CN105181728A - Method for nuclear magnetic resonance on-line detection of shale gas - Google Patents
Method for nuclear magnetic resonance on-line detection of shale gas Download PDFInfo
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Abstract
The invention provides a method for nuclear magnetic resonance on-line detection of shale gas. The method comprises steps: a shale sample is heated to a set temperature and pressurized to a set pressure by utilization of a high-temperature and high-pressure probe, the set temperature is 150-170 DEG C, and the set pressure is 50-60MPa; at the set temperature and the set pressure, the shale sample is subjected to nuclear magnetic resonance measurement by utilization of a pulse sequence, and the relaxation time T2 spectrum of the shale sample is obtained through inversion; the adsorbed gas saturability and the free gas saturability of the shale sample are calculated according to the relaxation time T2 spectrum. The detection method can evaluate occurrence of methane well and obtains the adsorbed gas saturability and the free gas saturability rapidly.
Description
Technical field
The present invention relates to oil exploration and development fields, particularly relate to a kind of method of nuclear magnetic resonance on-line checkingi shale gas.
Background technology
Shale gas is a kind of Unconventional forage be stored in free and ADSORPTION STATE in shale bed or shale layer, is becoming the strength of stirring world market, is greatly rewriting the energy general layout in the world.
The method of present analysis mud shale adsorbed gas mainly uses for reference the adsorption isotherm experiment of coal-seam gas.The method is that pulverous shale samples is placed in airtight container, measure the volume of the experimental gas such as its methane adsorbed when identical temperature, different pressures condition are issued to adsorption equilibrium, then according to Langmuir adsorption theory, Lan Shi volume, Lan Shi pressure and adsorption isothermal curve is calculated.The method complicated operation and analysis efficiency is lower.
In recent years, nuclear magnetic resonance technique was paid much attention in oil exploration and development fields and was developed, and had been widely used in the aspects such as nuclear magnetic resonance logging, nuclear magnetic resonance log and low permeability reservoir evaluation.Magnetic resonance detection shale gas is utilized to be a kind of direct measuring method.By the signal of hydrogen nuclei in direct-detection shale gas, determine in shale gas, to adsorb tolerance and free tolerance, the features such as quick, accurate, simple to operate can be had.
But, due to the NMR signal of shale gas cannot be detected under normal temperature and pressure conditions, so still do not carry out nuclear magnetic resonance on-line monitoring technique to shale samples at present.
Summary of the invention
The invention provides a kind of method of nuclear magnetic resonance on-line checkingi shale gas, to solve above-mentioned one or more disappearance.
The embodiment of the present invention provides a kind of method of nuclear magnetic resonance on-line checkingi shale gas, described method comprises: utilize a High Temperature High Pressure probe to shale samples temperature-pressure to design temperature wherein and a setting pressure, described design temperature is 150 ~ 170 DEG C, and described setting pressure is 50 ~ 60MPa; Under described design temperature and described setting pressure, utilize a pulse train to carry out Nuclear Magnetic Resonance Measurement to described shale samples, the relaxation time T2 that inverting obtains described shale samples composes; The adsorbed gas saturation degree and free gas saturation degree that calculate described shale samples is composed according to described relaxation time T2.
In an embodiment, utilize a High Temperature High Pressure probe to shale samples temperature-pressure to design temperature wherein and a setting pressure, comprising: the clamper putting into described High Temperature High Pressure probe after being dried by described shale samples; Described High Temperature High Pressure probe is vacuumized; Described shale samples is forced into described setting pressure by the displacement assembly utilizing described High Temperature High Pressure to pop one's head in; Described shale samples is heated to described design temperature by the high-temperature heating assembly utilizing described High Temperature High Pressure to pop one's head in.
