CN105699247B - A kind of synthesis of gas hydrates and decomposition experiment method and experimental system - Google Patents
A kind of synthesis of gas hydrates and decomposition experiment method and experimental system Download PDFInfo
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Abstract
The present invention provides a kind of synthesis of gas hydrates and decomposition experiment method and experimental system, the entrance criterion chamber volume and export standard chamber volume for including, the synthesis and decomposition of gas hydrates can be optimized, the use of its entrance criterion chamber volume can be not only used for stage by stage to the porous media supply natural gas in autoclave, it can be used for accurately calculating the consumption of natural gas in gas hydrates synthesis process, the use of export standard chamber volume can not only be such that the decomposition of gas hydrates carries out stage by stage, solve the problems, such as that temperature decrease leads to pipeline ice blockage when gas hydrate dissociation in common decomposition method, it can be used for the amount of natural gas of metering gas hydrate dissociation process release.
Description
Technical field
The invention belongs to gas hydrates experimental field, in particular to a kind of gas hydrates synthesis and decomposition experiment
Method and experimental system.
Background technique
Gas hydrates are given by many countries as a kind of cleaning, efficient and rich reserves novel potential energy source
It gives highest attention and carries out primary study.Since the 1990s, with the Gas Hydrate of countries in the world discovery
Increase the further intensification recognized with people gas hydrates, the research of gas hydrates is worldwide rapid
Expand.Its research emphasis has also turned to the practical development phase, this stage, gas hydrate study either method or depth
Degree is all a a progressive step.It is made great progress in terms of the basic research of gas hydrates in the past 20 years, is related to day
The physicochemical characteristics of right gas hydrate forms and decomposes thermodynamics and kinetics, output condition, the regularity of distribution, formation mechenism, surveys
Spy technology and environment influence etc..And prior art progress hydrate sediment scene coring is still not mature enough, therefore various countries
Scholar mainly prepares simulating hydrate deposit by laboratory test to the basic research of gas hydrates to realize.
In the prior art, there are mainly two types of methods with decomposition for the experiment synthesis of gas hydrates, first is that in aqueous solution
Middle progress, second is that carried out in porous media, and the synthesis of progress gas hydrates and decomposition experiment are ground in porous media
The case where studying carefully closer practical hydrate mineral reserve, can provide reliable basis for the exploitation of gas hydrates from now on.It is public
In the synthesis and decomposition experiment method and technology patent of the gas hydrates of cloth, to gas hydrates saturation degree in deposit
The method that detection calculates has electrical method, supersonic detection method and time domain reflection technology etc., but the design of these test methods it is complicated,
Higher cost can not accurately calculate gas hydrates saturation degree.Wherein electric-resistivity method is based on effects of ion content
Change and conductivity is caused to change, and methane is difficult to ionize in aqueous solution, ion variation is very little, and therefore, it is difficult to measure.Ultrasound
Detection method and time domain reflection technology must be set up on accurate known calculations model, could be to gas hydrates saturation degree
It is calculated, and the relationship about hydrate concentration and the velocity of sound and dielectric constant has some models at present, one kind is simple
Empirical equation, this class model lacks strict theoretical foundation；Another kind of theory and side to establish on complicated physical model
Journey etc., these model theories derive tightly, but the parameter for being related to calculating is more, and are difficult to determine each parameter under actual conditions
Value.In addition, very big according to having the hydrate concentration result difference that experiment shows that areal is calculated by different models.
Summary of the invention
To solve the above-mentioned problems, the present invention provides gas hydrates synthesis and decomposition experiment method and experimental system,
Can not only to the full extent synthesis of natural gas hydrate, real-time monitoring gas hydrates synthesis and decomposable process, moreover it is possible to
Gas hydrates saturation degree is accurately calculated by simple physical method with decomposable process in gas hydrates synthesis.
To achieve the above object, the present invention is as follows using scheme:
A kind of synthesis of gas hydrates and decomposition experiment method, comprising the following steps:
(1) to entrance criterion volume building volume V1, export standard volume building volume V2, autoclave and entrance criterion hold
Pipeline dead volume V between product room1s, pipeline dead volume V between autoclave and export standard chamber volume2sIt is demarcated；
(2) sand grains is filled up into autoclave, is successively tamped, and reaction kettle is sealed and checks the leakproofness of reaction kettle；
(3) into reaction kettle, porous media is saturated the simulated seawater solution prepared, measures the hole of porous media in reaction kettle
Porosity and permeability；
(4) natural gas is injected into reaction kettle, reaction kettle outlet valve is opened, by the part in porous media in reaction kettle
Simulated seawater discharge, closes reaction kettle outlet valve, establishes initial p-V-T equilibrium state；
(5) high-pressure natural gas is gradually filled with into autoclave, until being filled with after natural gas pressure in autoclave
When being no longer changed, stopping is filled with natural gas；Period acquires reaction under high pressure temperature in the kettle and pressure；Each gas replenishment process leads to
It crosses P-V-T equilibrium state equation calculation and is filled with gas volume；Finally statistics is filled with gas volume total amount, complete gas hydrates
Synthesis；
(6) gas hydrates to be formed are stablized after a certain period of time, and it is anti-to drive away that simulated seawater is injected into reaction kettle
Free natural gas extra in kettle is answered, the simulated seawater of the measurable natural gas volume and injection being forced out of this process is retained in instead
Answer the volume in kettle；
(7) outlet valve is opened, gas hydrate dissociation is made by export standard chamber volume stage by stage；It is marked by outlet
Quasi- chamber volume measures the natural gas volume that each stage decomposition of hydrate goes out, then measures hydrate point by total tolerance measuring container
The natural gas total volume solved；Whole process acquires reaction under high pressure temperature in the kettle and pressure.
