1) to normal pressure visualization reaction unit injection circulation fluid ethylene glycol；
(2) start cycle refrigeration system, the temperature in the normal pressure visualization reaction unit is adjusted to T1, (- 10) DEG C<T1<(-2)
℃；
(3) poured into the synthesis under normal pressure grooveThe pentamethylene of volume, cools down 20-40min；
(4) solid metal block is immersed in liquid nitrogen and cooled down, after after solid metal block completely cooling, using distilling the cold of water vapour
The solid metal block wall of solidifying effect after the cooling period generates one layer of snowy white ice film, and several described suprasil frames are passed through into institute
State neck to be arranged in the solid metal block, the solid metal block provided with suprasil frame several described is put into described normal
Press in the pentamethylene in reactive tank；
(5) cycle refrigeration system is adjusted, with 0.5-1.5 DEG C/min programming rate, cycle refrigeration system temperature is improved, until arriving
(- 0.5) DEG C -0.5 DEG C, and more than 30min is maintained in this temperature, continue, with 0.2-1.2 DEG C/min programming rate, to improve circulation
Refrigeration system temperature, until T2, (- 1) DEG C<T2<7℃；
(6) in step (1)-step (5), by the microscopic observation system Real Time Observation, the generation form of record hydrate, and
Every 20-40min syringes into the synthesis under normal pressure groove plus 0.05-0.15ml water, every 2h to the synthesis under normal pressure
Groove adds 4-6ml pentamethylene；
(7) refrigeration system temperature to be recycled reaches T2Afterwards, continue test 5-10h, rotate cross slid platform digital display type pull and push dynamometer to
Preceding movement, promotes the suprasil frame to be moved along stainless steel neck, and the wall hydrate of the suprasil inframe is peeled off,
The maximum of digital display type pull and push dynamometer record is hydrate wall adhesion；
(8) repeat to test several times according to step (1)-step (7), take several hydrate walls drawn under similarity condition to glue
Attached power, averages as final hydrate wall adhesion.
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