In an embodiment, under described design temperature and described setting pressure, utilize a pulse train to carry out Nuclear Magnetic Resonance Measurement to described shale samples, the relaxation time T2 that inverting obtains described shale samples composes, and comprising: according to described pulse train excited nucleus magnetic resonance excitation signal; Electric current driving and power amplification are carried out to described nuclear magnetic resonance pumping signal, the nuclear magnetic resonance pumping signal after generating process; Utilize the nuclear magnetic resonance pumping signal after described process, under described design temperature and described setting pressure, excite described shale samples, produce a nmr echo signal; Carry out inverting to described nmr echo signal to obtain described relaxation time T2 and compose.
In an embodiment, compose the adsorbed gas saturation degree and free gas saturation degree that calculate described shale samples according to described relaxation time T2, comprising: compose the cutoff calculating free state shale gas and ADSORPTION STATE shale gas according to described relaxation time T2; Described adsorbed gas saturation degree and described free gas saturation degree is calculated according to described cutoff.
In an embodiment, described method also comprises: according to the permeability of described shale samples arrange described relaxation time T2 compose in measuring intervals of TIME, to monitor the free state shale gas of described shale samples and ADSORPTION STATE shale gas.
In an embodiment, described high-temperature heating assembly comprises heating film, and described shale samples is heated to described design temperature by power consumption by described heating film.
The method of the nuclear magnetic resonance on-line checkingi shale gas of the embodiment of the present invention, by shale samples to be remained in high temperature and high pressure environment and to carry out detection shale gas, containing the situation of shale gas, the situation storing rock gas in accurate analysis stratum can be conducive in shale bed in analogue measurement stratum.The method of the nuclear magnetic resonance on-line checkingi shale gas of the embodiment of the present invention better can be evaluated the occurrence status of shale gas (methane gas) and obtain adsorbed gas, free gas saturation degree fast.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be 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 checkingi shale gas of the embodiment of the present invention;
Fig. 2 is the schematic flow sheet to the method for shale samples temperature-pressure in one embodiment of the invention;
Fig. 3 is the schematic flow sheet of the method for in one embodiment of the invention, shale samples being carried out to Nuclear Magnetic Resonance Measurement;
Fig. 4 is the schematic flow sheet calculating the adsorbed gas saturation degree of shale samples and the method for free gas saturation degree in one embodiment of the invention;
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 checkingi 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 High Temperature High Pressure probe in the embodiment of the present invention;
Fig. 9 is the curve map that in one embodiment of the invention, shale core 10MPa pressure saturated methane gas different time course relaxation time T2 composes;
Figure 10 is the curve map that the relaxation time T2 of different measuring time in one embodiment of the invention composes;
Figure 11 is the saturated methane gas free state of shale core 10MPa pressure, ADSORPTION STATE and resultant signal amount curve map over time in one embodiment of the invention.
Embodiment
For making the object of the embodiment of the present invention, technical scheme and advantage clearly understand, below in conjunction with accompanying drawing, the embodiment of the present invention is described in further details.At this, schematic description and description of the present invention is for explaining the present invention, but not as a limitation of the invention.
Fig. 1 is the schematic flow sheet of the method for the nuclear magnetic resonance on-line checkingi shale gas of the embodiment of the present invention.As shown in Figure 4, the method for the nuclear magnetic resonance on-line checkingi shale gas of the embodiment of the present invention, comprises step:
S101: utilize a High Temperature High Pressure probe to shale samples temperature-pressure to design temperature wherein and a setting pressure, described design temperature is 150 ~ 170 DEG C, and described setting pressure is 50 ~ 60MPa;
S102: under described design temperature and described setting pressure, utilize a pulse train to carry out Nuclear Magnetic Resonance Measurement to described shale samples, the relaxation time T2 that inverting obtains described shale samples composes;
S103: compose the adsorbed gas saturation degree and free gas saturation degree that calculate described shale samples according to described relaxation time T2.
The method of the nuclear magnetic resonance on-line checkingi shale gas of the embodiment of the present invention, by the high-temperature and high-pressure conditions in above-mentioned design temperature and setting pressure simulated formation, and detection shale gas is carried out to the shale samples remained in high temperature and high pressure environment, in analogue measurement stratum, shale bed is containing the situation of shale gas, is conducive to the situation storing rock gas in accurate analysis stratum.
