CN106596224B - Two-step method prepares the experimental provision and method of gas hydrates rock sample - Google Patents

Two-step method prepares the experimental provision and method of gas hydrates rock sample Download PDF

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CN106596224B
CN106596224B CN201611152896.0A CN201611152896A CN106596224B CN 106596224 B CN106596224 B CN 106596224B CN 201611152896 A CN201611152896 A CN 201611152896A CN 106596224 B CN106596224 B CN 106596224B
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rock sample
pressure
hydrate
gas
reaction kettle
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CN106596224A (en
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闫传梁
程远方
韩忠英
丁吉平
滕飞
李庆超
张怀文
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China University of Petroleum UPC East China
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China University of Petroleum UPC East China
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10LFUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L3/00Gaseous fuels; Natural gas; Synthetic natural gas obtained by processes not covered by subclass C10G, C10K; Liquefied petroleum gas
    • C10L3/06Natural gas; Synthetic natural gas obtained by processes not covered by C10G, C10K3/02 or C10K3/04
    • C10L3/10Working-up natural gas or synthetic natural gas
    • C10L3/108Production of gas hydrates
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10LFUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L7/00Fuels produced by solidifying fluid fuels
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/42Low-temperature sample treatment, e.g. cryofixation

Abstract

The present invention relates to experimental provisions and method that a kind of two-step method prepares gas hydrates rock sample;Its technical solution be include freezer, reaction kettle, confining pressure pump, air supply system, computer data acquisition system etc., all experimental systems are in low-temperature cold store, and the temperature control system carried by freezer adjusts temperature of ice house;Confining pressure pump output terminal is connected with reaction kettle;The output end of air supply system is connected with reaction kettle;Gas flowmeter, temperature sensor are connected with computer acquisition system, the method that two-step method prepares gas hydrates rock sample, it include: the first step, hydrate is generated in rock sample, second step, by near methane gas pressure reduction to vapor pressure but slightly above vapor pressure, recrystallize hydrate.It solves the problems, such as the preparation of gas hydrates rock sample using the present invention, can get the hydrate rock sample being more nearly with practical hydrate reservoir physico mechanical characteristic, provide experiment support for the probing and exploitation of natural gas hydrate resources.

Description

Two-step method prepares the experimental provision and method of gas hydrates rock sample
Technical field
The present invention relates to a kind of Gas Hydrate Drilling development field, in particular to a kind of two-step method prepares gas water Close the experimental provision and method of object rock sample.
Background technique
China is that maximum energy-consuming state, energy consumption account for the 23% of the whole world, while China's using energy source in the world Rate is low, unbalance of structure, and the natural gas proportion as clean energy resource is smaller, compare shared by petroleum, coal it is higher, it is global in recent years Climate change causes people to pay much attention to, low-carbon energy-saving, Optimization of Energy Structure, and it is imperative to develop clean energy resource.Gas water Closing object is crystalline compounds made of natural gas and water molecules, it has, and stock number is big, the high and low pollution of energy density etc. Advantage is acknowledged as the important subsequent clean energy resource with good prospect, realizes the development and utilization of natural gas hydrate resources For promote China's energy industry development, improve energy consumption structure, ensure energy security supply, promote Ecological Civilization Construction, The sustainable development of socio-economy is kept to be of great significance.Meanwhile being researched and developed and being planned according to state key, carry out gas hydrates Important energy source during pilot production becomes 13 is strategic.It is limited by hydrate phase balance condition, gas hydrates can only be Exist under high pressure low temperature, is difficult original position and gets hydrate formation rock core.During boring and coring, the variation of load will cause water The disturbance of object earth formation is closed, the variation of pressure and temperature also can make partially hydrated object decompose, and the core of acquirement cannot be true The physico mechanical characteristic of real reflection hydrate formation.Thus the experimental study of hydrate formation mainly passes through laboratory at present It synthesizes synthetic core sample containing hydrate and carries out dependence test.
