CN105181728B - The method of nuclear magnetic resonance on-line checking shale gas - Google Patents
The method of nuclear magnetic resonance on-line checking shale gas Download PDFInfo
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- CN105181728B CN105181728B CN201510441634.5A CN201510441634A CN105181728B CN 105181728 B CN105181728 B CN 105181728B CN 201510441634 A CN201510441634 A CN 201510441634A CN 105181728 B CN105181728 B CN 105181728B
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- shale
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- magnetic resonance
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- nuclear magnetic
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[C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000000499 gels Substances 0.000 description 1
- 235000005035 ginseng Nutrition 0.000 description 1
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Abstract
Description
Technical field
The present invention relates to oil exploration and development fields, more particularly to a kind of method of nuclear magnetic resonance on-line checking shale gas.
Background technology
Shale gas be it is a kind of with dissociate and ADSORPTION STATE be stored in rammell or shale layer in Unconventional gas, into To stir the strength of world market, the energy general layout in the world has greatly been rewritten.
The method of present analysis mud shale adsorbed gas is mainly the adsorption isotherm experiment for using for reference coal bed gas.The method is by powder The shale samples of last shape are placed in sealing container, determine it in mutually synthermal, different pressures condition when that is issued to adsorption equilibrium institute The volume of the experimental gas such as the methane of absorption, then according to Langmuir adsorption theories, calculate Lan Shi volumes, Lan Shi pressure with And adsorption isothermal curve.The method complex operation and analysis efficiency is relatively low.
In recent years, nuclear magnetic resonance technique was paid much attention to and was developed in oil exploration and development fields, was widely used to The aspects such as nuclear magnetic resonance logging, nuclear magnetic resonance log and low permeability reservoir evaluation.It is a kind of using magnetic resonance detection shale gas Direct measuring method.Absorption tolerance and free is determined in shale gas by the signal of hydrogen nuclei in direct detection shale gas Tolerance, can have it is quick, accurate, simple to operate the features such as.
However, the NMR signal due to shale gas cannot be detected under normal temperature and pressure conditionses, so not having still at present Nuclear magnetic resonance on-line monitoring technique is carried out to shale samples.
The content of the invention
The present invention provides a kind of method of nuclear magnetic resonance on-line checking shale gas, to solve above-mentioned one or more missing.
The embodiment of the present invention provides a kind of method of nuclear magnetic resonance on-line checking shale gas, and methods described includes：Using one HTHP probe sets pressure to shale samples temperature-pressure therein a to design temperature and one, and the design temperature is It is 150~170 DEG C, described to set pressure as 50~60MPa；Under the design temperature and the setting pressure, using a pulse Shale samples described in sequence pair carry out Nuclear Magnetic Resonance Measurement, and inverting obtains the relaxation time T2 spectrums of the shale samples；According to institute State absorption gas saturation and free gas saturation that relaxation time T2 spectrums calculate the shale samples.
In one embodiment, using HTHP probe to shale samples temperature-pressure therein a to design temperature and One setting pressure, including：It is put into after the shale samples are dried in the clamper of the HTHP probe；To described HTHP probe is vacuumized；Be forced into for the shale samples described by the displacement component popped one's head in using the HTHP Setting pressure；The shale samples are heated up to the design temperature by the high-temperature heating component popped one's head in using the HTHP.
In one embodiment, under the design temperature and the setting pressure, using a pulse train to the shale Sample carries out Nuclear Magnetic Resonance Measurement, and inverting obtains the relaxation time T2 spectrums of the shale samples, including：According to the pulse train Excited nucleus magnetic resonance excitation signal；Electric current driving and power amplification are carried out to the nuclear magnetic resonance pumping signal, after generation treatment Nuclear magnetic resonance pumping signal；Using the nuclear magnetic resonance pumping signal after the treatment, in the design temperature and the setting The shale samples are excited under pressure, a nmr echo signal is produced；Inverting is carried out to the nmr echo signal Obtain the relaxation time T2 spectrums.
In one embodiment, the absorption gas saturation of the shale samples is calculated according to relaxation time T2 spectrums and is dissociated Gas saturation, including：The cutoff of free state shale gas and ADSORPTION STATE shale gas is calculated according to relaxation time T2 spectrums；According to The cutoff calculates absorption gas saturation and the free gas saturation.