Fig. 2 is the schematic flow sheet to the method for shale samples temperature-pressure in one embodiment of the invention.As shown in Figure 2, in above-mentioned steps S101, utilize a High Temperature High Pressure probe shale samples temperature-pressure to design temperature wherein and one to be set to the method for pressure, can step be comprised:
S201: the clamper putting into described High Temperature High Pressure probe after being dried by described shale samples;
S202: described High Temperature High Pressure probe is vacuumized;
S203: described shale samples is forced into described setting pressure by the displacement assembly utilizing described High Temperature High Pressure to pop one's head in;
S204: described shale samples is heated to described design temperature by the high-temperature heating assembly utilizing described High Temperature High Pressure to pop one's head in.
In above-mentioned steps S203, the scope of setting pressure is 50MPa ~ 60MPa or other are higher than atmospheric pressure values, can be 55MPa in a preferred embodiment, with the High Voltage in simulated formation; In above-mentioned steps S204, the scope of design temperature is 150 DEG C ~ 170 DEG C, can be 160 DEG C in a preferred embodiment, with the high-temperature in simulated formation.
Existing nuclear magnetic resonance technique, can only detect at normal temperatures and pressures, the signal of shale gas cannot be detected.And shale samples can be remained on high temperature and high pressure environment by the embodiment of the present invention displacement assembly of being popped one's head in by above-mentioned High Temperature High Pressure and high-temperature heating assembly, thus realize nuclear magnetic resonance on-line checkingi shale gas.
Fig. 3 is the schematic flow sheet of the method for in one embodiment of the invention, shale samples being carried out to Nuclear Magnetic Resonance Measurement.As shown in Figure 3, under described design temperature and described setting pressure, utilize a pulse train to carry out Nuclear Magnetic Resonance Measurement to described shale samples, the method that the relaxation time T2 that inverting obtains described shale samples composes, can step be comprised:
S301: according to described pulse train excited nucleus magnetic resonance excitation signal;
S302: electric current driving and power amplification are carried out to described nuclear magnetic resonance pumping signal, the nuclear magnetic resonance pumping signal after generating process;
S303: utilize the nuclear magnetic resonance pumping signal after described process, excites described shale samples, produces a nmr echo signal under described design temperature and described setting pressure;
S304: inverting is carried out to described nmr echo signal and obtains described relaxation time T2 and compose.
In the embodiment of the present invention, by exciting shale samples under high-temperature and high-pressure conditions, produce the nmr echo signal of wherein shale gas, to detect the shale gas in shale samples, can obtain and more meet the nmr echo signal containing shale gas actual conditions of shale bed in stratum.
Fig. 4 is the schematic flow sheet calculating the adsorbed gas saturation degree of shale samples and the method for free gas saturation degree in one embodiment of the invention.As shown in Figure 4, in the method for the nuclear magnetic resonance on-line checkingi shale gas shown in Fig. 1, compose according to described relaxation time T2 and calculate the adsorbed gas saturation degree of described shale samples and the method for free gas saturation degree, can step be comprised:
S401: compose the cutoff calculating free state shale gas and ADSORPTION STATE shale gas according to described relaxation time T2;
S402: calculate described adsorbed gas saturation degree and described free gas saturation degree according to described cutoff.
In the embodiment of the present invention, what pass through that surveyed relaxation time T2 spectrum calculates is free with absorption T2 cutoff, thus obtains adsorbed gas saturation degree and free gas saturation degree.Free and the absorption T2 cutoff that the embodiment of the present invention obtains and movable fluid with to fetter fluid T2 cutoff different because moveable gel includes mobile water saturation, oil saturation and gas saturation, but not free gas and adsorbed gas.In addition, compared with conventional gas, the maximum feature of shale gas there is adsorbed gas, but it is movable, minable, and can not realize the technical scheme obtaining its saturation degree for this movable adsorbed gas in prior art.