Preferably, using P-V-T equilibrium state equation to entrance criterion volume building volume V1, export standard volume building volume
V2, pipeline dead volume V between autoclave and entrance criterion chamber volume1S, between autoclave and export standard chamber volume
Pipeline dead volume V2SCalibration, managed between orthobaric volume room, export standard chamber volume, autoclave and entrance criterion chamber volume
Pipeline is placed in water at low temperature bath system between line, autoclave and export standard chamber volume, before calibration, opens low temperature water-bath
System, and constant temperature is to experimental temperature；
The entrance criterion chamber volume V1And pipeline dead volume V between autoclave and entrance criterion chamber volume1SMark
It is fixed: it is packed into solid stainless steel module in autoclave, opens the first valve and the second valve, is filled with the gas of certain pressure,
The second valve is closed, the first valve is opened and discharges entrance orthobaric volume indoor gas, record original steady state pressure is PEnter 1, a；
The first valve is closed, the second valve is opened, record steady state pressure is PEnter 1, b；P-V-T equilibrium state equation is established at this time:
The first valve and the second valve are opened, gas in blowdown system is filled with the gas of certain pressure again, closes second
Valve opens the first valve and discharges entrance orthobaric volume indoor gas, and record steady state pressure is PEnter 2, a；It is closed toward orthobaric volume
Indoor loading known volume V2Module, close the first valve, open the second valve, record steady state pressure be PEnter 2, b；At this time
Establish P-V-T equilibrium state equation:
Repeatedly, replacement is packed into the indoor module volume of orthobaric volume for operation repeatedly；It can thus be concluded that multiple temperature constant states
Under P-V-T equilibrium state equation:
Wherein, i=1,2,3 ..., n, and V1=0；ZEnter n, aAnd ZEnter n, bRespectively pressure is PEnter n, aAnd PEnter n, bUnder the conditions of it is natural
The compressibility factor of gas；
Entrance criterion chamber volume V can be calculated by the P-V-T equilibrium state equation under multiple temperature constant states1And reaction under high pressure
Pipeline dead volume V between kettle and entrance criterion chamber volume1S；
Export standard chamber volume V2And pipeline between autoclave and export standard chamber volume
Dead volume V2SCalibration: demarcating steps are same as above；
Wherein, i=1,2,3 ..., n, and V1=0；ZN out, aAnd ZN out, bRespectively pressure is PN out, aAnd PN out, bUnder the conditions of it is natural
The compressibility factor of gas；
Entrance criterion chamber volume V can be calculated by the P-V-T equilibrium state equation under multiple temperature constant states2And reaction under high pressure
Pipeline dead volume V between kettle and entrance criterion chamber volume2S。
Preferably, the specific steps of gas hydrates synthetic method are as follows:
A) sand grains is filled up into autoclave, successively compacting forms pie porous media, ratio of height to diameter 1:6.Sealing
Reaction kettle and the leakproofness for checking reaction kettle；
B) third valve is closed, pumped vacuum systems is connected, autoclave is vacuumized, reaction kettle, pipeline, entrance is discharged
The indoor air of orthobaric volume.Simulated seawater is prepared, saturation is matched in porous media into reaction kettle using seawater metering front pump
Good simulated seawater solution measures the porosity and permeability of porous media in reaction kettle；
C) high-pressure natural gas bottle is connected, the natural gas of 4~10MPa is filled with into reaction kettle；Close the first valve, the second valve
Door opens third valve, drives in reaction kettle saturation simulation seawater in part in porous media out of；In order to form gas hydrates
Natural gas has enough channels to migrate in porous media and comes into full contact with simulated seawater in the process, and the mould in porous media
Quasi- seawater is entirely used for being formed the pore volume that volume after gas hydrates does not exceed porous media, according to experiment and theoretical
It is calculated, at least to drive the simulated seawater solution of porous media pore volume 25% out of, even if the mould in porous media at this time
After quasi- seawater forms gas hydrates generation volume expansion completely, some hole is filled by natural gas in porous media
It fills out；The available precision electronic balance metering for being equipped with calcium chloride jigger of the simulated seawater quality of discharge；According to the simulation of discharge
Seawer quality can calculate pore volume shared by natural gas in pie porous media；Third valve is closed, after stable system,
It can natural gas volume in calculating system according to P-V-T equilibrium state equation；
Remember that pore volume shared by natural gas is Ve in porous media1, temperature T, pressure P1,a, it is known that the pressure strip
Gas deviation factor is Z under part1,a, establish P-V-T equilibrium state equation:
P1,a(Ve1+V1s)=Z1,an1,aRT (5)
Thus the volume Vg of natural gas in normal conditions can be calculatedⅠ:
Wherein P0, T0, Z0 are respectively pressure, temperature and gas deviation factor under standard state；
