CN101975718A - Method for simultaneously measuring high-pressure gas adsorption capacity and adsorption swell capacity of coal petrography and measuring equipment - Google Patents

Method for simultaneously measuring high-pressure gas adsorption capacity and adsorption swell capacity of coal petrography and measuring equipment Download PDF

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CN101975718A
CN101975718A CN 201010255937 CN201010255937A CN101975718A CN 101975718 A CN101975718 A CN 101975718A CN 201010255937 CN201010255937 CN 201010255937 CN 201010255937 A CN201010255937 A CN 201010255937A CN 101975718 A CN101975718 A CN 101975718A
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pressure
container
unit
pot test
expression
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CN101975718B (en
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刘增厚
杨建丽
陈国青
刘振宇
李允梅
刘平光
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中国科学院山西煤炭化学研究所
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Abstract

The invention provides a method for simultaneously measuring high-pressure gas absorption capacity and adsorption sell capacity of coal petrography and measuring equipment, which can simultaneously measure the adsorption capacity and adsorption swell capacity of the coal petrography in high-pressure gas at a pressure of 0-20MPa and a temperature of 0-80 DEG C. In the process of measurement, a measurement and control device is used for performing signal transformation and analog-to-digital conversion on electrical signals of a displacement sensor, a temperature-measuring hot resistor and a pressure transmitter; a computer is used for automatically receiving pressure, temperature and displacement signal data from the measurement and control device and recording and saving the received data; and a computer screen is used for displaying the pressure, temperature, adsorption capacity and swell capacity data timely in the process of measurement and the change law curves of the pressure, the temperature and the swell capacity with the change of time in real time. In the method of the invention, the measurement on the adsorption capacity and the adsorption swell capacity can be finished simultaneously, so that the method is simple and convenient and fast, and has the advantages of simple structure, reliable and safe high-pressure seal, easy operation, high measurement accuracy, high resistance to pressure and automatic measurement.