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, the method for the nuclear magnetic resonance on-line checkingi shale gas shown in Fig. 1, also can comprise step:
S104: according to the permeability of described shale samples arrange described relaxation time T2 compose in measuring intervals of TIME, to monitor the free state shale gas of described shale samples and ADSORPTION STATE shale gas.
In the embodiment of the present invention, by arranging measuring intervals of TIME, the relaxation time T2 of repetitive measurement shale samples composes, free state shale gas and ADSORPTION STATE shale gas situation over time in shale samples can be detected, effectively can embody the difference of methane mass transfer and hosting pattern in different scale hole, thus to obtain in abundanter analysis stratum shale bed containing the experimental basis of shale gas situation, for clear and definite methane gas hosting pattern and coupling mass transfer rule lay the foundation.
The method of the nuclear magnetic resonance on-line checkingi shale gas of the embodiment of the present invention can be realized by the system of following each embodiment or device or assembly.
Fig. 6 is the structural representation of the system of the nuclear magnetic resonance on-line checkingi shale gas of the embodiment of the present invention.As shown in Figure 6, the system of the nuclear magnetic resonance on-line checkingi shale gas that the method for nuclear magnetic resonance on-line checkingi shale gas is as shown in Figure 1 used, can comprise: detection system 100 and control system 200.
Detection system 100 can comprise full diameter magnet 110, High Temperature High Pressure probe 120, temperature control assembly 130.Full diameter magnet 110 is a closed cavity; High Temperature High Pressure probe 120 is located at the inside of described full diameter magnet, for placing a shale samples, and provides above-mentioned design temperature for this shale samples and sets pressure, with simulated formation environment; The outside surface of this full diameter magnet is located at by temperature control assembly 130, and for controlling at above-mentioned design temperature by the temperature of this full diameter magnet, this design temperature can be a steady temperature.
Control system 200 can comprise computing machine 201, master controller 202, frequency generator 203, power amplifier 204, T/R match circuit 205, prime amplifier 206, receiver 207, A/D converter 208.Computing machine 201 is for setting an experiment parameter; Master controller 202 is connected with computing machine 201, to produce a pulse train according to this experiment parameter; Frequency generator 203 is connected with master controller 202, carries out electric current driving with the nuclear magnetic resonance pumping signal excited this pulse train; Power amplifier 204 is connected with frequency generator 203, carries out signal amplification with the nuclear magnetic resonance pumping signal after driving electric current; One end of T/R match circuit 205 is connected with this power amplifier 204, the other end and this High Temperature High Pressure of T/R match circuit 205 are popped one's head in and 120 to be connected, to carry out sending the nuclear magnetic resonance pumping signal of amplifying through signal and the conversion received between a nmr echo signal; Prime amplifier 206 is connected with this T/R match circuit 205, to carry out signal amplification to this nmr echo signal; Receiver 207 is connected with this prime amplifier 206, the nmr echo signal after amplifying with collection signal; One end of A/D converter 208 is connected with this receiver 207, the other end of A/D converter 208 is connected with this master controller 202, A/D conversion is carried out to the nmr echo signal after amplifying, and the nmr echo signal after being changed by A/D is sent to this computing machine 201 by this master controller 202, to show the Nuclear Magnetic Resonance Measurement result of this shale samples on this computing machine 201.
In the system of above-mentioned nuclear magnetic resonance on-line checkingi shale gas, High Temperature High Pressure probe can to shale samples temperature-pressure to the 150 wherein DEG C ~ design temperature of 170 DEG C and the setting pressure of 50MPa ~ 60MPa, to realize on-line checkingi shale gas.
Fig. 7 is the structural representation of full diameter magnet in the embodiment of the present invention.As shown in Figure 7, in the system of the nuclear magnetic resonance on-line checkingi shale gas shown in Fig. 6, full diameter magnet 110 can comprise pole plate 111, magnet steel 112, threshold 113, yoke plate 114 and side yoke plate 115.