D) water at low temperature bath system is opened, reduces experimental temperature to 1 DEG C or so and constant temperature；According to temperature and pressure acquisition system it is found that
Reacting kettle inner pressure gradually decreases, and will no longer change after pressure reduction to certain value, and system reaches stable state at this time, and record is anti-
Answering system temperature is T, pressure P1,b；Due to the generation of gas hydrates, the hole originally occupied in porous media by natural gas
Inflated gas hydrates are occupied a part, the pore volume occupied in porous media by natural gas after balance by gap volume
It is denoted as Ve2, it thus can list the P-V-T equilibrium state equation under stable state:
P1,b(Ve2+V1s)=Z1,bn1,bRT (7)
The first valve is opened, the natural gas of certain pressure is filled with to entrance criterion chamber volume, closes the first valve 1；Wait enter
After natural gas is stablized in mouth orthobaric volume room, record natural gas temperature is T, pressure P3；Day in entrance criterion chamber volume at this time
The P-V-T equilibrium state equation of right gas are as follows:
P3V1=Z3n3RT (8)
The second valve is opened, the natural gas in entrance criterion chamber volume is made to be expanded into autoclave, expansion will reach
To Fast-Balance, record whole system temperature is T, pressure P2,a, it can be obtained by isothermal expansion process:
P2,a(Ve2+V1s+ V1)=Z2,a(n1,b+n3)RT (9)
Ve2 is denoted as by the pore volume that formula (9) can derive that natural gas occupies in porous media:
Formula (10) is brought into formula (7), can derive and be remained in system after gas hydrates generation reaches balance
The volume Vg of remaining natural gas in normal conditions2:
Therefore in reaction process natural gas consumption Δ Vg1:
ΔVg1=Vg2-Vg1 (12)
E) the second valve, according to temperature and pressure acquisition system it is found that reacting kettle inner pressure gradually decreases, pressure reduction to one are closed
To no longer it change after definite value, system reaches stable state at this time；The first valve is opened, is filled with a level pressure to entrance criterion chamber volume
The natural gas of power closes the first valve 1；After natural gas in entrance criterion chamber volume is stablized, record natural gas temperature is T, pressure
Power is P3；The second valve is opened, the natural gas in entrance criterion chamber volume is made to be expanded into autoclave, expansion is up to
Fast-Balance；
As same formula (3) to the derivation of formula (9), disappearing for second of gas hydrates generating process natural gas can be calculated
Consumption Δ Vg2:
ΔVg2=Vg3-Vg2 (13)
F) previous step is repeated, after reacting kettle inner pressure no longer changes after being filled with natural gas to reaction system；This
When reaction kettle in water completely formed gas hydrates；And according to each natural-gas consumed calculated in the process
Product, can obtain the natural gas total volume Δ Vg that gas hydrates form post consumption completely:
Δ Vg=Δ Vg1+ΔVg2+ΔVg3+……(14)
G) after gas hydrates balance and stability for a period of time after, connect back pressure system, to back pressure system plus control pressure,
It controls the pressure that pressure must be greater than or equal in autoclave；It connects seawater and measures front pump, mould is injected into reaction kettle
Quasi- sea water solution, opens outlet third valve, and displacement goes out free natural gas extra in autoclave.
Preferably, the specific steps of gas hydrate dissociation are as follows:
A) the second valve of import, outlet third valve and the 4th valve are closed, removes back pressure system or by back pressure system
Control pressure is adjusted to 0；Connection outlet orthobaric volume room, the precision electronic balance for being equipped with calcium chloride jigger and the metering of total tolerance
System.The 4th valve is closed, opens outlet third valve 3, the pressure in autoclave will be gradually decrease to balance at this time；
B) outlet third valve is closed, the 4th valve, the release outlet indoor pressure of orthobaric volume to atmospheric pressure are opened；Again
The 4th valve is closed, outlet third valve is opened, makes the gas hydrates in autoclave continue to decompose, until reaction under high pressure
Pressure reaches balance in kettle；
C) b) step is repeated, until the gas hydrates in autoclave decompose completely；
D) system meters gas hydrate dissociation can be measured by total tolerance in the complete decomposable process of gas hydrates to release
The natural gas total volume put.It is total to measure the natural gas that obtained natural gas total volume can be consumed with gas hydrates generating process
Volume delta Vg compares correction.
Preferably, the calculation method of gas hydrates saturation degree are as follows:
Last time gas replenishment process in gas hydrates synthesis, the natural gas which is filled with no longer is consumed, i.e., on
Simulated seawater in one step in porous media has been totally consumed to form gas hydrates, therefore last time opens second
Valve inflates an only isothermal expansion process into autoclave.Natural gas in porous media at this time can be calculated by formula
Occupied pore volume Ve, it is known that the pore volume of porous media is VΦ, gas hydrates volume V=can be calculated
VΦThus-Ve can calculate gas hydrates saturation degree.
