CN105699247A - Experimental method for synthesizing and decomposing natural gas hydrate and experiment system - Google Patents
Experimental method for synthesizing and decomposing natural gas hydrate and experiment system Download PDFInfo
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Abstract
The invention provides an experimental method for synthesizing and decomposing natural gas hydrate and an experiment system. An inlet standard volume chamber and an outlet standard volume chamber are included and can optimize synthesis and decomposition of the natural gas hydrate, the inlet standard volume chamber can be used for supplying natural gas to a porous medium in a high-pressure reaction kettle in stages and accurately calculating the consumption of the natural gas in the synthesizing process of the natural gas hydrate, and the outlet standard volume chamber is used for enabling the natural gas hydrate to be decomposed in stages, solving the problem that a pipeline is frozen and blocked as temperature drops abruptly when the natural gas hydrate is decomposed in a common decomposition method and metering the amount of natural gas released in the decomposing process of the natural gas hydrate.
Description
Technical field
The invention belongs to gas hydrates experiment field, particularly to a kind of gas hydrates synthesis and decomposition experiment method and experimental system。
Background technology
Gas hydrates as a kind of cleaning, efficiently and the novel potential energy source of rich reserves, shown great attention to by many countries and carry out primary study。Since the nineties in 20th century, what gas hydrates recognizes by the increasing of the Gas Hydrate found along with countries in the world with people deepens further, and the research of gas hydrates worldwide expands rapidly。Its research emphasis has also turned to the practical development phase, this stage, and gas hydrate study is method or the degree of depth is all a a progressive step。In the basic research of gas hydrates, achieve bigger progress over nearly 20 years, relate to the physicochemical characteristics of gas hydrates, form aspects such as decomposing thermodynamics and kinetics, output condition, the regularity of distribution, formation mechenism, exploration engineering and environmental effect。And prior art carries out hydrate sediment scene and cores still not mature enough, therefore the basic research of gas hydrates is prepared simulating hydrate deposit mainly by laboratory test and is realized by scholars。
In the prior art, the experiment synthesis of gas hydrates mainly has two kinds of methods with decomposing, one is carry out in aqueous, two is carry out in porous media, and in porous media, carry out the synthesis of gas hydrates and the decomposition experiment research situation closer to actual hydrate mineral reserve, it is possible to for the exploitation offer reliable basis of gas hydrates from now on。In the synthesis of the gas hydrates announced and decomposition experiment method and technology patent, the method that the detection of gas hydrates saturation in deposit is calculated has electrical method, supersonic detection method and time domain reflection technology etc., but the design of these method of testings is complicated, relatively costly, can not calculate gas hydrates saturation accurately。Wherein electric-resistivity method is based on the change of effects of ion content and causes conductivity to change, and methane is difficult to ionization in aqueous, and ion changes very little, therefore, it is difficult to measure。Supersonic detection method and time domain reflection technology must be set up on known calculations model accurately, gas hydrates saturation could be calculated, and at present relation about hydrate concentration with the velocity of sound and dielectric constant has some models, one class is simple empirical equation, and this class model lacks tight theoretical foundation；Another kind of for being based upon theory on complicated physical model and equation etc., these model theories are derived tight, but the parameter relating to calculating is more, and are difficult to determine the value of each parameter under practical situation。It addition, experiments show that according to existing, the hydrate concentration result difference that areal is calculated by different models is very big。
Summary of the invention
In order to solve the problems referred to above, the present invention provides gas hydrates synthesis and decomposition experiment method and experimental system, can not only synthesis of natural gas hydrate, in real time monitoring gas hydrates synthesize and catabolic process to the full extent, moreover it is possible in gas hydrates synthesis with catabolic process, accurately calculate gas hydrates saturation by simple physical method。
For achieving the above object, the present invention adopts scheme as follows:
A kind of gas hydrates synthesis and decomposition experiment method, comprise the following steps:
(1) to entrance criterion chamber volume volume V1, export standard chamber volume volume V2, pipeline dead volume V between autoclave and entrance criterion chamber volume1s, pipeline dead volume V between autoclave and export standard chamber volume2sDemarcate；
(2) filling up sand grains in autoclave, successively tamp, sealed reactor also checks the sealing of reactor；
(3) to the saturated simulated seawater solution prepared of porous media in reactor, the porosity of porous media and permeability in assaying reaction still；
(4) in reactor, inject natural gas, open reactor outlet valve, the partial simulation sea water in porous media in reactor is discharged, close reactor outlet valve, set up initial p-V-T poised state；