In one embodiment, methods described also includes：Permeability according to the shale samples sets the relaxation time Time of measuring interval in T2 spectrums, is monitored with the free state shale gas and ADSORPTION STATE shale gas to the shale samples.
In one embodiment, the high-temperature heating component includes heating film, and the heating film will be described by power consumption Shale samples are heated up to the design temperature.
The method of the nuclear magnetic resonance on-line checking shale gas of the embodiment of the present invention is high by the way that shale samples are maintained at into high temperature In pressure ring border and carry out detection shale gas, can situation of the rammell containing shale gas in analogue measurement stratum, be conducive to accurate analysis The situation of natural gas is stored in stratum.The method of the nuclear magnetic resonance on-line checking shale gas of the embodiment of the present invention can be evaluated preferably The occurrence status of shale gas (methane gas) and quickly acquisition adsorbed gas, free gas saturation.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing The accompanying drawing to be used needed for having technology description is briefly described, it should be apparent that, drawings in the following description are only this hairs Some bright embodiments, for those of ordinary skill in the art, on the premise of not paying creative work, can be with root Other accompanying drawings are obtained according to these accompanying drawings.In the accompanying drawings：
Fig. 1 is the schematic flow sheet of the method for the nuclear magnetic resonance on-line checking shale gas of the embodiment of the present invention；
Fig. 2 is the schematic flow sheet of the method to shale samples temperature-pressure in one embodiment of the invention；
Fig. 3 is the schematic flow sheet of the method that in one embodiment of the invention shale samples are carried out with Nuclear Magnetic Resonance Measurement；
Fig. 4 is the method for the absorption gas saturation and free gas saturation of calculating shale samples in one embodiment of the invention Schematic flow sheet；
Fig. 5 is the schematic flow sheet of the shale gas magnetic resonance detection method of one embodiment of the invention；
Fig. 6 is the structural representation of the system of the nuclear magnetic resonance on-line checking shale gas of the embodiment of the present invention；
Fig. 7 is the structural representation of full diameter magnet in the embodiment of the present invention；
Fig. 8 is the structural representation of embodiment of the present invention high temperature high-voltage probe；
Fig. 9 is the shale core 10MPa pressure saturation methane gas different time course relaxation times in one embodiment of the invention The curve map of T2 spectrums；
Figure 10 is the curve map of the relaxation time T2 spectrums of different time of measuring in one embodiment of the invention；
Figure 11 is shale core 10MPa pressure saturation methane gas free state in one embodiment of the invention, ADSORPTION STATE and total Semaphore versus time curve figure.
Specific embodiment
For the purpose, technical scheme and advantage for making the embodiment of the present invention become more apparent, below in conjunction with the accompanying drawings to this hair Bright embodiment is described in further details.Here, schematic description and description of the invention is used to explain the present invention, but simultaneously It is not as a limitation of the invention.
Fig. 1 is the schematic flow sheet of the method for the nuclear magnetic resonance on-line checking shale gas of the embodiment of the present invention.Such as Fig. 4 institutes Show, the method for the nuclear magnetic resonance on-line checking shale gas of the embodiment of the present invention, including step：
S101：Using HTHP probe to shale samples temperature-pressure therein a to design temperature and a setting pressure By force, the design temperature is 150~170 DEG C, described to set pressure as 50~60MPa；
S102：Under the design temperature and the setting pressure, the shale samples are carried out using a pulse train Nuclear Magnetic Resonance Measurement, inverting obtains the relaxation time T2 spectrums of the shale samples；
S103：The absorption gas saturation and free gas saturation of the shale samples are calculated according to relaxation time T2 spectrums Degree.
The method of the nuclear magnetic resonance on-line checking shale gas of the embodiment of the present invention, by above-mentioned design temperature and setting pressure High-temperature and high-pressure conditions in simulated formation, and shale samples to being maintained in high temperature and high pressure environment carry out detection shale gas, mould Plan measures situation of the rammell containing shale gas in stratum, is conducive to accurately analyzing the situation of storage natural gas in stratum.