The two pieces of yoke plates 114 be oppositely arranged and the two pieces of side yoke plates 115 be oppositely arranged connect and compose a framework, successively to form a closed-loop path; Two blocks of magnet steel 112 are individually fixed in the relative inner side of two pieces of yoke plates 114, think that above-mentioned shale samples provides a magnetic field; Two pieces of pole plates 111 are individually fixed in the relative inner side of two blocks of magnet steel 112, to carry out carrying out magnetic conduction to this magnetic field; Two thresholds 113 embed the relative inner side of two pieces of pole plates 111 respectively.
In an embodiment, yoke plate 114 is dull and stereotyped, and length is between 560 ~ 600mm, and width is between 400 ~ 550mm, and thickness is between 10 ~ 20mm.Side yoke plate 115 is dull and stereotyped, and length is between 400 ~ 550mm, and width is between 300 ~ 450mm, and thickness is between 10 ~ 20mm.Two pieces of side yoke plates 115 and two pieces of yoke plates 114 form a framework, for magnet forms a closed-loop path.One block of magnet steel 112 is fixed respectively at the relative medial surface of two pieces of yoke plates 114.The length of magnet steel 112 is between 460 ~ 500mm, and width is between 300 ~ 450mm, and thickness is between 10 ~ 20mm.Magnet steel 112 is as magnetic source.The relative plane of magnet steel is fixed with piece of pole plate 111 respectively.The length of pole plate 111 is between 480 ~ 520mm, and width is between 320 ~ 470mm, and thickness is between 10 ~ 20mm.Pole plate 111 plays magnetic conduction effect.Full diameter magnet 110 outside surface is one group of temperature control assembly 130, can carry out 10 ~ 60 degree of thermostatic controls to full diameter magnet 110, reduces temperature to the impact of apparatus measures result.
Fig. 8 is the structural representation of High Temperature High Pressure probe in the embodiment of the present invention.As shown in Figure 8, the High Temperature High Pressure probe 120 in said system can comprise ring pressure assembly, high-temperature heating assembly, displacement assembly and nuclear magnetic resonance assembly.
Ring pressure assembly can comprise the clamper cavity 1212 that an end cover 1211 is fixed at two ends respectively, to apply ring pressure to shale samples 1213, also can comprise ring and compress into oil pipe 1214 and Huan Ya oil discharge pipe 1215.
High-temperature heating assembly can comprise is located at spiral heat-conducting oil pipes 1221 outside clamper cavity 1212 and lagging casing 1222, from inside to outside successively to heat this shale samples 1213.
Displacement assembly can comprise displacement flowline 1234, second seal 1235, the second shale samples top 1236 that the first shale samples connected successively comes directly towards the 1231, first seal 1232, displacement oil inlet pipe 1233 and connects successively, displacement oil inlet pipe 1218 and displacement flowline 1219 are also connected with the end cover 1211 at clamper cavity 1212 two ends respectively, to carry out displacement test to this shale samples 1213.
This nuclear magnetic resonance assembly can comprise the nuclear magnetic resonance skeleton 1241 that outside surface is wound with malcoils and the extraction joint 1242 be connected with described malcoils, and this nuclear magnetic resonance skeleton 1241 is located at the inside of this clamper cavity 1212, with receive through signal amplify above-mentioned nuclear magnetic resonance pumping signal and launch described nmr echo signal.
During the method for nuclear magnetic resonance on-line checkingi shale gas of the present invention, high-temperature heating assembly wherein, can substitute above-mentioned spiral heat-conducting oil pipes 1221 by heating film, heating film produces heat by power consumption thus makes clamper inside produce high temperature, system can be made succinct, easy to operate with this.
In an embodiment, again as shown in Figure 8, this High Temperature High Pressure probe 120, with between this T/R match circuit 205, be all connected by cable between this T/R match circuit 205 with this power amplifier 204, between this T/R match circuit 205 with this prime amplifier 206, between this power amplifier 204 with this frequency generator 203, between this frequency generator 203 with this master controller 202, between this receiver 207 with this A/D converter 208, is connected by USB interface between this master controller 202 with this computing machine 201.