(5) in autoclave, high-pressure natural gas gradually it is filled with, until when pressure no longer changes in autoclave after being filled with natural gas, stopping being filled with natural gas；Period, gather reaction under high pressure temperature in the kettle and pressure；Each gas replenishment process, by P-V-T poised state Equation for Calculating insufflation gas volume；Finally statistics insufflation gas volume total amount, complete gas hydrates synthesize；
(6) after gas hydrates to be formed stablize certain time, simulated seawater is injected to drive free natural gas unnecessary in reactor away, the volume that the simulated seawater of the measurable natural gas volume being forced out of this process and injection is retained in reactor in reactor；
(7) open outlet valve, make gas hydrate dissociation stage by stage by export standard chamber volume；Measure, by export standard chamber volume, the natural gas volume that each stage decomposition of hydrate goes out, measure, again through total tolerance measuring container, the natural gas cumulative volume that decomposition of hydrate goes out；Whole process gathers reaction under high pressure temperature in the kettle and pressure。
Preferably, adopt P-V-T poised state equation to entrance criterion chamber volume volume V1, export standard chamber volume volume V2, pipeline dead volume V between autoclave and entrance criterion chamber volume1S, pipeline dead volume V between autoclave and export standard chamber volume2SDemarcation, between orthobaric volume room, export standard chamber volume, autoclave and entrance criterion chamber volume, between pipeline, autoclave and export standard chamber volume, pipeline is placed in water at low temperature bath system, before demarcation, open water at low temperature bath system, and constant temperature is to experimental temperature；
Described entrance criterion chamber volume V1And pipeline dead volume V between autoclave and entrance criterion chamber volume1SDemarcation: loading solid rustless steel module in autoclave, open the first valve and the second valve, be filled with the gas of certain pressure, close the second valve, open the first valve release entrance orthobaric volume indoor gas, record original steady state pressure is PEnter 1, a；Closing the first valve, open the second valve, record steady state pressure is PEnter 1, b；Now set up P-V-T poised state equation:
Opening the first valve and the second valve, gas in blowdown system, be again filled with the gas of certain pressure, close the second valve, open the first valve release entrance orthobaric volume indoor gas, record steady state pressure is PEnter 2, a；Known volume V is loaded in orthobaric volume closed chamber2Module, close the first valve, open the second valve, record steady state pressure is PEnter 2, b；Now set up P-V-T poised state equation:
Such repeatable operation repeatedly, is changed and is loaded the module volume that orthobaric volume is indoor；Thus can obtain the P-V-T poised state equation under multiple temperature constant state:
Wherein, i=1,2,3 ..., n, and V1=0；ZEnter n, aAnd ZEnter n, bRespectively pressure is PEnter n, aAnd PEnter n, bThe compressibility factor of natural gas under condition；
Entrance criterion chamber volume V can be calculated by the P-V-T poised state equation under multiple temperature constant states1And pipeline dead volume V between autoclave and entrance criterion chamber volume1S；
Export standard chamber volume V2And pipeline between autoclave and export standard chamber volume
Dead volume V2SDemarcation: demarcating steps is ibid；
Wherein, i=1,2,3 ..., n, and V1=0；ZGo out n, aAnd ZGo out n, bRespectively pressure is PGo out n, aAnd PGo out n, bThe compressibility factor of natural gas under condition；
Entrance criterion chamber volume V can be calculated by the P-V-T poised state equation under multiple temperature constant states2And pipeline dead volume V between autoclave and entrance criterion chamber volume2S。
Preferably, the concretely comprising the following steps of gas hydrates synthetic method:
A) filling up sand grains in autoclave, successively compacting forms pie porous media, and its ratio of height to diameter is 1:6。Sealed reactor also checks the sealing of reactor；
B) close the 3rd valve, connect pumped vacuum systems, to autoclave evacuation, discharge the air in reactor, pipeline, entrance criterion chamber volume。Preparation simulated seawater, uses sea water metering front pump to the simulated seawater solution prepared saturated in porous media in reactor, the porosity of porous media and permeability in assaying reaction still；
C) connect high-pressure natural gas bottle, in reactor, be filled with the natural gas of 4～10MPa；Close the first valve, the second valve, open the 3rd valve, drive in reactor part saturation simulation sea water in porous media out of；In order to make natural gas in natural gas hydrate formation have enough passage migrations in porous media and be fully contacted with simulated seawater, and the simulated seawater in porous media is entirely used for being formed after gas hydrates volume not over the pore volume of porous media, obtain according to experimental and theoretical computation, at least to drive the simulated seawater solution of porous media pore volume 25% out of, even if after the simulated seawater full form now in porous media becomes gas hydrates generation volumetric expansion, in porous media, some hole is the filling of natural gas institute；The simulated seawater quality discharged can be measured by the precision electronic balance being provided with calcium chloride jigger；According to the simulated seawater quality discharged, the pore volume shared by natural gas in pie porous media can be calculated；Close the 3rd valve, after stable system, the natural gas volume in system can be calculated according to P-V-T poised state equation；
