CN109655371A - A kind of experiment analytical method of raw coal adsorbed gas characteristic - Google Patents

A kind of experiment analytical method of raw coal adsorbed gas characteristic Download PDF

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Publication number
CN109655371A
CN109655371A CN201710942899.2A CN201710942899A CN109655371A CN 109655371 A CN109655371 A CN 109655371A CN 201710942899 A CN201710942899 A CN 201710942899A CN 109655371 A CN109655371 A CN 109655371A
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cylinder
pressure
sample
adsorption
raw coal
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李呈呈
张克非
马中高
周枫
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China Petroleum and Chemical Corp
Sinopec Geophysical Research Institute
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China Petroleum and Chemical Corp
Sinopec Geophysical Research Institute
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N7/00Analysing materials by measuring the pressure or volume of a gas or vapour
    • G01N7/02Analysing materials by measuring the pressure or volume of a gas or vapour by absorption, adsorption, or combustion of components and measurement of the change in pressure or volume of the remainder
    • G01N7/04Analysing materials by measuring the pressure or volume of a gas or vapour by absorption, adsorption, or combustion of components and measurement of the change in pressure or volume of the remainder by absorption or adsorption alone

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Abstract

The invention proposes a kind of experiment analytical methods of raw coal adsorbed gas characteristic, this method comprises: carrying out continuous adsorption test by the way of pressurizeing step by step;Measure adsorbance;Determine the adsorption saturation period of sample.The continuous adsorption test includes: to be filled with methane gas, pressure of the record referring to cylinder to referring to cylinder;Connection writes down the pressure of reference cylinder and sample cylinder after balance referring to cylinder and sample cylinder;Experimental pressure is successively improved by the way of pressurizeing step by step, repeats above-mentioned two step, until reaching the pressure of requirement of experiment.This method is the development raw coal isothermal adsorption under the Temperature-pressure Conditions of stratum, closer to coal seam actual conditions.This provides theoretical basis to carry out coal bed gas prediction using geophysical method.