In an embodiment, this A/D converter 208 can carry out buffer memory to the echoed signal of described collection; The scope of above-mentioned setting steady temperature can be [10 degree, 60 degree]; Above-mentioned echoed signal can be amplified 70DB by this prime amplifier 206.
Shale gas magnetic resonance detection device of the present invention, owing to have employed High Temperature High Pressure probe and the design of major diameter uniform field, can under high-temperature and high-pressure conditions, carry out nuclear magnetic resonance on-line testing, the relaxation time T2 obtaining one dimension composes, Quick Measurement free state gas saturation and ADSORPTION STATE gas saturation, can better Real-Time Evaluation shale reservoir and identify shale gas occurrence status.Simultaneously, nuclear magnetic resonance on-line checkingi shale gas measurement mechanism can the saturated methane gas of high pressure, by the change that T2 composes, effectively can embody the difference of shale gas (such as methane) mass transfer and hosting pattern in different scale hole, for clear and definite shale gas (methane gas) hosting pattern and coupling mass transfer rule lay the foundation.
The method of nuclear magnetic resonance on-line checkingi shale gas according to an embodiment of the invention, carries out nuclear magnetic resonance on-line checkingi to the shale samples containing methane gas.Utilize CPMG pulse train to measure shale samples, inverting obtains relaxation time T2 and composes.According to the permeability of shale, the interval time of measurement is set, reaches the object of monitoring.Table 1 display measurement time and corresponding cpmg sequence row measurement parameter.
Table 1
| Which sky | 2 | 4 | 8 | 10 | 13 | 16 | 20 | 26 | 31 | 37 |
| Tau(us) | 150 | 150 | 150 | 150 | 150 | 150 | 150 | 150 | 150 | 150 |
| NECH (individual) | 2048 | 2048 | 2048 | 2048 | 2048 | 2048 | 2048 | 2048 | 2048 | 2048 |
| NS (secondary) | 512 | 512 | 512 | 512 | 512 | 512 | 512 | 512 | 512 | 512 |
| RD(ms) | 3000 | 3000 | 3000 | 3000 | 3000 | 3000 | 3000 | 3000 | 3000 | 3000 |
Fig. 9 is the curve map that in one embodiment of the invention, shale core 10MPa pressure saturated methane gas different time course relaxation time T2 composes.As shown in Figure 9, relaxation time T2 spectrum is mainly distributed between 0.3ms ~ 20ms, and along with the increase of time, T2 spectrum constantly moves left and right.Relaxation time T2 spectrum is moved to the left and represents that gas enters fine porosity or is adsorbed onto organic surface.Relaxation time T2 spectrum moves right mainly because shale core permeability is very low, methane gas is subject to the restriction of pore throat, be difficult to enter fast in hole, in hole, methane gas pressure is lower, the intrapore methane gas of increase along with the time constantly increases, pressure is caused to increase, so the relaxation time T2 spectrum of saturated methane can move to right in shale core.
Figure 10 is the curve map that the relaxation time T2 of different measuring time in one embodiment of the invention composes.As shown in Figure 10.When shale core by methane gas abundant saturated time, relaxation time T2 composes existence two peaks, and therefore, a peak is the methane gas of free state, another peak is the methane gas of ADSORPTION STATE, determines that the ADSORPTION STATE of this block shale core and free state T2 cutoff are 1.3ms.Adsorbed gas saturation degree is 37.3%, and free gas saturation degree is 62.7%.
Figure 11 is the saturated methane gas free state of shale core 10MPa pressure, ADSORPTION STATE and resultant signal amount curve map over time in one embodiment of the invention.As shown in figure 11, methane gas enters after in shale, and starting stage free gas gathers way comparatively fast, and methane gas is mainly present in shale hole with free state form, this is because methane gas pressure is less in starting stage hole, is unfavorable for absorption.Interstage adsorbed gas gathers way comparatively fast, and free gas gathers way slack-off, and mainly because methane gas pressure in hole increases gradually, and methane gas progresses into the more organic surface contact of more hole, and adsorption rate is accelerated.Terminal stage free gas gathers way and slows down, and adsorbed gas gathers way slack-off, reaches pressure equilibrium gradually.