In note porous media, the pore volume shared by natural gas is Ve1, temperature is T, and pressure is P1,a, it is known that under this pressure condition, gas deviation factor is Z1,a, set up P-V-T poised state equation:
P1,a(Ve1+V1s)=Z1,an1,aRT(5)
Thus can calculate natural gas volume Vg in normal conditionsⅠ:
Wherein P0, T0, Z0 respectively mark the pressure under state, temperature and gas deviation factor；
D) open water at low temperature bath system, reduce experimental temperature to about 1 DEG C and constant temperature；According to temperature and pressure acquisition system it can be seen that reacting kettle inner pressure is gradually lowered, pressure will no longer change after being reduced to certain value, and now system reaches steady statue, and record temperature of reaction system is T, and pressure is P1,b；Due to the generation of gas hydrates, inflated gas hydrates are occupied a part by the pore volume originally occupied by natural gas in porous media, and the pore volume occupied by natural gas in porous media after balance is designated as Ve2, thus can list the P-V-T poised state equation under steady statue:
P1,b(Ve2+V1s)=Z1,bn1,bRT(7)
Open the first valve, be filled with the natural gas of certain pressure to entrance criterion chamber volume, close the first valve 1；After natural gas in entrance criterion chamber volume is stable, record natural gas temperature is T, and pressure is P3；Now in entrance criterion chamber volume, the P-V-T poised state equation of natural gas is:
P3V1=Z3n3RT(8)
Opening the second valve, make the natural gas in entrance criterion chamber volume be expanded into autoclave, its expansion is up to Fast-Balance, and recording whole system temperature is T, and pressure is P2,a, isothermal expansion process can obtain:
P2,a(Ve2+V1s+ V1)=Z2,a(n1,b+n3)RT(9)
Can be derived, by formula (9), the pore volume that in porous media, natural gas occupies and be designated as Ve2:
Formula (10) is brought in formula (7), can derive and remain natural gas volume Vg in normal conditions in system after a gas hydrates generation reaches balance2:
Therefore the consumption Δ Vg of natural gas in course of reaction1:
ΔVg1=Vg2-Vg1(12)
E) closing the second valve, according to temperature and pressure acquisition system it can be seen that reacting kettle inner pressure is gradually lowered, pressure will no longer change after being reduced to certain value, and now system reaches steady statue；Open the first valve, be filled with the natural gas of certain pressure to entrance criterion chamber volume, close the first valve 1；After natural gas in entrance criterion chamber volume is stable, record natural gas temperature is T, and pressure is P3；Opening the second valve, make the natural gas in entrance criterion chamber volume be expanded into autoclave, its expansion is up to Fast-Balance；
Cotype (3) is the same to the derivation of formula (9), can calculate second time gas hydrates and generate the consumption Δ Vg of process natural gas2:
ΔVg2=Vg3-Vg2(13)
F) previous step is repeated, until after after being filled with natural gas to reaction system, reacting kettle inner pressure no longer changes；Now the full form of the water in reactor becomes gas hydrates；And according to the natural gas volume consumed calculated in each process, gas hydrates can be obtained and form the natural gas cumulative volume Δ Vg of post consumption completely:
Δ Vg=Δ Vg1+ΔVg2+ΔVg3+……(14)
G) after gas hydrates balance and stability a period of time, connecting back pressure system, add control pressure to back pressure system, it controls pressure must more than or equal to the pressure in autoclave；Connecting sea water metering front pump, inject simulated seawater solution in reactor, open outlet the 3rd valve, displacement goes out free natural gas unnecessary in autoclave。
Preferably, the concretely comprising the following steps of gas hydrate dissociation:
A) close import the second valve, outlet the 3rd valve and the 4th valve, remove back pressure system or back pressure system is controlled pressure be adjusted to 0；Connection outlet orthobaric volume room, the precision electronic balance being provided with calcium chloride jigger and total tolerance metering system。Closing the 4th valve, open outlet the 3rd valve 3, now the pressure in autoclave will be gradually decrease to balance；
B) closing outlet the 3rd valve, open the 4th valve, the indoor pressure of release outlet orthobaric volume is to atmospheric pressure；Turn off the 4th valve, open outlet the 3rd valve, make the gas hydrates in autoclave continue to decompose, reach balance to high pressure reacting kettle inner pressure；
C) repeating b) step, the gas hydrates to autoclave decompose completely；
D) the complete catabolic process of gas hydrates can be measured the natural gas cumulative volume of system meters gas hydrate dissociation release by total tolerance。The natural gas cumulative volume that obtains of metering can generate the natural gas cumulative volume Δ Vg of process consumption with gas hydrates to carry out contrast and corrects。
Preferably, the computational methods of gas hydrates saturation are:
Last gas replenishment process in gas hydrates synthesis, the natural gas that this process is filled with no longer is consumed, namely in previous step, the simulated seawater in porous media has been totally consumed formation gas hydrates, therefore opens the second valve for the last time and inflates an only isothermal expansion process in autoclave。The pore volume Ve occupied by natural gas can be calculated in now porous media, it is known that the pore volume of porous media is V by formulaΦ, can calculate and obtain gas hydrates volume V=VΦ-Ve, thus can calculate gas hydrates saturation。