A kind of synthesis of gas hydrates and decomposition experiment system, including water at low temperature bath system, autoclave, entrance mark
Quasi- chamber volume, export standard chamber volume, total tolerance measuring container, pumped vacuum systems, pure methane high pressure gas cylinder, seawater metering input
Pump, back pressure system and temperature and pressure acquire system, and wherein orthobaric volume room in entry and exit is provided with normal volume module, for calibrating,
Entrance criterion volume building volume, and its pipeline dead volume between reaction kettle.
Compared with prior art, the invention has the following advantages that
1, the entrance criterion chamber volume that includes in a kind of provided gas hydrates synthesis and decomposition experiment system and
Export standard chamber volume can optimize the synthesis and decomposition of gas hydrates.The use of its entrance criterion chamber volume not only can be with
For giving the porous media in autoclave to supply natural gas stage by stage, moreover it can be used to accurately calculate gas hydrates synthesis
The consumption of natural gas in the process.The use of export standard chamber volume can not only make the decomposition of gas hydrates stage by stage into
Row, solves the problems, such as that temperature decrease leads to pipeline ice blockage when gas hydrate dissociation in common decomposition method, moreover it is possible to
For measuring the amount of natural gas of gas hydrate dissociation process release.
2, the generation of gas hydrates can make to be saturated in porous media using the method for sustainable supply natural gas stage by stage
Simulated seawater generate gas hydrates completely.
3, in the prior art, the metering conventional means of the consumption of gas hydrates synthesis process natural gas is to react
Kettle imports and exports installation quality flowmeter, and the synthesis of gas hydrates is an extremely slow process, around here mass flow
It is very difficult to collect flows for meter, therefore this method is difficult accurately to measure the consumption of natural gas.The present invention uses entrance criterion volume
The method of room establishes P-V-T equilibrium state equation, can accurately calculate the consumption of natural gas in gas hydrates synthesis process
Amount.
4, gas hydrates synthesis provided by the invention and decomposition experiment method, during gas hydrate dissociation
Gradually make its decomposition stage by stage using with export standard chamber volume, and using the day discharged in the metering decomposition of total tolerance measuring container
Right gas total amount can compare the gas consumption calculated in correction synthesis process.
Detailed description of the invention
Fig. 1 is gas hydrates of the present invention synthesis and decomposition experiment schematic diagram
Fig. 2 is experimental system schematic diagram of the present invention
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, the technical solution below in the present invention carries out clear
Chu is fully described by, it is clear that described embodiments are some of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Its specific implementation method is as follows with decomposition experiment method for a kind of gas hydrates synthesis:
(1) to entrance criterion volume building volume V1, export standard volume building volume V2, autoclave and entrance criterion hold
Pipeline dead volume V between product room1S, pipeline dead volume V between autoclave and export standard chamber volume2SCalibration use P-
V-T equilibrium state equation, as shown in Figure 1.Orthobaric volume room, export standard chamber volume, autoclave and entrance criterion volume
Pipeline is placed in water at low temperature bath system between pipeline, autoclave and export standard chamber volume between room, before calibration, is opened
Water at low temperature bath system, and constant temperature is to experimental temperature.
Entrance criterion chamber volume V1And pipeline dead volume V between autoclave and entrance criterion chamber volume1SCalibration: it is high
It presses and is packed into solid stainless steel module in reaction kettle, open the first valve 1 and the first valve 2, be filled with the gas of certain pressure, close
First valve 2 opens the first valve 1 and discharges entrance orthobaric volume indoor gas, and record original steady state pressure is PEnter 1, a；It closes
The first valve 1 is closed, the first valve 2 is opened, record steady state pressure is PEnter 1, b.P-V-T equilibrium state equation is established at this time:
Open the first valve 1 and the first valve 2, gas in blowdown system is filled with the gas of certain pressure again, closes the
One valve 2 opens the first valve 1 and discharges entrance orthobaric volume indoor gas, and record steady state pressure is PEnter 2, a；Hold toward standard
Known volume V is packed into product closed chamber2Module, close the first valve 1, open the first valve 2, record steady state pressure be
PEnter 2, b.P-V-T equilibrium state equation is established at this time:
Repeatedly, replacement is packed into the indoor module volume of orthobaric volume for operation repeatedly.
It can thus be concluded that the P-V-T equilibrium state equation under multiple temperature constant states:
Wherein, i=1,2,3 ..., n, and V1=0；ZEnter n, aAnd ZEnter n, bRespectively pressure is PEnter n, aAnd PEnter n, bUnder the conditions of it is natural
The compressibility factor of gas；
Entrance criterion chamber volume V can be calculated by the P-V-T equilibrium state equation under multiple temperature constant states1And reaction under high pressure
Pipeline dead volume V between kettle and entrance criterion chamber volume1S。
Export standard chamber volume V2And pipeline dead volume V between autoclave and export standard chamber volume2SCalibration: mark
Determine step to be same as above.