Description

A kind of experiment analytical method of raw coal adsorbed gas characteristic
Technical field
The invention belongs to rock physics research fields, and the present invention relates to three axis simulating test device of coal bed gas, absorption to measure Amount and isothermal adsorption, in particular to a kind of experiment analytical method of raw coal adsorbed gas characteristic.
Background technique
Coal-bed gas content is an important indicator in coal bed gas industry.The air content difference of coal petrography can cause coal petrography speed Decline.The air content of coal bed gas is by temperature, pressure, coal rank, lithotype of coal, coal petrography macroscopic view component and coal petrography under normal conditions Equilibrium water conten etc. influence.In fact, the maximum value of coal-bed gas content is the suction of coal seam under this condition under certain condition Attached ability, that is to say, that the adsorption capacity of coalbed methane reservoir is also influenced by above-mentioned condition and restriction.
But at home and abroad what is be more concerned about at present in disclosed document is the characterization of adsorption of powdery coal sample, it is (blocky to raw coal Coal sample) characterization of adsorption research it is less.The adsorption isotherm experiment of existing coal is carried out in the case where powdery coal sample.It is opposite and Speech, this method coal are easy to reach adsorption saturation state.For raw coal (lump coal) absorption closer to coal seam actual conditions, no It crosses, the research of raw coal adsorption isotherm experiment is few, needs how long to reach adsorption saturation and knows together not yet, this just needs to carry out phase It tests to study the gas absorption characteristic of blocky coal sample pass.
Summary of the invention
The present invention provides a kind of experiment analytical methods of raw coal adsorbed gas characteristic.Carry out under different adsorptive pressures first The testing research of adsorbance test measurement, the number that pressurizes;Then pass through the continuous adsorption test under isothermal different pressures, research The relationship of coal petrography adsorbance and adsorption time, the final period for determining coal sample adsorption saturation.
According to an aspect of the present invention, a kind of experiment analytical method of raw coal adsorbed gas characteristic, this method packet are provided It includes:
Continuous adsorption test is carried out by the way of pressurizeing step by step;
Measure adsorbance;
Determine the adsorption saturation period of sample.
Further, the continuous adsorption test includes:
Methane gas, pressure of the record referring to cylinder are filled with to referring to cylinder;
Connection writes down the pressure of reference cylinder and sample cylinder after balance referring to cylinder and sample cylinder;
Experimental pressure is successively improved by the way of pressurizeing step by step, repeats above-mentioned two step, until reaching requirement of experiment Pressure.
Further, the measurement adsorbance includes:
Gas and adsorbent are put together in simulation system, after reaching balance, by comparing the gas of absorption front and back Pressure measures adsorbance.
It further, to before being filled with methane gas referring to cylinder, will include existing referring to cylinder and sample cylinder and connecting pipeline Interior adsorption system vacuumizes, and sets system temperature.
Further, high-pressure cylinder methane gas is made to be filled with methane gas to referring to cylinder.
Further, the purity of the methane gas is greater than 99.99%.
Further, the system pumpdown time is 20~30 minutes.
Further, the adsorption saturation period of the determining sample includes:
Record sample reaches the time required for adsorption saturation at various pressures, to determine the adsorption saturation week of sample Phase.
Further, before the continuous adsorption test, coal sample is prepared first, coal sample is packed into sample cylinder, and carry out Airtight test.
Further, before the continuous adsorption test, it is first determined confining pressure, temperature and the highest test pressure of coal sample Power;
Adsorption equilibrium simultaneously, acquire adsorption time, pressure and temperature.
The present invention provides a kind of experiment analytical methods of raw coal adsorbed gas characteristic.This method is in stratum Temperature-pressure Conditions Lower development raw coal isothermal adsorption, closer to coal seam actual conditions.This is provided to carry out coal bed gas prediction using geophysical method Theoretical basis.
Detailed description of the invention
Disclosure illustrative embodiments are described in more detail in conjunction with the accompanying drawings, the disclosure above-mentioned and its Its purpose, feature and advantage will be apparent, wherein in disclosure illustrative embodiments, identical reference label Typically represent same parts.
Fig. 1 shows the flow chart of coal petrography adsorbed gas.
Fig. 2 shows gas pressures with the change curve of adsorption time.
Fig. 3 shows gas pressure with the change curve of adsorption time.
Fig. 4 shows gas pressure with the change curve of adsorption time.
Fig. 5 is shown under low-pressure state, gas pressure with adsorption time change curve.
Fig. 6 is shown under elevated pressures state, gas pressure with adsorption time change curve.
Fig. 7 is shown under high pressure conditions, gas pressure with adsorption time change curve.
Specific embodiment
The preferred embodiment of the disclosure is more fully described below with reference to accompanying drawings.Although showing the disclosure in attached drawing Preferred embodiment, however, it is to be appreciated that may be realized in various forms the disclosure without the embodiment party that should be illustrated here Formula is limited.On the contrary, these embodiments are provided so that this disclosure will be more thorough and complete, and can be by the disclosure Range is completely communicated to those skilled in the art.
Coal bed gas is largely stored in coal with adsorption form, is carried out further investigation to the adsorpting characteristic of coal and is even more important. Most of researchs at present are the isothermal adsorption tests carried out based on powdery coal sample, lack the reality that raw coal adsorbs under the Temperature-pressure Conditions of stratum Test data.