Description

Coal petrography gases at high pressure adsorbance and simultaneously-measured method of adsorption swelling amount and measurement mechanism
Technical field
The invention belongs to a kind of method and measurement mechanism that coal petrography gases at high pressure adsorbance and adsorption swelling amount are measured simultaneously.
Background technology
Coal and rock is a kind of porous medium that contains a large amount of absorption coal-seam gas, and its mechanical property has material impact to coal-bed gas exploitation.The hole characteristic of coal and coal seam reservoirs, adsorption-desorption feature and geology control mechanism thereof are the coal seam aerospheres always, the popular problem that geology circle is concerned about.The adsorbability of coal is to estimate the important foundation of coal seam gas-bearing property and coal-seam gas recoverability, to the understanding of coal-seam gas adsorption/desorption feature, has a deep effect on coal-seam gas and can adopt RESERVE EVALUATION, coal seam reservoirs production capacity numerical simulation.Overcritical kinetics of adsorption model of coal-seam gas and mechanism can be preferred coal-seam gas favourable district band and development coal-bed gas exploitation technology provides direct scientific basis.So, the structure of coal petrography and the further investigation of absorption property and adsorption swelling distortion thereof are had crucial meaning.
Studies have shown that matrix of coal absorption N in a large number 2, CH 4, CO 2Gas will produce dilatational strain, and gas desorption can make matrix of coal shrink.
In recent years, along with people to CO 2Improving constantly of technical concerns degree such as seal up for safekeeping in the coal seam, coal-seam gas gas injecting mining (mainly is CO about coal petrography to gas with various 2, N 2, CH 4Deng) the research of adsorptive power (adsorbance, absorption distortion and the infiltration coefficient that causes thus change) more and more be subject to people's attention, the research coal petrography is under high pressure to the adsorption swelling deformation rule of gas with various, and the relation of adsorbance and coal and rock adsorption swelling rate is significant for the seepage characteristic of gas in the research coal seam and coal bed gas resource evaluation and work of exploration and development.Particularly study coal petrography to gas with various (as CO 2, N 2, CH 4Deng) adsorbance, the distortion that causes of absorption and infiltration coefficient thereof change, to understanding CO 2The mechanism of technology such as seal up for safekeeping in the coal seam, coal-seam gas gas injecting mining is significant equally.
For many years, people are carrying out a large amount of research aspect coal petrography absorption and the absorption deformation measurement, have also developed the technology and the device of the distortion that many test coal petrography adsorbances and absorption causes.In this respect, adsorbance method of testing and technology are more, and static method and dynamic method are arranged, and using more is static method.The high pressure adsorbance measuring technology of coal mainly contains volumetric method and gravimetric method high pressure determining adsorption method, and all there is application these two kinds of method countries in the world.And volumetric method is traditional classical way, uses more.Aspect the absorption distortion expansion of measurement coal petrography in gases at high pressure, external researchist mainly adopts optical measuring method and foil gauge mensuration at present.The report of domestic relevant this respect research work is less, employing also be the foil gauge mensuration.The foil gauge mensuration is pasted on the coal cinder surface with resistance strain gage with cementing agent exactly, and the expansion of coal cinder causes the resistance value of foil gauge to change.Obtain the swell increment of coal by the variation of measured resistance value.The precision of foil gauge mensuration is higher, but this method needs special resistance strain gage and cementing agent, and complicated operating process is to having relatively high expectations of operating personnel.Supercritical CO particularly 2Chemical action takes place in gas and cementing agent easily, thereby causes measurement result distortion or failure.Optical measuring method utilizes camera or microscope by a high pressure resistant transparent glass window coal sample to be taken pictures exactly, utilizes image analysis software that the photo of gained is analyzed then, thereby calculates the swell increment of producing coal.But this method institute use equipment complexity, cost is higher, and measuring accuracy is lower.
Because coal is a kind of porous crack heterogeneity object, all coal samples all have the pore volume distribution characteristics of various ways, and the pore volume of single coal lithotypes distributes and adsorpting characteristic is also had nothing in common with each other.There is test result to show. the adsorbance of identical rank coal changes within the specific limits, same mine same coal seam, it is close that the adsorbance of coal can only reach.
And above these measuring techniques and apparatus features are, can only measure adsorbance or can only measure deflection.In these measuring methods, the adsorbance test adopts powder coal sample or packaged coal sample as test specimen usually, adsorption swelling measures examination and then adopts packaged coal sample as test specimen, is not same coal sample because adsorbance and adsorption swelling measure that pilot production uses, also can't measure simultaneously.Thus, the adsorbance of measurement and adsorption swelling distortion can not be well corresponding, and the adsorbance of coal petrography, absorption distortion actual value differ bigger under the adsorbance of measurement, absorption distortion and the original place condition.