Fig. 2 is the schematic flow sheet of the method to shale samples temperature-pressure in one embodiment of the invention.Such as Fig. 2 institutes Show, in above-mentioned steps S101, using HTHP probe to shale samples temperature-pressure therein a to design temperature and The method for setting pressure, it may include step：
S201：It is put into after the shale samples are dried in the clamper of the HTHP probe；
S202：HTHP probe is vacuumized；
S203：The shale samples are forced into the setting pressure by the displacement component popped one's head in using the HTHP；
S204：The shale samples are heated up to the setting temperature by the high-temperature heating component popped one's head in using the HTHP Degree.
In above-mentioned steps S203, the scope for setting pressure is 50MPa~60MPa or the pressure values of other superatmospherics, Can be in a preferred embodiment 55MPa, with the High Voltage in simulated formation；In above-mentioned steps S204, the model of design temperature It is 150 DEG C~170 DEG C to enclose, and can be in a preferred embodiment 160 DEG C, with the high-temperature in simulated formation.
Existing nuclear magnetic resonance technique, can only be detected at normal temperatures and pressures, it is impossible to detect the signal of shale gas.And this Shale samples can be maintained at high by the displacement component and high-temperature heating component that inventive embodiments are popped one's head in by above-mentioned HTHP Warm hyperbaric environment, so as to realize nuclear magnetic resonance on-line checking shale gas.
Fig. 3 is the schematic flow sheet of the method that in one embodiment of the invention shale samples are carried out with Nuclear Magnetic Resonance Measurement. As shown in figure 3, under the design temperature and the setting pressure, nuclear-magnetism is carried out to the shale samples using a pulse train Resonance measuring, the method that inverting obtains the relaxation time T2 spectrums of the shale samples, it may include step：
S301：According to the pulse train excited nucleus magnetic resonance excitation signal；
S302：Electric current driving and power amplification are carried out to the nuclear magnetic resonance pumping signal, the nuclear-magnetism after generation treatment is total to Shake pumping signal；
S303：Using the nuclear magnetic resonance pumping signal after the treatment, under the design temperature and the setting pressure The shale samples are excited, a nmr echo signal is produced；
S304：Inverting is carried out to the nmr echo signal and obtains the relaxation time T2 spectrums.
In the embodiment of the present invention, by exciting shale samples under high-temperature and high-pressure conditions, the nuclear-magnetism of wherein shale gas is produced Resonance echo signal, to detect the shale gas in shale samples, can obtain and more meet rammell reality containing shale gas in stratum The nmr echo signal of situation.
Fig. 4 is the method for the absorption gas saturation and free gas saturation of calculating shale samples in one embodiment of the invention Schematic flow sheet.As shown in figure 4, in the method for nuclear magnetic resonance on-line checking shale gas shown in Fig. 1, during according to the relaxation Between T2 spectrums calculate the shale samples absorption gas saturation and free gas saturation method, it may include step：
S401：The cutoff of free state shale gas and ADSORPTION STATE shale gas is calculated according to relaxation time T2 spectrums；
S402：Absorption gas saturation and the free gas saturation are calculated according to the cutoff.
In the embodiment of the present invention, pass through that surveyed relaxation time T2 spectrum is calculated be it is free with absorption T2 cutoffs, from And obtain absorption gas saturation and free gas saturation.Obtained by the embodiment of the present invention it is free with adsorb T2 cutoffs with it is movable Fluid with constraint fluid T2 cutoffs it is different because moveable gel include mobile water saturation, oil saturation and Gas saturation, rather than free gas and adsorbed gas.It is exist to inhale the characteristics of shale gas are maximum additionally, compared with conventional gas Attached gas, but it be it is movable, it is minable, and can not realize obtaining it for the movable adsorbed gas in the prior art The technical scheme of saturation degree.
Fig. 5 is the schematic flow sheet of the shale gas magnetic resonance detection method of one embodiment of the invention.As shown in figure 5, Fig. 1 The method of shown nuclear magnetic resonance on-line checking shale gas, may also include step：
S104：Permeability according to the shale samples sets the time of measuring interval in the relaxation time T2 spectrums, with Free state shale gas and ADSORPTION STATE shale gas to the shale samples are monitored.