It in recent years, is to undergo to overflow in sedimentation environment by hydrate although being manually prepared for rock sample containing hydrate What long period was formed, depositional environment is complicated, and indoor preparation is rapid synthesis, synthesis condition also differed with actual formation compared with Greatly.Such as application No. is hydrate sediment in-situ preparations and decomposition and its infiltration that the patent of invention of CN201110353136.7 is announced Saturating rate measures integrated apparatus, although the fabricated in situ of achievable hydrate sediment and test, hydrate is advanced when preparing Row pressurization, which prepares rock sample skeleton and inputs methane gas and water again, generates hydrate in rock sample hole, this is with partially hydrated object with stratum Physical condition existing for the form of skeleton is not inconsistent, while being difficult to control accurately the realization of hydrate concentration yet;Invention preparation It is that methane and hydrate rapid crystallization is made to generate hydrate in the great situation of degree of supercooling when hydrate, and in actual formation then It is the hydrate slowly generated under the pressure and temperature close to phase balance condition, and degree of supercooling is bigger, will affect hydrate crystalline substance The tissue topography of body and crystalline types keep the lattice of artificial hydrate sample mechanical cementing, rather than the lattice of actual formation Cementing form, these physico mechanical characteristics that will lead to the rock sample containing hydrate of preparation differ larger with actual reservoir.
It is accurate to obtain and actual formation physico mechanical characteristic for the requirement for meeting natural gas hydrate resources probing and exploitation Hydrate synthetic core sample the most similar, need develop the hydrate people that can really reflect hydrate formation physico mechanical characteristic Lithogenesis sample preparation method.
Summary of the invention
The purpose of the present invention is to drawbacks described above of the existing technology, a kind of two-step method is provided and prepares gas water The experimental provision and method of object rock sample are closed, is prepared with obtaining the hydrate rock sample being more nearly with actual formation physico mechanical characteristic Method provides experiment support for the probing and exploitation of natural gas hydrate resources.
A kind of two-step method that the present invention mentions prepares the experimental provision of gas hydrates rock sample, installation reaction in freezer 1 Kettle 2, methane gas cylinder 3, gas flowmeter 6, recycling air bag 15, confining pressure pump 17, computer data acquisition system 21, the first blow valve 14, the second blow valve 19, freezer 1 can realize the temperature control of -20 DEG C ~ room temperature,
The methane gas cylinder 3 is connected by the first high pressure line 11 with reaction kettle 2 after pressure reducing valve 4, is used to in sample The generation of hydrate provides methane;
Confining pressure pump 17 is connected by the second high pressure line 16 with reaction kettle 2, for enclosing to the sample application in reaction kettle 2 Pressure;
First blow valve 14 is mounted on third high pressure line 12, and is connected by third high pressure line 12 with reaction kettle 2, For being vented to the methane in reaction kettle 2;
Second blow valve 19 is mounted on the 6th high pressure line 18, and is connected by the 6th high pressure line 18 with reaction kettle 2, For being vented to confining pressure fluid in reaction kettle 2;
Second shut-off valve 10 is on the 4th high pressure line 22, one end of the 4th high pressure line 22 and the first high pressure line 11 It is connected, the other end is connected with third high pressure line 12, for realizing sample both ends while supplying;
One end of first data transmission line 7 is connected with gas flowmeter 6, the other end and 21 phase of computer data acquisition system Even, for realizing the real-time monitoring to methane flow;
One end of second data line 20 is connected with temperature sensor 29, the other end and computer data acquisition system 21 It is connected, for realizing the real-time monitoring generated to hydrate with decomposition.
Preferably, aforesaid reaction vessel 2 includes push-down head 23, seaming chuck 26, the first seepage flow pad 27, the second seepage flow pad 28, rock Sample oil removal set 24, rock sample 25 is clipped between push-down head 23 and seaming chuck 26, and the first infiltration is equipped between rock sample 25 and push-down head 23 Pad 27 is flowed, the second seepage flow pad 28 is installed between rock sample 25 and seaming chuck 26, blocks pipeline for preventing sedimentary particle from falling off; Rock sample oil removal set 24 is located at 25 outside of rock sample, for realizing the separation to rock sample pore pressure system and confining pressure system.
Preferably, set in above-mentioned seaming chuck 26 there are two circular channel, one of circular channel to realize methane from It flows out the end face of rock sample 25;Another circular channel is used to place temperature sensor 29.
Preferably, processed on the lower end surface section of above-mentioned seaming chuck 26 it is fluted, convenient for methane in 25 exit end face of rock sample Flowing.