A kind of gas hydrates synthesis and decomposition experiment system, system is gathered including water at low temperature bath system, autoclave, entrance criterion chamber volume, export standard chamber volume, total tolerance measuring container, pumped vacuum systems, pure methane gas cylinder, sea water metering front pump, back pressure system and temperature and pressure, wherein orthobaric volume room in entry and exit is provided with normal volume module, for calibrating, entrance criterion chamber volume volume, and and pipeline dead volume between reactor。
Compared with prior art, the invention have the advantages that
1, the entrance criterion chamber volume comprised in a kind of gas hydrates synthesis provided and decomposition experiment system and export standard chamber volume, can optimize synthesis and the decomposition of gas hydrates。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, moreover it can be used to accurately calculates the consumption of natural gas in gas hydrates building-up process。The use of export standard chamber volume can not only make the decomposition of gas hydrates carry out stage by stage, the problem that when solving gas hydrate dissociation in conventional decomposition method, temperature decrease causes pipeline ice blockage, moreover it can be used to the amount of natural gas of metering gas hydrate dissociation process release。
2, the method that the generation of gas hydrates adopts sustainable supply natural gas stage by stage, can make simulated seawater saturated in porous media generate gas hydrates completely。
3, in prior art, the metering conventional means of the consumption of gas hydrates building-up process natural gas is to import and export installation quality effusion meter at reactor, and the synthesis of gas hydrates is a process extremely slowly, mass flowmenter is difficult to collect flow around here, and therefore the method is difficult to accurately measure the consumption of natural gas。The present invention adopts the method for entrance criterion chamber volume, sets up P-V-T poised state equation, it is possible to accurately calculate the consumption of natural gas in gas hydrates building-up process。
4, gas hydrates provided by the invention synthesis and decomposition experiment method, in gas hydrate dissociation process, employing export standard chamber volume makes it decompose stage by stage gradually, and the natural gas total amount of release in adopting the metering of total tolerance measuring container to decompose, it is possible to the gas consumption calculated in building-up process is corrected in contrast。
Accompanying drawing explanation
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
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention clearly, below technical scheme in the present invention be clearly and completely described, it is clear that described embodiment is a part of embodiment of the present invention, rather than whole embodiments。Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain under not making creative work premise, broadly fall into the scope of protection of the invention。
Described a kind of gas hydrates synthesis is as follows with its specific implementation method of decomposition experiment method:
(1) to entrance criterion chamber volume volume V1, export standard chamber volume volume V2, pipeline dead volume V between autoclave and entrance criterion chamber volume1S, pipeline dead volume V between autoclave and export standard chamber volume2SDemarcation adopt P-V-T poised state equation, as shown in Figure 1。Between orthobaric volume room, export standard chamber volume, autoclave and entrance criterion chamber volume, between pipeline, autoclave and export standard chamber volume, pipeline is placed in water at low temperature bath system, before demarcation, opens 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 volume1SDemarcation: loading solid rustless steel module in autoclave, open the first valve 1 and the first valve 2, be filled with the gas of certain pressure, close the first valve 2, open the first valve 1 and discharge entrance orthobaric volume indoor gas, record original steady state pressure is PEnter 1, a；Closing the first valve 1, open the first valve 2, record steady state pressure is PEnter 1, b。Now set up P-V-T poised state equation:
Opening the first valve 1 and the first valve 2, gas in blowdown system, be again filled with the gas of certain pressure, close the first valve 2, open the first valve 1 and discharge entrance orthobaric volume indoor gas, record steady state pressure is PEnter 2, a；Known volume V is loaded in orthobaric volume closed chamber2Module, close the first valve 1, open the first valve 2, record steady state pressure is PEnter 2, b。Now set up P-V-T poised state equation:
Such repeatable operation repeatedly, is changed and is loaded the module volume that orthobaric volume is indoor。
Thus can obtain the P-V-T poised state equation under multiple temperature constant state:
Wherein, i=1,2,3 ..., n, and V1=0；ZEnter n, aAnd ZEnter n, bRespectively pressure is PEnter n, aAnd PEnter n, bThe compressibility factor of natural gas under condition；
Entrance criterion chamber volume V can be calculated by the P-V-T poised state equation under multiple temperature constant states1And pipeline dead volume V between autoclave and entrance criterion chamber volume1S。
Export standard chamber volume V2And pipeline dead volume V between autoclave and export standard chamber volume2SDemarcation: demarcating steps is ibid。