In the embodiment of the present invention, it is spaced by setting time of measuring, repeatedly the relaxation time T2 spectrums of measurement shale samples, can To detect in shale samples that free state shale gas and ADSORPTION STATE shale gas change with time situation, different scale can be effectively embodied The difference of methane mass transfer and hosting pattern in hole, so that rammell contains shale gas situation in obtaining more rich analysis stratum Experimental basis, are that clear and definite methane gas hosting pattern and coupling mass transfer rule lay the foundation.
The method of the nuclear magnetic resonance on-line checking shale gas of the embodiment of the present invention can be by the system of following each embodiments or dress Put or component is realized.
Fig. 6 is the structural representation of the system of the nuclear magnetic resonance on-line checking shale gas of the embodiment of the present invention.Such as Fig. 6 institutes Show, the system of the nuclear magnetic resonance on-line checking shale gas used by the method for nuclear magnetic resonance on-line checking shale gas as shown in Figure 1, May include：Detection system 100 and control system 200.
Detection system 100 may include full diameter magnet 110, HTHP probe 120, temperature control component 130.Full diameter magnet 110 is a closed cavity；HTHP probe 120 is located at the inside of the full diameter magnet, for placing a shale samples, and For the shale samples provide above-mentioned design temperature and setting pressure, with simulated formation environment；Temperature control component 130 is located at the full diameter The outer surface of magnet, for, in above-mentioned design temperature, the design temperature can be one constant by the temperature control of the full diameter magnet Temperature.
Control system 200 may include computer 201, master controller 202, frequency generator 203, power amplifier 204, T/ R match circuits 205, preamplifier 206, receiver 207, A/D converter 208.Computer 201 is used to set an experiment ginseng Number；Master controller 202 is connected with computer 201, and a pulse train is produced with according to the experiment parameter；Frequency generator 203 with Master controller 202 is connected, and electric current driving is carried out with the nuclear magnetic resonance pumping signal excited to the pulse train；Power amplifier 204 are connected with frequency generator 203, and signal amplification is carried out with the nuclear magnetic resonance pumping signal after being driven to electric current；T/R matching electricity The one end on road 205 is connected with the power amplifier 204, and the other end of T/R match circuits 205 connects with HTHP probe 120 Connect, to be transmitted turning between one nmr echo signal of nuclear magnetic resonance pumping signal and reception amplified by signal Change；Preamplifier 206 is connected with the T/R match circuits 205, and signal amplification is carried out with to the nmr echo signal；Connect Receive device 207 to be connected with the preamplifier 206, to gather the nmr echo signal after signal amplifies；A/D converter 208 One end be connected with the receiver 207, the other end of A/D converter 208 is connected with the master controller 202, to the core after amplification Magnetic resonance echo signals carry out A/D conversions, and nmr echo signal after A/D is changed is passed by the master controller 202 The computer 201 is delivered to, to show the Nuclear Magnetic Resonance Measurement result of the shale samples on the computer 201.
In the system of above-mentioned nuclear magnetic resonance on-line checking shale gas, HTHP probe can be heated to shale samples therein 150 DEG C~170 DEG C of design temperature and the setting pressure of 50MPa~60MPa are forced into, to realize on-line checking shale gas.
Fig. 7 is the structural representation of full diameter magnet in the embodiment of the present invention.As shown in fig. 7, the nuclear magnetic resonance shown in Fig. 6 In the system of on-line checking shale gas, full diameter magnet 110 may include pole plate 111, magnet steel 112, threshold 113, yoke plate 114 and side Yoke plate 115.
Two pieces of yoke plates 114 being oppositely arranged and two pieces of side yoke plates 115 being oppositely arranged are sequentially connected one framework of composition, with shape Into a closed-loop path；Two blocks of magnet steel 112 are individually fixed in two pieces of relative inner sides of yoke plate 114, think that above-mentioned shale samples are carried For a magnetic field；Two pieces of pole plates 111 are individually fixed in two pieces of relative inner sides of magnet steel 112, to carry out carrying out magnetic conduction to the magnetic field； Two thresholds 113 are respectively embedded into two pieces of relative inner sides of pole plate 111.