The present invention provides a kind of experiment analytical methods of raw coal adsorbed gas characteristic, and this method is under the Temperature-pressure Conditions of stratum The relationship for studying coal petrography adsorbance and adsorption time, closer to coal seam actual conditions.This is to carry out coal using geophysical method The gas distribution prediction of layer provides theoretical basis.
The present invention provides a kind of experiment analytical methods of raw coal adsorbed gas characteristic, this method comprises:
Continuous adsorption test is carried out by the way of pressurizeing step by step;
Measure adsorbance;
Determine the adsorption saturation period of sample.
Further, the continuous adsorption test includes:
Methane gas, pressure of the record referring to cylinder are filled with to referring to cylinder;
Connection writes down the pressure of reference cylinder and sample cylinder after balance referring to cylinder and sample cylinder;
Experimental pressure is successively improved by the way of pressurizeing step by step, repeats above-mentioned two step, until reaching requirement of experiment Pressure.
It is easy to be crushed since coal sample carries out isothermal adsorption under the Temperature-pressure Conditions of stratum, this is just needed during the test Adsorption test is carried out by the way of gradually increasing pressure and testing pressure to highest.
Carry out continuous adsorption test include: will be including referring to cylinder and sample cylinder (equipped with coal sample) and connecting pipeline Adsorption system vacuumizes 20~30min, sets system temperature;It opens charge valve and referring to cylinder control valve, makes high-pressure cylinder methane Gas (purity > 99.99%) enters referring to cylinder, closes charge valve, and records the pressure P1 referring to cylinder;Balanced valve is slowly opened, Connection writes down the pressure after balancing referring to cylinder and sample cylinder from expanding referring to cylinder to sample cylinder referring to cylinder and sample cylinder, methane gas P2.Experimental pressure is successively improved by the way of gradually increasing pressure and testing pressure to highest, until reaching the pressure of requirement of experiment Power.
Next estimation adsorbance.For example, can adopt in the following method, the absorption in adsorption test of the present invention is estimated Amount.
Gas and adsorbent are put together in the simulation system of three axis simulating test device of coal bed gas, after reaching balance Compare absorption front and back gas pressure again to measure adsorbance.Three axis simulating test device of coal bed gas is simulated by displacement system, stratum 5 systems such as data collection systems, data processing system, the auxiliary systems such as system, sound wave, foil gauge instrument, grease automatic gauge Composition.The device is the prior art, and details are not described herein again for particular content.
Finally, record sample reaches the time required for adsorption saturation at various pressures, to determine the absorption of sample It is saturated the period.
As shown in Figure 1, the experiment analytical method of one embodiment of the present invention, first before the continuous adsorption test Coal sample is first prepared, coal sample is packed into sample cylinder, and carry out airtight test;
Then determine that the confining pressure, temperature and highest of coal sample test pressure;
Next carry out continuous adsorption test, determine test pressure spot, be inflated to goal pressure;
Adsorption equilibrium simultaneously, acquire adsorption time, the pressure and temperature of sample;
Experimental pressure is successively improved, until reaching the pressure of requirement of experiment.
A concrete application example is given below in the scheme and its effect of the embodiment of the present invention for ease of understanding.This field It should be understood to the one skilled in the art that the example is only for the purposes of understanding the present invention, any detail is not intended to be limited in any way The system present invention.
This method is applied to actual coal bed gas work area.For coal petrography sample 10#0508, experimental temperature is arranged for we Be 30 DEG C, highest test pressure is set as 5MPa, and sets pressurization number to 4 times, pressure be respectively 2MPa, 3MPa, 4MPa, 5MPa.Meanwhile we have recorded coal petrography under each pressure spot and reach the time required for adsorption saturation, to determine the suction of coal petrography The attached saturation period, as shown in Figure 2.
For sample 10#0507, experimental temperature is set 30 DEG C by we, and highest test pressure is set as 6MPa, and will Pressurization number is set as 4 times, and pressure is respectively 1.5MPa, 3MPa, 5MPa, 6MPa.Meanwhile we have recorded under each pressure spot Coal petrography reaches the time required for adsorption saturation, to determine the adsorption saturation period of coal petrography, as shown in Figure 3.
For sample 10#0513, experimental temperature is set 30 DEG C by we, and highest test pressure is set as 8MPa, and will Pressurization number is set as 4 times, and pressure is respectively 2MPa, 4MPa, 6MPa, 8MPa.Meanwhile we have recorded coal under each pressure spot Rock reaches the time required for adsorption saturation, to determine the adsorption saturation period of coal petrography, as shown in Figure 4.
When Fig. 5 to Fig. 7 draws the gas pressure under the low pressure of three samples, mesohigh, high pressure conditions with absorption respectively Between change curve study the adsorption saturation period under different pressures state.
It can be seen from the figure that coal sample reaches adsorption saturation needs 24 hours or more under low-pressure state;Elevated pressures state Under, coal sample reaches adsorption saturation needs 40 hours or more;Under high pressure conditions, coal sample reaches adsorption saturation needs 50 hours or more. Simultaneously it can also be seen that with gas pressure increase, coal sample reach the time required for adsorption saturation be present increase become Gesture.
The presently disclosed embodiments is described above, above description is exemplary, and non-exclusive, and It is not limited to disclosed each embodiment.Without departing from the scope and spirit of illustrated each embodiment, for this skill Many modifications and changes are obvious for the those of ordinary skill in art field.The selection of term used herein, purport In principle, the practical application or to the technological improvement in market for best explaining each embodiment, or make the art its Its those of ordinary skill can understand each embodiment disclosed herein.