Preferably, the centre of above-mentioned push-down head 23 is equipped with a circular channel, real methane to be transmitted in rock sample 25 Uniformly gas supply is realized in the flowing of existing methane gas.
Preferably, on the upper surface section of above-mentioned push-down head 23 with fluted, convenient for methane gas in 25 arrival end of rock sample The flowing in face.
A kind of two-step method that the present invention mentions prepares the application method of the experimental provision of gas hydrates rock sample, preparation Process is carried out in two steps, the first step, and hydrate, second step, by methane gas pressure reduction to the pressure that balances each other are generated in rock sample Power nearby but slightly above vapor pressure, aggravates lattice activity, lattice form and actual reservoir are closer.
A kind of two-step method that the present invention mentions prepares the application method of the experimental provision of gas hydrates rock sample, specific real Test that steps are as follows:
(1) in subzero low temperature environment according to the mineral composition of actual formation and hydrate concentration sand, soil and Powder shaped distillation water-ice block is pressed into the skeleton of rock sample;
(2) rock sample oil removal set 24 will be superscribed on the outside of rock sample to be placed in reaction kettle 2;
(3) confining pressure pump 17 is opened, make to be full of low temperature resistant fluid in reaction kettle 2 and applies 0.5MPa confining pressure;
(4) the second shut-off valve 10, third shut-off valve 13 and vacuum block valve 9 is opened to vacuumize rock sample hole;
(5) the first shut-off valve 5 is opened, rock sample is supplied using methane gas cylinder 3, increases pore pressure, utilizes simultaneously Confining pressure pump 17 increases confining pressure, adds axis pressure using the servo-control system being connected with push-down head 23, remains that confining pressure is greater than gas Pressure 0.5MPa or more maintains confining pressure, axis pressure and gas pressure constant when pressure reaches setting value;
(6) temperature of ice house is slowly increased to 0 DEG C or more, keeps confining pressure, axis pressure and gas pressure constant, methane and water generate Hydrate;
(7) it when the accumulative reading of gas flowmeter 6 is no longer changed, maintains 24 hours, hydrate generates completely;
(8) gas pressure is reduced to the hydrate above 0.1MPa of Critical Stability pressure according to hydrate phase balance curve, protected It holds 12 hours, the cementing lattice that becomes of machinery when making crystal of hydrate form from just generating is cementing, prepared by rock sample containing hydrate Finish.
Preferably, the diameter 25mm of above-mentioned rock sample, height 50mm.
Compared with the prior art, the present invention has the following beneficial effects:
(1), the present invention solves in artificial natural gas hydrate reservoir rock sample part hydrate existing for bound form Problem, while hydrate is generated under practical crustal stress states, it is more close with actual reservoir;
(2), by two-step method, hydrate is recrystallized near vapor pressure, makes the lattice types of hydrate rock sample It is more close with actual reservoir, it is more guiding to hydrate reservoir Related Experimental Study;
(3), hydrate is generated by the way of the gas supply of both ends, reduces the spilling of fluid, makes the meter of hydrate concentration It calculates more accurate;
(4), main equipment of the invention is in original hydrate fabricated in situ and rock mechanics triaxial tests equipment base It is transformed on plinth, equipment cost is greatly saved, and can satisfy requirement of experiment;
(5), good simulation can be carried out to the gas hydrates synthesis in seabed and frozen soil field, natural gas is hydrated The research of object physico mechanical characteristic has great impetus.
Detailed description of the invention
Fig. 1 is the experimental provision schematic diagram that two-step method of the present invention prepares gas hydrates rock sample;
Fig. 2 is reaction kettle schematic diagram of internal structure;
Fig. 3 is seaming chuck schematic diagram in reaction kettle;
Fig. 4 is the bottom view in Fig. 3;
Fig. 5 is push-down head schematic diagram in reaction kettle;
Fig. 6 is the top view in Fig. 5;
In figure, 1, freezer, 2, reaction kettle, 3, methane gas cylinder, 4, pressure reducing valve, the 5, first shut-off valve, 6, gas flowmeter, 7, First data transmission line, the 8, the 5th high pressure line, 9, vacuum block valve, the 10, second shut-off valve, the 11, first high pressure line, 12, Third high pressure line, 13, third shut-off valve, the 14, first blow valve, 15, recycling air bag, the 16, second high pressure line, 17, confining pressure Pump, the 18, the 6th high pressure line, the 19, second blow valve, the 20, second data line, 21, computer data acquisition system, 22, 4th high pressure line, 23, push-down head, 24, oil removal set, 25, rock sample, 26, seaming chuck, the 27, first seepage flow pad, the 28, second seepage flow Pad, 29, temperature sensor.