In one embodiment, yoke plate 114 be flat board, length between 560~600mm, width between 400~550mm, Thickness is between 10~20mm.Side yoke plate 115 be flat board, length between 400~550mm, width between 300~450mm, Thickness is between 10~20mm.Two pieces of side yoke plates 115 and two pieces of yoke plates 114 constitute a framework, are that magnet forms a closure Loop.One block of magnet steel 112 is fixed respectively in the relative medial surface of two pieces of yoke plates 114.The length of magnet steel 112 is in 460~500mm Between, between 300~450mm, thickness is between 10~20mm for width.Magnet steel 112 is used as magnetic source.Relative in magnet steel is put down One piece of pole plate 111 is respectively fixed with face.The length of pole plate 111 between 480~520mm, width between 320~470mm, Thickness is between 10~20mm.Pole plate 111 plays magnetic conduction effect.The full outer surface of diameter magnet 110 is one group of temperature control component 130, 10~60 degree of thermostatic controls can be carried out to full diameter magnet 110, influence of the temperature to apparatus measures result is reduced.
Fig. 8 is the structural representation of embodiment of the present invention high temperature high-voltage probe.As shown in figure 8, the height in said system Warm high-voltage probe 120 may include ring pressure component, high-temperature heating component, displacement component and nuclear magnetic resonance assembly.
Ring pressure component may include that a clamper cavity 1212 for end cover 1211 is fixed at two ends respectively, with to shale sample Product 1213 apply ring pressure, may also include ring and are pressed into oil pipe 1214 and Huan Ya oil discharge pipes 1215.
High-temperature heating component may include to be sequentially arranged in the spiral heat-conducting oil pipes in the outside of clamper cavity 1212 from inside to outside 1221 and lagging casing 1222, heated with to the shale samples 1213.
Displacement component may include that the first shale samples being sequentially connected come directly towards the 1231, first seal 1232, displacement oil-feed Pipe 1233 and the displacement flowline 1234 being sequentially connected, the second seal 1235, the second shale samples top 1236, displacement oil-feed The end cover 1211 of pipe 1218 and displacement flowline 1219 also respectively with the two ends of clamper cavity 1212 is connected, with to the shale Sample 1213 carries out displacement test.
The nuclear magnetic resonance assembly may include outer surface be wound with malcoils nuclear magnetic resonance skeleton 1241 and with institute The extraction joint 1242 of malcoils connection, and the nuclear magnetic resonance skeleton 1241 are stated located at the interior of the clamper cavity 1212 Portion, with receive by signal amplify above-mentioned nuclear magnetic resonance pumping signal and launch the nmr echo signal.
During the method for nuclear magnetic resonance on-line checking shale gas of the invention, high-temperature heating component therein can be thin by heating Film substitutes above-mentioned spiral heat-conducting oil pipes 1221, and heating film produces heat so that producing high temperature inside clamper by power consumption, With this system can be made succinct, easy to operate.
In one embodiment, then as shown in figure 8, the HTHP probe 120 and the T/R match circuits 205 between, the T/ Between R match circuits 205 and the power amplifier 204, between the T/R match circuits 205 and the preamplifier 206, the work( Between rate amplifier 204 and the frequency generator 203, between the frequency generator 203 and the master controller 202, the receiver USB can be passed through by cable connection between the master controller 202 and the computer 201 between 207 and the A/D converter 208 Interface is connected.
In one embodiment, the A/D converter 208 can be cached to the echo-signal of the collection；Above-mentioned setting is permanent The scope of constant temperature degree can be [10 degree, 60 degree]；Above-mentioned echo-signal can be amplified 70DB by the preamplifier 206.
Shale gas magnetic resonance detection device of the invention, sets as a result of HTHP probe and major diameter uniform field Meter, can carry out nuclear magnetic resonance on-line testing under high-temperature and high-pressure conditions, obtain one-dimensional relaxation time T2 spectrums, quick measurement Free state gas saturation and ADSORPTION STATE gas saturation, can preferably Real-Time Evaluation shale reservoir and identification shale gas preservation State.Meanwhile, nuclear magnetic resonance on-line checking shale gas measurement apparatus can be with high pressure saturation methane gas, the change composed by T2, The difference of shale gas (such as methane) mass transfer and hosting pattern in different scale hole can be effectively embodied, is clear and definite shale gas (first Alkane gas) hosting pattern and coupling mass transfer rule lay the foundation.