Wherein, i=1,2,3 ..., n, and V1=0；ZGo out n, aAnd ZGo out n, bRespectively pressure is PGo out n, aAnd PGo out n, bThe compressibility factor of natural gas under condition；
Entrance criterion chamber volume V can be calculated by the P-V-T poised state equation under multiple temperature constant states2And pipeline dead volume V between autoclave and entrance criterion chamber volume2S。
(2) experimental system principle is as shown in Figure 2。Concretely comprising the following steps of gas hydrates synthesis:
A) filling up sand grains in autoclave, successively compacting forms pie porous media, and its ratio of height to diameter is 1:6。Sealed reactor also checks the sealing of reactor。
B) close the 3rd valve 3, connect pumped vacuum systems, to autoclave evacuation, discharge the air in reactor, pipeline, entrance criterion chamber volume。Preparation simulated seawater, uses sea water metering front pump to the simulated seawater solution prepared saturated in porous media in reactor, the porosity of porous media and permeability in assaying reaction still。
C) connect high-pressure natural gas bottle, open the 5th valve 5, in reactor, be filled with the natural gas of certain pressure (4～10MPa)。Close first valve the 1, first valve 2, open the 3rd valve 3, drive in reactor part saturation simulation sea water in porous media out of。In order to make natural gas in natural gas hydrate formation have enough passage migrations in porous media and be fully contacted with simulated seawater, and the simulated seawater in porous media is entirely used for being formed after gas hydrates volume not over the pore volume of porous media, obtain according to experimental and theoretical computation, at least to drive the simulated seawater solution of porous media pore volume 25% out of, even if after the simulated seawater full form now in porous media becomes gas hydrates generation volumetric expansion, in porous media, some hole is the filling of natural gas institute。The simulated seawater quality discharged can be measured by the precision electronic balance being provided with calcium chloride jigger；According to the simulated seawater quality discharged, the pore volume shared by natural gas in pie porous media can be calculated；Close the 3rd valve 3, after stable system, the natural gas volume in system can be calculated according to P-V-T poised state equation。
D) in note porous media, pore volume shared by natural gas is Ve1, temperature is T, and pressure is P1,a, it is known that under this pressure condition, gas deviation factor is Z1,a。Set up P-V-T poised state equation:
P1,a(Ve1+V1s)=Z1,an1,aRT(5)
Thus can calculate natural gas volume Vg in normal conditionsⅠ:
Wherein P0, T0, Z0 respectively mark the pressure under state, temperature and gas deviation factor。
E) open water at low temperature bath system, reduce experimental temperature to about 1 DEG C and constant temperature。According to temperature and pressure acquisition system it can be seen that reacting kettle inner pressure is gradually lowered, pressure will no longer change after being reduced to certain value, and now system reaches steady statue, and record temperature of reaction system is T, and pressure is P1,b。Due to the generation of gas hydrates, inflated gas hydrates are occupied a part by the pore volume originally occupied by natural gas in porous media, and the pore volume occupied by natural gas in porous media after balance is designated as Ve2, thus can list the P-V-T poised state equation under steady statue:
P1,b(Ve2+V1s)=Z1,bn1,bRT(7)
Open the first valve 1, be filled with the natural gas of certain pressure to entrance criterion chamber volume, close the first valve 1。After natural gas in entrance criterion chamber volume is stable, record natural gas temperature is T, and pressure is P3。Now in entrance criterion chamber volume, the P-V-T poised state equation of natural gas is:
P3V1=Z3n3RT(8)
Opening the first valve 2, make the natural gas in entrance criterion chamber volume be expanded into autoclave, its expansion is up to Fast-Balance, and recording whole system temperature is T, and pressure is P2,a, isothermal expansion process can obtain:
P2,a(Ve2+V1s+ V1)=Z2,a(n1,b+n3)RT(9)
Can be derived, by formula (9), the pore volume that in porous media, natural gas occupies and be designated as Ve2:
Formula (10) is brought in formula (7), can derive and remain natural gas volume Vg in normal conditions in system after a gas hydrates generation reaches balance2:
Therefore the consumption Δ Vg of natural gas in course of reaction1:
ΔVg1=Vg2-Vg1(12)
F) closing the first valve 2, according to temperature and pressure acquisition system it can be seen that reacting kettle inner pressure is gradually lowered, pressure will no longer change after being reduced to certain value, and now system reaches steady statue。Open the first valve 1, be filled with the natural gas of certain pressure to entrance criterion chamber volume, close the first valve 1。After natural gas in entrance criterion chamber volume is stable, record natural gas temperature is T, and pressure is P3。Opening the first valve 2, make the natural gas in entrance criterion chamber volume be expanded into autoclave, its expansion is up to Fast-Balance。
G) cotype (3) is the same to the derivation of formula (9), can calculate second time gas hydrates and generate the consumption Δ Vg of process natural gas2:
ΔVg2=Vg3-Vg2(13)
H) previous step is repeated, until after after being filled with natural gas to reaction system, reacting kettle inner pressure no longer changes。Now the full form of the water in reactor becomes gas hydrates。And according to the natural gas volume consumed calculated in each process, gas hydrates can be obtained and form the natural gas cumulative volume Δ Vg of post consumption completely:
Δ Vg=Δ Vg1+ΔVg2+ΔVg3+……(14)
I) after gas hydrates balance and stability a period of time, connecting back pressure system, add control pressure to back pressure system, it controls pressure must more than or equal to the pressure in autoclave。Connecting sea water metering front pump, inject simulated seawater solution in reactor, open outlet the 3rd valve 3, displacement goes out free natural gas unnecessary in autoclave。
(3) the concretely comprising the following steps of gas hydrate dissociation:
A) close import the first valve 2, outlet the 3rd valve 3 and the 4th valve 4, remove back pressure system or back pressure system is controlled pressure be adjusted to 0。Connection outlet orthobaric volume room, the precision electronic balance being provided with calcium chloride jigger and total tolerance metering system。Closing the 4th valve 4, open outlet the 3rd valve 3, now the pressure in autoclave will be gradually decrease to balance。
B) closing outlet the 3rd valve 3, open the 4th valve 4, the indoor pressure of release outlet orthobaric volume is to atmospheric pressure。Turn off the 4th valve 4, open outlet the 3rd valve 3, make the gas hydrates in autoclave continue to decompose, reach balance to high pressure reacting kettle inner pressure。
C) repeating b) step, the gas hydrates to autoclave decompose completely。The complete catabolic process of gas hydrates can be measured the natural gas cumulative volume of system meters gas hydrate dissociation release by total tolerance。The natural gas cumulative volume that obtains of metering can generate the natural gas cumulative volume Δ Vg of process consumption with gas hydrates to carry out contrast and corrects。
(4) calculating of gas hydrates saturation
Last gas replenishment process in gas hydrates synthesis, the natural gas that this process is filled with no longer is consumed, namely in previous step, the simulated seawater in porous media has been totally consumed formation gas hydrates, therefore opens the second valve 2 for the last time and inflates an only isothermal expansion process in autoclave。The pore volume Ve occupied by natural gas can be calculated in now porous media, it is known that the pore volume of porous media is V by formula (8)Φ, can calculate and obtain gas hydrates volume V=VΦ-Ve, thus can calculate gas hydrates saturation。
A kind of gas hydrates synthesis and decomposition experiment system, system is gathered including water at low temperature bath system, autoclave, entrance criterion chamber volume, export standard chamber volume, total tolerance measuring container, pumped vacuum systems, pure methane gas cylinder, sea water metering front pump, back pressure system and temperature and pressure, wherein orthobaric volume room in entry and exit is provided with normal volume module, for calibrating, entrance criterion chamber volume volume, and and pipeline dead volume between reactor。
Last it is noted that above example is only in order to illustrate technical scheme, it is not intended to limit；Although the present invention being described in detail with reference to previous embodiment, it will be understood by those within the art that: the technical scheme described in foregoing embodiments still can be modified by it, or wherein portion of techniques feature is carried out equivalent replacement；And these amendments or replacement, do not make the essence of appropriate technical solution depart from the spirit and scope of various embodiments of the present invention technical scheme。
Claims (6)
1. a gas hydrates synthesis and decomposition experiment method, it is characterised in that comprise the following steps:
(1) to entrance criterion chamber volume volume V1, export standard chamber volume volume V2, pipeline dead volume V between autoclave and entrance criterion chamber volume1s, pipeline dead volume V between autoclave and export standard chamber volume2sDemarcate；
(2) filling up sand grains in autoclave, successively tamp, sealed reactor also checks the sealing of reactor；
(3) to the saturated simulated seawater solution prepared of porous media in reactor, the porosity of porous media and permeability in assaying reaction still；
(4) in reactor, inject natural gas, open reactor outlet valve, the partial simulation sea water in porous media in reactor is discharged, close reactor outlet valve, set up initial p-V-T poised state；
(5) in autoclave, high-pressure natural gas gradually it is filled with, until when pressure no longer changes in autoclave after being filled with natural gas, stopping being filled with natural gas；Period, gather reaction under high pressure temperature in the kettle and pressure；Each gas replenishment process, by P-V-T poised state Equation for Calculating insufflation gas volume；Finally statistics insufflation gas volume total amount, complete gas hydrates synthesize；
(6) after gas hydrates to be formed stablize certain time, simulated seawater is injected to drive free natural gas unnecessary in reactor away, the volume that the simulated seawater of the measurable natural gas volume being forced out of this process and injection is retained in reactor in reactor；
(7) open outlet valve, make gas hydrate dissociation stage by stage by export standard chamber volume；Measure, by export standard chamber volume, the natural gas volume that each stage decomposition of hydrate goes out, measure, again through total tolerance measuring container, the natural gas cumulative volume that decomposition of hydrate goes out；Whole process gathers reaction under high pressure temperature in the kettle and pressure。