Wherein, i=1,2,3 ..., n, and V1=0；ZN out, aAnd ZN out, bRespectively pressure is PN out, aAnd PN out, bUnder the conditions of it is natural
The compressibility factor of gas；
Entrance criterion chamber volume V can be calculated by the P-V-T equilibrium state equation under multiple temperature constant states2And reaction under high pressure
Pipeline dead volume V between kettle and entrance criterion chamber volume2S。
(2) experimental system principle is as shown in Figure 2.The specific steps of gas hydrates synthesis are as follows:
A) sand grains is filled up into autoclave, successively compacting forms pie porous media, ratio of height to diameter 1:6.Sealing
Reaction kettle and the leakproofness for checking reaction kettle.
B) third valve 3 is closed, pumped vacuum systems is connected, autoclave is vacuumized, discharge reaction kettle, enters pipeline
The mouth indoor air of orthobaric volume.Simulated seawater is prepared, is saturated in porous media using seawater metering front pump into reaction kettle
The simulated seawater solution prepared measures the porosity and permeability of porous media in reaction kettle.
C) high-pressure natural gas bottle is connected, the 5th valve 5 is opened, the day of certain pressure (4~10MPa) is filled with into reaction kettle
Right gas.It closes the first valve 1, the first valve 2, opens third valve 3, drive in reaction kettle part saturation simulation in porous media out of
Seawater.In order to make in natural gas hydrate formation natural gas have in porous media enough channels migrate and with simulation sea
Water comes into full contact with, and the simulated seawater in porous media is entirely used for volume after forming gas hydrates and does not exceed porous Jie
The pore volume of matter, obtains according to experimental and theoretical computation, at least to drive the simulated seawater of porous media pore volume 25% out of
Solution, even if after the simulated seawater in porous media forms gas hydrates generation volume expansion completely at this time, porous media
In some hole filled by natural gas.The available precision electricity for being equipped with calcium chloride jigger of the simulated seawater quality of discharge
Sub- balance metering；According to the simulated seawater quality of discharge, pore volume shared by natural gas in pie porous media can be calculated；It closes
Third valve 3 is closed, it, can natural gas volume in calculating system according to P-V-T equilibrium state equation after stable system.
D) remember that pore volume shared by natural gas is Ve in porous media1, temperature T, pressure P1,a, it is known that the pressure
Under the conditions of gas deviation factor be Z1,a.Establish P-V-T equilibrium state equation:
P1,a(Ve1+V1s)=Z1,an1,aRT (5)
Thus the volume Vg of natural gas in normal conditions can be calculatedⅠ:
Wherein P0, T0, Z0 are respectively pressure, temperature and gas deviation factor under standard state.
E) water at low temperature bath system is opened, reduces experimental temperature to 1 DEG C or so and constant temperature.According to temperature and pressure acquisition system it is found that
Reacting kettle inner pressure gradually decreases, and will no longer change after pressure reduction to certain value, and system reaches stable state at this time, and record is anti-
Answering system temperature is T, pressure P1,b.Due to the generation of gas hydrates, the hole originally occupied in porous media by natural gas
Inflated gas hydrates are occupied a part, the pore volume occupied in porous media by natural gas after balance by gap volume
It is denoted as Ve2, it thus can list the P-V-T equilibrium state equation under stable state:
P1,b(Ve2+V1s)=Z1,bn1,bRT (7)
The first valve 1 is opened, the natural gas of certain pressure is filled with to entrance criterion chamber volume, closes the first valve 1.Wait enter
After natural gas is stablized in mouth orthobaric volume room, record natural gas temperature is T, pressure P3.Day in entrance criterion chamber volume at this time
The P-V-T equilibrium state equation of right gas are as follows:
P3V1=Z3n3RT (8)
The first valve 2 is opened, the natural gas in entrance criterion chamber volume is made to be expanded into autoclave, expansion will reach
To Fast-Balance, record whole system temperature is T, pressure P2,a, it can be obtained by isothermal expansion process:
P2,a(Ve2+V1s+ V1)=Z2,a(n1,b+n3)RT (9)
Ve is denoted as by the pore volume that formula (9) can derive that natural gas occupies in porous media2:
Formula (10) is brought into formula (7), can derive and be remained in system after gas hydrates generation reaches balance
The volume Vg of remaining natural gas in normal conditions2:
Therefore in reaction process natural gas consumption Δ Vg1:
ΔVg1=Vg2-Vg1 (12)
F) the first valve 2 is closed, according to temperature and pressure acquisition system it is found that reacting kettle inner pressure gradually decreases, pressure reduction is arrived
To no longer it change after certain value, system reaches stable state at this time.The first valve 1 is opened, is filled with one to entrance criterion chamber volume
The natural gas of constant-pressure closes the first valve 1.After natural gas in entrance criterion chamber volume is stablized, record natural gas temperature is
T, pressure P3.The first valve 2 is opened, the natural gas in entrance criterion chamber volume is made to be expanded into autoclave, is expanded
It is up to Fast-Balance.