The method of nuclear magnetic resonance on-line checking shale gas according to an embodiment of the invention, to the shale containing methane gas Sample carries out nuclear magnetic resonance on-line checking.Shale samples are measured using CPMG pulse sequence, inverting obtains the relaxation time T2 is composed.According to the permeability of shale, the interval time of measurement is set, the purpose of monitoring is reached.Table 1 shows time of measuring and correspondence CPMG sequence measurement parameter.
Table 1
Fig. 9 is the shale core 10MPa pressure saturation methane gas different time course relaxation times in one embodiment of the invention The curve map of T2 spectrums.As shown in figure 9, relaxation time T2 spectrums are mainly distributed between 0.3ms~20ms, increase over time, T2 spectrums are constantly moved left and right.Relaxation time T2 spectrums are moved to the left expression gas into fine pore or are adsorbed onto organic matter table Face.Relaxation time T2 spectrums move right very low mainly due to shale core permeability, and methane gas is limited by pore throat, very Difficulty is rapidly entered in hole, and methane gas pressure is relatively low in hole, is increased over time intrapore methane gas and is constantly increased Plus, cause pressure to increase, so the relaxation time T2 spectrums of saturation methane can be moved to right in shale core.
Figure 10 is the curve map of the relaxation time T2 spectrums of different time of measuring in one embodiment of the invention.As shown in Figure 10. When shale core saturation abundant by methane gas, there are two peaks in relaxation time T2 spectrums, therefore, a peak is the first of free state Alkane gas, another peak is the methane gas of ADSORPTION STATE, and the ADSORPTION STATE and free state T2 cutoffs for determining this block shale core are 1.3ms.Absorption gas saturation is 37.3%, and the gas saturation that dissociates is 62.7%.
Figure 11 is shale core 10MPa pressure saturation methane gas free state in one embodiment of the invention, ADSORPTION STATE and total Semaphore versus time curve figure.As shown in figure 11, after methane gas enters in shale, starting stage free gas increases speed Degree is very fast, and methane gas is mainly present in shale hole in free state form, because methane gas in starting stage hole Body pressure is smaller, is unfavorable for absorption.Interstage adsorbed gas gathers way comparatively fast, free gas gather way it is slack-off, mainly by Gradually increase in methane gas pressure in hole, and methane gas progresses into the more organic matter surfaces of more holes and connects Touch, adsorption rate is accelerated.Terminal stage free gas gathers way and slows down, adsorbed gas gather way it is slack-off, progressively reach pressure put down Weighing apparatus.
The method of the nuclear magnetic resonance on-line checking shale gas of the embodiment of the present invention is high by the way that shale samples are maintained at into high temperature In pressure ring border and carry out detection shale gas, can situation of the rammell containing shale gas in analogue measurement stratum, be conducive to accurate analysis The situation of natural gas is stored in stratum.The method of the nuclear magnetic resonance on-line checking shale gas of the embodiment of the present invention can be evaluated preferably The occurrence status of shale gas (methane gas) and quickly acquisition adsorbed gas, free gas saturation.
Particular embodiments described above, has been carried out further in detail to the purpose of the present invention, technical scheme and beneficial effect Describe in detail bright, should be understood that and the foregoing is only specific embodiment of the invention, the guarantor being not intended to limit the present invention Shield scope, all any modification, equivalent substitution and improvements within the spirit and principles in the present invention, done etc., should be included in this Within the protection domain of invention.
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| CN106770413B (en) * | 2016-11-29 | 2018-05-29 | 中国矿业大学 | A kind of method for measuring coal adsorbed methane or horizontal number of molecule layers |
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| CN107202811B (en) * | 2017-08-03 | 2019-06-28 | 中国地质大学（北京） | It is a kind of while measuring ADSORPTION STATE and the measuring method of free state methane in shale |
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