The method of the nuclear magnetic resonance on-line checkingi shale gas of the embodiment of the present invention, by shale samples to be remained in high temperature and high pressure environment and to carry out detection shale gas, containing the situation of shale gas, the situation storing rock gas in accurate analysis stratum can be conducive in shale bed in analogue measurement stratum.The method of the nuclear magnetic resonance on-line checkingi shale gas of the embodiment of the present invention better can be evaluated the occurrence status of shale gas (methane gas) and obtain adsorbed gas, free gas saturation degree fast.
Above-described specific embodiment; object of the present invention, technical scheme and beneficial effect are further described; be understood that; the foregoing is only specific embodiments of the invention; the protection domain be not intended to limit the present invention; within the spirit and principles in the present invention all, any amendment made, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (6)
1. a method for nuclear magnetic resonance on-line checkingi shale gas, is characterized in that, described method comprises:
Utilize a High Temperature High Pressure probe to shale samples temperature-pressure to design temperature wherein and a setting pressure, described design temperature is 150 ~ 170 DEG C, and described setting pressure is 50 ~ 60MPa;
Under described design temperature and described setting pressure, utilize a pulse train to carry out Nuclear Magnetic Resonance Measurement to described shale samples, the relaxation time T2 that inverting obtains described shale samples composes;
The adsorbed gas saturation degree and free gas saturation degree that calculate described shale samples is composed according to described relaxation time T2.
2. the method for nuclear magnetic resonance on-line checkingi shale gas as claimed in claim 1, is characterized in that, utilizes a High Temperature High Pressure probe to shale samples temperature-pressure to design temperature wherein and a setting pressure, comprising:
The clamper of described High Temperature High Pressure probe is put into after being dried by described shale samples;
Described High Temperature High Pressure probe is vacuumized;
Described shale samples is forced into described setting pressure by the displacement assembly utilizing described High Temperature High Pressure to pop one's head in;
Described shale samples is heated to described design temperature by the high-temperature heating assembly utilizing described High Temperature High Pressure to pop one's head in.
3. the method for nuclear magnetic resonance on-line checkingi shale gas as claimed in claim 1, it is characterized in that, under described design temperature and described setting pressure, utilize a pulse train to carry out Nuclear Magnetic Resonance Measurement to described shale samples, the relaxation time T2 that inverting obtains described shale samples composes, and comprising:
According to described pulse train excited nucleus magnetic resonance excitation signal;
Electric current driving and power amplification are carried out to described nuclear magnetic resonance pumping signal, the nuclear magnetic resonance pumping signal after generating process;
Utilize the nuclear magnetic resonance pumping signal after described process, under described design temperature and described setting pressure, excite described shale samples, produce a nmr echo signal;
Carry out inverting to described nmr echo signal to obtain described relaxation time T2 and compose.
4. the method for nuclear magnetic resonance on-line checkingi shale gas as claimed in claim 1, is characterized in that, composes the adsorbed gas saturation degree and free gas saturation degree that calculate described shale samples, comprising according to described relaxation time T2:
The cutoff calculating free state shale gas and ADSORPTION STATE shale gas is composed according to described relaxation time T2;
Described adsorbed gas saturation degree and described free gas saturation degree is calculated according to described cutoff.
5. the method for nuclear magnetic resonance on-line checkingi shale gas as claimed in claim 1, is characterized in that, also comprise:
According to the permeability of described shale samples arrange described relaxation time T2 compose in measuring intervals of TIME, to monitor the free state shale gas of described shale samples and ADSORPTION STATE shale gas.
6. the method for nuclear magnetic resonance on-line checkingi shale gas as claimed in claim 2, it is characterized in that, described high-temperature heating assembly comprises heating film, and described shale samples is heated to described design temperature by power consumption by described heating film.
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