2. gas hydrates according to claim 1 synthesis and decomposition experiment method, it is characterised in that: adopt P-V-T poised state equation to entrance criterion chamber volume volume V1, export standard chamber volume volume V2, pipeline dead volume V between autoclave and entrance criterion chamber volume1S, pipeline dead volume V between autoclave and export standard chamber volume2SDemarcation, between orthobaric volume room, export standard chamber volume, autoclave and entrance criterion chamber volume, between pipeline, autoclave and export standard chamber volume, pipeline is placed in water at low temperature bath system, before demarcation, open water at low temperature bath system, and constant temperature is to experimental temperature；
Described entrance criterion chamber volume V1And pipeline dead volume V between autoclave and entrance criterion chamber volume1SDemarcation: load solid rustless steel module in autoclave, open the first valve (1) and the second valve (2), it is filled with the gas of certain pressure, close the second valve (2), opening the first valve (1) release entrance orthobaric volume indoor gas, record original steady state pressure is PEnter 1, a；Closing the first valve (1), open the second valve (2), record steady state pressure is PEnter 1, b；Now set up P-V-T poised 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 second valve (2), opening the first valve (1) release entrance orthobaric volume indoor gas, record steady state pressure is PEnter 2, a；Known volume V is loaded in orthobaric volume closed chamber2Module, close the first valve (1), open the second valve (2), record steady state pressure is PEnter 2, b；Now set up P-V-T poised state equation:
Such repeatable operation repeatedly, is changed and is loaded the module volume that orthobaric volume is indoor；Thus can obtain the P-V-T poised state equation under multiple temperature constant state:
Wherein, i=1,2,3 ..., n, and V1=0；ZEnter n, aAnd ZEnter n, bRespectively pressure is PEnter n, aAnd PEnter n, bThe compressibility factor of natural gas under condition；
Pipeline dead volume V between entrance criterion chamber volume V1 and autoclave and entrance criterion chamber volume can be calculated by the P-V-T poised state equation under multiple temperature constant states1S；
Export standard chamber volume V2And pipeline dead volume V between autoclave and export standard chamber volume2SDemarcation: demarcating steps is ibid；
Wherein, i=1,2,3 ..., n, and V1=0；ZGo out n, aAnd ZGo out n, bRespectively pressure is PGo out n, aAnd PGo out n, bThe compressibility factor of natural gas under condition；
Pipeline dead volume V between entrance criterion chamber volume V2 and autoclave and entrance criterion chamber volume can be calculated by the P-V-T poised state equation under multiple temperature constant states2S。
3. gas hydrates according to claim 1 synthesis and decomposition experiment method, it is characterised in that concretely comprising the following steps of gas hydrates synthetic method:
A) filling up sand grains in autoclave, successively compacting forms pie porous media, and its ratio of height to diameter is 1:6；Sealed reactor also checks the sealing of reactor；
B) close the 3rd valve (3), connect pumped vacuum systems, to autoclave evacuation, discharge the air in reactor, pipeline, entrance criterion chamber volume；Preparation simulated seawater, uses sea water metering front pump to the simulated seawater solution prepared saturated in porous media in reactor, the porosity of porous media and permeability in assaying reaction still；
C) connect high-pressure natural gas bottle, in reactor, be filled with the natural gas of 4～10MPa；Close the first valve (1), the second valve (2), open the 3rd valve (3), drive in reactor part saturation simulation sea water in porous media out of；In order to make natural gas in natural gas hydrate formation have enough passage migrations in porous media and be fully contacted with simulated seawater, and the simulated seawater in porous media is entirely used for being formed after gas hydrates volume not over the pore volume of porous media, obtain according to experimental and theoretical computation, at least to drive the simulated seawater solution of porous media pore volume 25% out of, even if after the simulated seawater full form now in porous media becomes gas hydrates generation volumetric expansion, in porous media, some hole is the filling of natural gas institute；The simulated seawater quality discharged can be measured by the precision electronic balance being provided with calcium chloride jigger；According to the simulated seawater quality discharged, the pore volume shared by natural gas in pie porous media can be calculated；Close the 3rd valve (3), after stable system, the natural gas volume in system can be calculated according to P-V-T poised state equation；
In note porous media, the pore volume shared by natural gas is Ve1, temperature is T, and pressure is P1,a, it is known that under this pressure condition, gas deviation factor is Z1,a, set up P-V-T poised state equation:
P1,a(Ve1+V1s)=Z1,an1,aRT(5)
Thus can calculate natural gas volume Vg in normal conditionsⅠ:
Wherein P0, T0, Z0 respectively mark the pressure under state, temperature and gas deviation factor；
D) open water at low temperature bath system, reduce experimental temperature to about 1 DEG C and constant temperature；According to temperature and pressure acquisition system it can be seen that reacting kettle inner pressure is gradually lowered, pressure will no longer change after being reduced to certain value, and now system reaches steady statue, and record temperature of reaction system is T, and pressure is P1,b；Due to the generation of gas hydrates, inflated gas hydrates are occupied a part by the pore volume originally occupied by natural gas in porous media, and the pore volume occupied by natural gas in porous media after balance is designated as Ve2, thus can list the P-V-T poised state equation under steady statue:
P1,b(Ve2+V1s)=Z1,bn1,bRT(7)
Open the first valve (1), be filled with the natural gas of certain pressure to entrance criterion chamber volume, close the first valve (1)；After natural gas in entrance criterion chamber volume is stable, record natural gas temperature is T, and pressure is P3；Now in entrance criterion chamber volume, the P-V-T poised state equation of natural gas is:
P3V1=Z3n3RT(8)
Opening the second valve (2), make the natural gas in entrance criterion chamber volume be expanded into autoclave, its expansion is up to Fast-Balance, and recording whole system temperature is T, and pressure is P2,a, isothermal expansion process can obtain:
P2,a(Ve2+V1s+ V1)=Z2,a(n1,b+n3)RT(9)
Can be derived, by formula (9), the pore volume that in porous media, natural gas occupies and be designated as Ve2:
Formula (10) is brought in formula (7), can derive and remain natural gas volume Vg in normal conditions in system after a gas hydrates generation reaches balance2:
Therefore the consumption Δ Vg of natural gas in course of reaction1:
ΔVg1=Vg2-Vg1(12)
E) closing the second valve (2), according to temperature and pressure acquisition system it can be seen that reacting kettle inner pressure is gradually lowered, pressure will no longer change after being reduced to certain value, and now system reaches steady statue；Open the first valve (1), be filled with the natural gas of certain pressure to entrance criterion chamber volume, close the first valve (1)；After natural gas in entrance criterion chamber volume is stable, record natural gas temperature is T, and pressure is P3；Opening the second valve (2), make the natural gas in entrance criterion chamber volume be expanded into autoclave, its expansion is up to Fast-Balance；
Cotype (3) is the same to the derivation of formula (9), can calculate second time gas hydrates and generate the consumption Δ Vg of process natural gas2:
ΔVg2=Vg3-Vg2(13)
F) previous step is repeated, until after after being filled with natural gas to reaction system, reacting kettle inner pressure no longer changes；Now the full form of the water in reactor becomes gas hydrates；And according to the natural gas volume consumed calculated in each process, gas hydrates can be obtained and form the natural gas cumulative volume Δ Vg of post consumption completely:
Δ Vg=Δ Vg1+ΔVg2+ΔVg3+……(14)
G) after gas hydrates balance and stability a period of time, connecting back pressure system, add control pressure to back pressure system, it controls pressure must more than or equal to the pressure in autoclave；Connecting sea water metering front pump, inject simulated seawater solution in reactor, open outlet the 3rd valve (3), displacement goes out free natural gas unnecessary in autoclave。
4. gas hydrates according to claim 3 synthesis and decomposition experiment method, it is characterised in that concretely comprising the following steps of gas hydrate dissociation:
A) import the second valve (2), outlet the 3rd valve (3) and the 4th valve (4) are closed, dismounting back pressure system or back pressure system is controlled pressure be adjusted to 0；Connection outlet orthobaric volume room, the precision electronic balance being provided with calcium chloride jigger and total tolerance metering system；Closing the 4th valve (4), open outlet the 3rd valve (3), now the pressure in autoclave will be gradually decrease to balance；
B) closing outlet the 3rd valve (3), open the 4th valve (4), the indoor pressure of release outlet orthobaric volume is to atmospheric pressure；Turn off the 4th valve (4), open outlet the 3rd valve (3), make the gas hydrates in autoclave continue to decompose, reach balance to high pressure reacting kettle inner pressure；
C) repeating b) step, the gas hydrates to autoclave decompose completely；
D) the complete catabolic process of gas hydrates can be measured the natural gas cumulative volume of system meters gas hydrate dissociation release by total tolerance；The natural gas cumulative volume that obtains of metering can generate the natural gas cumulative volume Δ Vg of process consumption with gas hydrates to carry out contrast and corrects。
5. gas hydrates according to claim 3 synthesis and decomposition experiment method, it is characterised in that the computational methods of gas hydrates saturation are:
Last gas replenishment process in gas hydrates synthesis, the natural gas that this process is filled with no longer is consumed, namely in previous step, the simulated seawater in porous media has been totally consumed formation gas hydrates, therefore opens the second valve (2) for the last time and inflates an only isothermal expansion process in autoclave；The pore volume Ve occupied by natural gas can be calculated in now porous media, it is known that the pore volume of porous media is V by formula (8)Φ, can calculate and obtain gas hydrates volume V=VΦ-Ve, thus can calculate gas hydrates saturation。
6. a gas hydrates synthesis and decomposition experiment system, it is characterized in that: include water at low temperature bath system, autoclave, entrance criterion chamber volume, export standard chamber volume, total tolerance measuring container, pumped vacuum systems, pure methane gas cylinder, sea water metering front pump, back pressure system and temperature and pressure and gather system, wherein orthobaric volume room in entry and exit is provided with normal volume module, for calibrating, entrance criterion chamber volume volume, and and pipeline dead volume between reactor。
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