G) as same formula (3) to the derivation of formula (9), second of gas hydrates generating process natural gas can be calculated
Consumption Δ Vg2:
ΔVg2=Vg3-Vg2 (13)
H) previous step is repeated, after reacting kettle inner pressure no longer changes after being filled with natural gas to reaction system.This
When reaction kettle in water completely formed gas hydrates.And according to each natural-gas consumed calculated in the process
Product, can obtain the natural gas total volume Δ Vg that gas hydrates form post consumption completely:
Δ Vg=Δ Vg1+ΔVg2+ΔVg3+……(14)
I) after gas hydrates balance and stability for a period of time after, connect back pressure system, to back pressure system plus control pressure,
It controls the pressure that pressure must be greater than or equal in autoclave.It connects seawater and measures front pump, mould is injected into reaction kettle
Quasi- sea water solution, opens outlet third valve 3, and displacement goes out free natural gas extra in autoclave.
(3) specific steps of gas hydrate dissociation are as follows:
A) the first valve of import 2, outlet third valve 3 and the 4th valve 4 are closed, removes back pressure system or by back pressure system
System control pressure is adjusted to 0.Connection outlet orthobaric volume room, the precision electronic balance for being equipped with calcium chloride jigger and total gas gauge
Amount system.The 4th valve 4 is closed, opens outlet third valve 3, the pressure in autoclave will be gradually decrease to put down at this time
Weighing apparatus.
B) outlet third valve 3 is closed, the 4th valve 4, the release outlet indoor pressure of orthobaric volume to atmospheric pressure are opened.
The 4th valve 4 is turned off, outlet third valve 3 is opened, makes the gas hydrates in autoclave continue to decompose, until high pressure
Reacting kettle inner pressure reaches balance.
C) b) step is repeated, until the gas hydrates in autoclave decompose completely.Gas hydrates divide completely
The natural gas total volume of system meters gas hydrate dissociation release can be measured in solution preocess by total tolerance.Measure obtained day
The natural gas total volume Δ Vg that right gas total volume can be consumed with gas hydrates generating process compares correction.
(4) calculating of gas hydrates saturation degree
Last time gas replenishment process in gas hydrates synthesis, the natural gas which is filled with no longer is consumed, i.e., on
Simulated seawater in one step in porous media has been totally consumed to form gas hydrates, therefore last time opens second
Valve 2 inflates an only isothermal expansion process into autoclave.Day in porous media at this time can be calculated by formula (8)
Pore volume Ve occupied by right gas, it is known that the pore volume of porous media is VΦ, gas hydrates volume V can be calculated
=VΦThus-Ve can calculate gas hydrates saturation degree.
A kind of synthesis of gas hydrates and decomposition experiment system, including water at low temperature bath system, autoclave, entrance mark
Quasi- chamber volume, export standard chamber volume, total tolerance measuring container, pumped vacuum systems, pure methane high pressure gas cylinder, seawater metering input
Pump, back pressure system and temperature and pressure acquire system, and wherein orthobaric volume room in entry and exit is provided with normal volume module, for calibrating,
Entrance criterion volume building volume, and its pipeline dead volume between reaction kettle.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
Present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: it still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features；
And these are modified or replaceed, technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution spirit and
Range.
Claims (5)
1. a kind of gas hydrates synthesis and decomposition experiment method, which comprises the following steps:
(1) to entrance criterion volume building volume V1, export standard volume building volume V2, autoclave and entrance criterion chamber volume
Between pipeline dead volume V1s, pipeline dead volume V between autoclave and export standard chamber volume2sIt is demarcated；
(2) sand grains is filled up into autoclave, is successively tamped, and reaction kettle is sealed and checks the leakproofness of reaction kettle；
(3) into reaction kettle, porous media is saturated the simulated seawater solution prepared, measures the porosity of porous media in reaction kettle
And permeability；
(4) natural gas is injected into reaction kettle, reaction kettle outlet valve is opened, by the partial simulation in porous media in reaction kettle
Seawater discharge, closes reaction kettle outlet valve, establishes initial p-V-T equilibrium state；
(5) high-pressure natural gas is gradually filled with into autoclave, until being filled with after natural gas in autoclave pressure no longer
When changing, stopping is filled with natural gas；Period acquires reaction under high pressure temperature in the kettle and pressure；Each gas replenishment process, passes through P-
V-T equilibrium state equation calculation is filled with gas volume；Finally statistics is filled with gas volume total amount, completes gas hydrates and closes
At；
(6) gas hydrates to be formed are stablized after a certain period of time, inject simulated seawater into reaction kettle to drive reaction kettle away
The simulated seawater of interior extra free natural gas, the measurable natural gas volume and injection being forced out of this process is retained in reaction kettle
Interior volume；
(7) outlet valve is opened, gas hydrate dissociation is made by export standard chamber volume stage by stage；Held by export standard
The natural gas volume that each stage decomposition of hydrate goes out is measured in product room, then measures decomposition of hydrate by total tolerance measuring container and go out
Natural gas total volume；Whole process acquires reaction under high pressure temperature in the kettle and pressure.