Claims (10)

1. a kind of experiment analytical method of raw coal adsorbed gas characteristic, which is characterized in that this method comprises:
Continuous adsorption test is carried out by the way of pressurizeing step by step;
Measure adsorbance;
Determine the adsorption saturation period of sample.
2. the experiment analytical method of raw coal adsorbed gas characteristic according to claim 1, which is characterized in that the continuous suction Adhesion test includes:
Methane gas, pressure of the record referring to cylinder are filled with to referring to cylinder;
Connection writes down the pressure of reference cylinder and sample cylinder after balance referring to cylinder and sample cylinder;
Experimental pressure is successively improved by the way of pressurizeing step by step, repeats above-mentioned two step, until reaching the pressure of requirement of experiment.
3. the experiment analytical method of raw coal adsorbed gas characteristic according to claim 1, which is characterized in that the measurement is inhaled Attached amount includes:
Gas and adsorbent are put together in simulation system, after reaching balance, by comparing the gas pressure of absorption front and back To measure adsorbance.
4. the experiment analytical method of raw coal adsorbed gas characteristic according to claim 2, which is characterized in that referring to cylinder It is filled with before methane gas, by including being vacuumized referring to the adsorption system including cylinder and sample cylinder and connecting pipeline, and sets and be System temperature.
5. the experiment analytical method of raw coal adsorbed gas characteristic according to claim 2, which is characterized in that make high-pressure cylinder Methane gas is filled with methane gas to referring to cylinder.
6. the experiment analytical method of raw coal adsorbed gas characteristic according to claim 5, which is characterized in that the methane gas Purity be greater than 99.99%.
7. the experiment analytical method of raw coal adsorbed gas characteristic according to claim 4, which is characterized in that system vacuumizes Time is 20~30 minutes.
8. the experiment analytical method of raw coal adsorbed gas characteristic according to claim 1, which is characterized in that the determining sample The adsorption saturation period of product includes:
Record sample reaches the time required for adsorption saturation at various pressures, to determine the adsorption saturation period of sample.
9. the experiment analytical method of raw coal adsorbed gas characteristic according to claim 1, which is characterized in that described continuous Before adsorption test, coal sample is prepared first, coal sample is packed into sample cylinder, and carry out airtight test.
10. the experiment analytical method of raw coal adsorbed gas characteristic according to claim 1, which is characterized in that in the company Before continuous adsorption test, it is first determined confining pressure, temperature and the highest of coal sample test pressure;
While adsorption equilibrium, adsorption time, the pressure and temperature of sample are acquired.
CN201710942899.2A 2017-10-11 2017-10-11 A kind of experiment analytical method of raw coal adsorbed gas characteristic Pending CN109655371A (en)

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