Specific embodiment
As shown in Figure 1, two-step method prepares the experimental provision of gas hydrates rock sample, installed in freezer 1 reaction kettle 2, Methane gas cylinder 3, gas flowmeter 6, recycling air bag 15, confining pressure pump 17, computer data acquisition system 21, the first blow valve 14, Second blow valve 19 etc..
The methane gas cylinder is connected by the first high pressure line 11 with reaction kettle 2 after pressure reducing valve 4, is used to water in sample The generation for closing object provides methane;
Confining pressure pump 17 is connected by the second high pressure line 16 with reaction kettle 2, for enclosing to the sample application in reaction kettle 2 Pressure;
Freezer 1 can realize the temperature control of -20 DEG C ~ room temperature, and all experimental facilities and experimentation carry out in freezer;
First blow valve 14 is mounted on third high pressure line 14, and is connected by third high pressure line 14 with reaction kettle 2, For being vented to the methane in reaction kettle 2;
Second blow valve 19 is mounted on the 6th high pressure line 18, and is connected by the 6th high pressure line 18 with reaction kettle 2, For being vented to confining pressure fluid in reaction kettle 2;
First shut-off valve 10 is on the 4th high pressure line 22, one end of the 4th high pressure line 22 and the first high pressure line 11 It is connected, the other end is connected with third high pressure line 12, for realizing sample both ends while supplying;
One end of first data transmission line 7 is connected with gas flowmeter 6, the other end and 21 phase of computer data acquisition system Even, for realizing the real-time monitoring to methane flow;
One end of second data line 20 is connected with temperature sensor 29, the other end and computer data acquisition system 21 Be connected, hydrate is generated and the real-time monitoring of decomposition for realizing (decomposition of hydrate is absorbed heat, and hydrate generates heat release).
As shown in Fig. 2, the reaction kettle 2 includes: push-down head 23, seaming chuck 26, the first seepage flow pad 27, the second seepage flow pad 28, rock sample oil removal set 24.Rock sample 25 is clipped between push-down head 23 and seaming chuck 26, and is equipped between rock sample 25 and push-down head 23 One seepage flow pad 27 is equipped with the second seepage flow pad 28 between rock sample 25 and seaming chuck 26, for preventing sedimentary particle from falling off blocking Pipeline.Rock sample oil removal set 24 is located at 25 outside of rock sample, for realizing the separation to rock sample pore pressure system (methane) and confining pressure system It is independent.
As shown in Figure 3-4, circular channel there are two setting in seaming chuck 26, one of channel is to realize methane from rock sample 25 end face outflow;Another channel is used to place temperature sensor 29;It is machined on the lower end surface section of seaming chuck 26 multiple Groove, convenient for methane 25 exit end face of rock sample flowing, and above-mentioned groove be a quarter size eight arc grooves combine At two circular configurations.
As seen in figs. 5-6, the centre of push-down head 23 is equipped with a circular channel, methane to be transmitted in rock sample 25, Realize the flowing of methane gas;With fluted on the upper surface section of push-down head 23, convenient for methane gas in 25 arrival end of rock sample The flowing in face, and above-mentioned groove is combined into two circular configurations for eight arc grooves of a quarter size.
The two-step method that the present invention mentions prepares the application method of the experimental provision of gas hydrates rock sample, preparation process It is carried out in two steps, the first step, hydrate is generated in rock sample, second step is attached to vapor pressure by methane gas pressure reduction Closely but slightly above vapor pressure aggravates lattice activity, and lattice form and actual reservoir are closer.
Steps are as follows for specific experiment of the invention:
(1) mineral composition and hydrate of (this experiment is -5 DEG C) according to actual formation in subzero low temperature environment Saturation degree sand, soil and powder shaped distillation water-ice block are pressed into rock sample bone with certain mass ratio (this experiment is 1:1:0.5) Frame.The diameter 25mm of rock sample, height 50mm.