2. gas hydrates synthesis according to claim 1 and decomposition experiment method, it is characterised in that: use P-V-T
Equilibrium state equation is to entrance criterion volume building volume V1, export standard volume building volume V2, autoclave and entrance criterion hold
Pipeline dead volume V between product room1S, pipeline dead volume V between autoclave and export standard chamber volume2SCalibration, standard hold
Pipeline, autoclave and export standard are held between product room, entrance criterion chamber volume, autoclave and entrance criterion chamber volume
Pipeline is placed in water at low temperature bath system between product room, before calibration, opens water at low temperature bath system, and constant temperature is to experimental temperature；
The entrance criterion chamber volume V1And pipeline dead volume V between autoclave and entrance criterion chamber volume1SCalibration: it is high
It presses and is packed into solid stainless steel module in reaction kettle, open the first valve (1) and the second valve (2), be filled with the gas of certain pressure,
It closes the second valve (2), opens the first valve (1) and discharge entrance orthobaric volume indoor gas, record original steady state pressure
For PEnter 1, a；It closes the first valve (1), opens the second valve (2), record steady state pressure is PEnter 1, b；It is flat that P-V-T is established at this time
Weigh state equation:
Open the first valve (1) and the second valve (2), gas in blowdown system is filled with the gas of certain pressure again, closes the
Two valves (2) open the first valve (1) and discharge entrance orthobaric volume indoor gas, and record steady state pressure is PEnter 2, a；Toward mark
Known volume V is packed into quasi- volume closed chamber2Module, close the first valve (1), open the second valve (2), record stable state pressure
Power is PEnter 2, b；P-V-T equilibrium state equation is established at this time:
Repeatedly, replacement is packed into the indoor module volume of orthobaric volume for operation repeatedly；It can thus be concluded that under multiple temperature constant states
P-V-T equilibrium state equation:
Wherein, n=1,2,3 ..., N, and V1=0；ZEnter n, aAnd ZEnter n, bRespectively pressure is PEnter n, aAnd PEnter n, bUnder the conditions of natural gas
Compressibility factor；
Entrance criterion chamber volume V can be calculated by the P-V-T equilibrium state equation under multiple temperature constant states1And autoclave with
Pipeline dead volume V between entrance criterion chamber volume1S；
Export standard chamber volume V2And pipeline dead volume V between autoclave and export standard chamber volume2SCalibration: calibration step
It is rapid to be same as above；
Wherein, i=1,2,3 ..., n, and V1=0；ZN out, aAnd ZN out, bRespectively pressure is PN out, aAnd PN out, bUnder the conditions of natural gas
Compressibility factor；
Entrance criterion chamber volume V can be calculated by the P-V-T equilibrium state equation under multiple temperature constant states2And autoclave with
Pipeline dead volume V between entrance criterion chamber volume2S。
3. gas hydrates synthesis according to claim 1 and decomposition experiment method, which is characterized in that natural gas hydration
The specific steps of object synthetic method are as follows:
A) sand grains is filled up into autoclave, successively compacting forms pie porous media, ratio of height to diameter 1:6；Sealing reaction
Kettle and the leakproofness for checking reaction kettle；
B) third valve (3) are closed, connects pumped vacuum systems, autoclave is vacuumized, reaction kettle, pipeline, entrance is discharged
The indoor air of orthobaric volume；Simulated seawater is prepared, saturation is matched in porous media into reaction kettle using seawater metering front pump
Good simulated seawater solution measures the porosity and permeability of porous media in reaction kettle；
C) high-pressure natural gas bottle is connected, the natural gas of 4~10MPa is filled with into reaction kettle；Close the first valve (1), the second valve
Door (2) is opened third valve (3), drives in reaction kettle saturation simulation seawater in part in porous media out of；In order to be hydrated natural gas
Natural gas has enough channels to migrate in porous media and comes into full contact with simulated seawater in object forming process, and porous media
In simulated seawater be entirely used for being formed the pore volume that volume after gas hydrates does not exceed porous media, according to experiment
It is obtained with theoretical calculation, at least to drive the simulated seawater solution of porous media pore volume 25% out of, even if porous media at this time
In simulated seawater formed completely gas hydrates occur volume expansion after, in porous media some hole be natural gas
It is filled；The precision electronic balance metering for being equipped with calcium chloride jigger of the simulated seawater quality of discharge；According to the mould of discharge
Quasi- seawer quality, can calculate pore volume shared by natural gas in pie porous media；It closes third valve (3), it is steady to system
It, can natural gas volume in calculating system according to P-V-T equilibrium state equation after fixed；
Remember that pore volume shared by natural gas is V in porous mediae1, temperature T, pressure P1,a, it is known that day under the pressure condition
Right gas compressibility factor is Z1,a, establish P-V-T equilibrium state equation:
P1,a(Ve1+V1s)=Z1,an1,aRT (5)
In above formula, n1,aRepresent the molal weight of gas in porous media, mol；
Thus the volume Vg of natural gas in normal conditions can be calculatedⅠ:
Wherein P0, T0, Z0Pressure, temperature and gas deviation factor respectively under standard state；
D) water at low temperature bath system is opened, reduces experimental temperature to 1 DEG C or so and constant temperature；According to temperature and pressure acquisition system it is found that reaction
Pressure gradually decreases in kettle, will no longer change after pressure reduction to certain value, and system reaches stable state at this time, records reactant
Be temperature be T, pressure P1,b；Due to the generation of gas hydrates, the pore-body originally occupied in porous media by natural gas
Inflated gas hydrates are occupied a part by product, are denoted as in porous media by the pore volume that natural gas occupies after balance
Ve2, it thus can list the P-V-T equilibrium state equation under stable state:
P1,b(Ve2+V1s)=Z1,bn1,bRT (7)
In above formula, n1,bRepresent the molal weight of gas in reaction kettle body, mol；
The first valve (1) is opened, the natural gas of certain pressure is filled with to entrance criterion chamber volume, is closed the first valve (1)；Wait enter
After natural gas is stablized in mouth orthobaric volume room, record natural gas temperature is T, pressure P3；Day in entrance criterion chamber volume at this time
The P-V-T equilibrium state equation of right gas are as follows:
P3V1=Z3n3RT (8)
In above formula, n3Represent the molal weight of entrance criterion volume indoor gas, mol；
The second valve (2) are opened, the natural gas in entrance criterion chamber volume is made to be expanded into autoclave, expansion is up to
Fast-Balance, record whole system temperature are T, pressure P2,a, it can be obtained by isothermal expansion process:
P2,a(Ve2+V1s+V1)=Z2,a(n1,b+n3)RT (9)
In above formula, n1,b、n3Respectively represent mole matter of the molal weight of gas in reaction kettle body, entrance criterion volume indoor gas
Amount, mol；
Ve is denoted as by the pore volume that formula (9) can derive that natural gas occupies in porous media2:
Formula (10) is brought into formula (7), can derive after gas hydrates generation reaches balance remaining day in system
The volume Vg of right gas in normal conditions2:
Therefore in reaction process natural gas consumption Δ Vg1:
ΔVg1=Vg2-Vg1 (12)
E) the second valve (2) are closed, according to temperature and pressure acquisition system it is found that reacting kettle inner pressure gradually decreases, pressure reduction to one
To no longer it change after definite value, system reaches stable state at this time；The first valve (1) is opened, is filled with one to entrance criterion chamber volume
The natural gas of constant-pressure is closed the first valve (1)；After natural gas in entrance criterion chamber volume is stablized, natural gas temperature is recorded
For T, pressure P3；The second valve (2) are opened, the natural gas in entrance criterion chamber volume is made to be expanded into autoclave,
Expansion is up to Fast-Balance；
As same formula (3) to the derivation of formula (9), the consumption of second of gas hydrates generating process natural gas can be calculated
ΔVg2:
ΔVg2=Vg3-Vg2 (13)
F) previous step is repeated, after reacting kettle inner pressure no longer changes after being filled with natural gas to reaction system；It is anti-at this time
The water in kettle is answered to form gas hydrates completely；It, can and according to each natural gas volume consumed calculated in the process
Obtain the natural gas total volume Δ Vg that gas hydrates form post consumption completely:
Δ Vg=Δ Vg1+ΔVg2+ΔVg3+…… (14)
G) after gas hydrates balance and stability for a period of time after, connect back pressure system, to back pressure system plus control pressure, control
Pressing pressure must be greater than or equal to the pressure in autoclave；It connects seawater and measures front pump, the injection simulation sea into reaction kettle
Aqueous solution, opens outlet third valve (3), and displacement goes out free natural gas extra in autoclave.
4. gas hydrates synthesis according to claim 3 and decomposition experiment method, which is characterized in that natural gas hydration
The specific steps that object decomposes are as follows:
A) the second valve of import (2), outlet third valve (3) and the 4th valve (4) are closed, dismounting back pressure system or by back pressure
System control pressure is adjusted to 0；Connection outlet orthobaric volume room, the precision electronic balance and total tolerance for being equipped with calcium chloride jigger
Metering system；The 4th valve (4) is closed, opens outlet third valve (3), the pressure in autoclave will be gradually reduced at this time
To balance；
B) outlet third valve (3) is closed, the 4th valve (4), the release outlet indoor pressure of orthobaric volume to atmospheric pressure are opened；
The 4th valve (4) is turned off, outlet third valve (3) is opened, the gas hydrates in autoclave is made to continue to decompose, until
Pressure reaches balance in autoclave；
C) b) step is repeated, until the gas hydrates in autoclave decompose completely；
D) release of system meters gas hydrate dissociation can be measured in the complete decomposable process of gas hydrates by total tolerance
Natural gas total volume；Measure the natural gas total volume that obtained natural gas total volume can be consumed with gas hydrates generating process
Δ Vg compares correction.
5. gas hydrates synthesis according to claim 3 and decomposition experiment method, which is characterized in that natural gas hydration
The calculation method of object saturation degree are as follows:
Last time gas replenishment process in gas hydrates synthesis, the natural gas which is filled with no longer are consumed, i.e. previous step
Simulated seawater in rapid in porous media has been totally consumed to form gas hydrates, therefore last time opens the second valve
(2) into autoclave, inflation is only an isothermal expansion process；It can be calculated by formula (8) natural in porous media at this time
Pore volume Ve occupied by gas, it is known that the pore volume of porous media is VΦ, gas hydrates volume V=can be calculated
VΦThus-Ve can calculate gas hydrates saturation degree.
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