(2) rock sample oil removal set 24 will be superscribed on the outside of the rock sample suppressed to be placed in reaction kettle 2.
(3) confining pressure pump 17 is opened, make to be full of low temperature resistant fluid in reaction kettle 2 and applies 0.5MPa confining pressure.
(4) open the second shut-off valve 10, third shut-off valve 13 and vacuum block valve 9 rock sample hole is carried out vacuumizing 1 it is small When.
(5) the first shut-off valve 5 is opened, rock sample is supplied using methane gas cylinder 3, increases rock sample pore pressure, simultaneously Increase confining pressure using confining pressure pump 17, adds axis pressure using the servo-control system being connected with push-down head 23, remain that confining pressure is greater than Gas pressure 0.5MPa or more (according to the reservoir conditions of this experiment simulation, sets methane air pressure when pressure reaches setting value Power is 10MPa, and axis presses 14MPa, confining pressure 12MPa), maintain confining pressure, axis pressure and gas pressure constant.
(6) temperature of ice house is slowly increased to 0 DEG C or more (this experiment is set as 5 DEG C), keeps confining pressure and gas pressure not Become, methane and water generate hydrate.
(7) it when the accumulative reading of gas flowmeter 6 is no longer changed, maintains 24 hours, it is believed that hydrate is complete It is complete to generate, using the variation calculated hydration object saturation degree of gas flow count value, with the hydrate using ice cube Mass Calculation Saturation degree mutually corrects.
(8) according to hydrate phase balance curve reduce gas pressure to the above 0.1MPa(of hydrate Critical Stability pressure such as This experimental temperature is 5 DEG C, critical pressure 4.2MPa, then reduces pressure to 4.3MPa), it is unknown if other decomposition pressures When hydrate, temperature sensor 29 and gas flowmeter 6 can be paid close attention to the moment, if temperature changes or pressure flow becomes extremely Change, illustrate that hydrate starts to decompose, then stop being depressured and increasing 0.1MPa pressure) it is kept for 12 hours, make crystal of hydrate form The cementing lattice that becomes of machinery when from just generating is cementing, and the preparation of rock sample containing hydrate finishes.
The above, is only part preferred embodiment of the invention, and anyone skilled in the art may benefit Equivalent technical solution is modified or is revised as with the technical solution of above-mentioned elaboration.Therefore, technology according to the present invention Any simple modification or substitute equivalents that scheme is carried out, belong to the greatest extent the scope of protection of present invention.

Claims (2)

1. a kind of two-step method prepares the application method of the experimental provision of gas hydrates rock sample, it is characterized in that specific experiment step It is as follows:
(1) according to the mineral composition of actual formation and hydrate concentration sand, soil and powder in subzero low temperature environment Shape distilled water ice cube is pressed into the skeleton of rock sample;
(2) rock sample oil removal set (24) will be superscribed on the outside of rock sample to be placed in reaction kettle (2);
(3) confining pressure pump (17) is opened, make to be full of low temperature resistant fluid in reaction kettle (2) and applies 0.5MPa confining pressure;
(4) the second shut-off valve (10), third shut-off valve (13) and vacuum block valve (9) is opened to vacuumize rock sample hole;
(5) the first shut-off valve (5) are opened, rock sample is supplied using methane gas cylinder (3), increased pore pressure, utilize simultaneously Confining pressure pumps (17) and increases confining pressure, adds axis pressure using the servo-control system being connected with push-down head (23), remains that confining pressure is greater than Gas pressure 0.5MPa maintains confining pressure, axis pressure and gas pressure constant when pressure reaches setting value;
(6) temperature of ice house is slowly increased to 0 DEG C or more, keeps confining pressure, axis pressure and gas pressure constant, and methane and water are generated and is hydrated Object;
(7) it when gas flowmeter (6) accumulative reading is no longer changed, maintains 24 hours, hydrate generates completely;
(8) gas pressure is reduced to the hydrate above 0.1MPa of Critical Stability pressure according to hydrate phase balance curve, keeps 12 Hour, the cementing lattice that becomes of machinery when making crystal of hydrate form from just generating is cementing, and the preparation of rock sample containing hydrate finishes.
2. two-step method according to claim 1 prepares the application method of the experimental provision of gas hydrates rock sample, special Sign is: the diameter 25mm of the rock sample, height 50mm.
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