Measure difficulty of adsorbance and absorption deformation ratio on a sample simultaneously, the report of therefore relevant this respect work is less.At present, also there are not to find on a sample, to measure simultaneously adsorbance and the device of absorption distortion expansion and the relevant report of measuring method.
Summary of the invention
The purpose of this invention is to provide a kind of method and measurement mechanism that coal petrography gases at high pressure adsorbance and adsorption swelling amount are measured simultaneously.
Measuring method concrete operations step of the present invention is as follows:
(1) preparation of test coal petrography sample:
At first coal petrography to be measured is processed into the bulk sample of column type or rectangular build, and guarantees that coal petrography sample upper and lower end face is parallel and smooth, as required the coal petrography sample is carried out equilibrium moisture then and handle or dried, accurately measure the height L of coal petrography sample 0, and accurately take by weighing the weight G of coal petrography sample 0
(2) installation of test coal petrography sample:
At first open the measuring and controlling instrument power supply, start computing machine and operation;
With pack into the sample tube of measurement mechanism of coal petrography sample, the bottom of sample tube with the upper cylinder body of Hi-pot test container is connected, by regulating the position of sample tube, guarantee that the coal petrography sample reliably contacts with the displacement transducer measuring staff that is contained in upper cylinder body; Observe the displacement data that shows on measuring and controlling instrument or the computer screen simultaneously, accurately regulate the zero point of displacement transducer, with stay the bottom and the sample tube of upper cylinder body are fixed, then the sample wound packages is gone into the lower cylinder body of Hi-pot test container, be tightly connected with the upper cylinder body and the lower cylinder body of cutting ferrule with the Hi-pot test container;
(3) work is prepared before the test:
According to experimental program, set the temperature required T of experiment, start and add heat control, thermostatic bath is heated, when treating that the thermostatic bath temperature arrives design temperature T, start vacuum pump and extract high pressure reference container and Hi-pot test container and measuring system inner air, make high pressure reference container and Hi-pot test container and measuring system inside be in vacuum state, stop vacuum pump then, closeall valve;
(4) free space volumes is measured:
Free space volumes is meant the summation of the volume of Hi-pot test container loading coal rock sample product back coal petrography sample interior fine voids, the remaining free space of Hi-pot test container, associated line inner space, helium (H e) be a kind of not adsorbed gas, measure the free space volumes of Hi-pot test container to the expansion of Hi-pot test container from the high pressure reference container by helium;
Open high-pressure helium (H e) valve, in system, charge into helium, open air intake valve, to the helium that the high pressure reference container charges into, regulate high pressure reference container pressure to goal pressure, close gas admittance valve then, treat after the pressure stability record high pressure reference container this moment internal pressure P 2With Hi-pot test container internal pressure P 3, open the compensation flap between high pressure reference container and the Hi-pot test container, make helium enter the Hi-pot test container from the high pressure reference container, treat high pressure reference container and Hi-pot test container internal pressure stable equilibrium after, record this moment pressure P 1, obtain one group of data T, P this moment 1, P 2, P 3, calculate the volume V that places the Hi-pot test internal tank free space behind the sample by following formula F
The free space volumes computing formula is:
V F＝V R(ρ R0-ρ R1)/(ρ F1-ρ F0) ——(1)
Wherein: ρ R0=f (T, P 2) ρ F0=f (T, P 3)
ρ R1＝ρ F1＝f(T，P 1)
In the formula:
V F: expression free space volumes, unit are cubic centimetre (cm 3);
V R: expression high pressure reference container volume (known), unit are cubic centimetre (cm 3);
P 1: pressure after the expression balance, unit is MPa (MPa);
P 2: expression high pressure reference container original pressure, unit is MPa (MPa);
P 3: expression Hi-pot test container original pressure, unit is MPa (MPa);
T: the expression experimental temperature, unit is (K);
ρ R0: expression high pressure reference container initial gas density, unit is every cubic centimetre of (mmol/cm of mM 3);
ρ F0: expression Hi-pot test container initial gas density, unit is every cubic centimetre of (mmol/cm of mM 3);
ρ R1: gas density after the expression high pressure reference container balance, unit is every cubic centimetre of (mmol/cm of mM 3);
ρ F1: gas density after the expression Hi-pot test container balance, unit is every cubic centimetre of (mmol/cm of mM 3);
After free space volumes has been measured, with the gas emptying, start vacuum pump once more and extract high pressure reference container and Hi-pot test container and measuring system internal gas, make high pressure reference container and Hi-pot test container and measuring system inside be in vacuum state, stop vacuum pump then, closeall valve;
(5) adsorbance and adsorption swelling amount are measured simultaneously:
Open Hi-pot test gas (as CH 4, N 2, CO 2Gas) valve starts the gases at high pressure supercharge pump as required, at first opens gas admittance valve, to the Hi-pot test gas that the high pressure reference container charges into, regulate high pressure reference container pressure to goal pressure, close air intake valve then, after treating pressure stability, record high pressure reference container this moment internal pressure P 5With Hi-pot test container internal pressure P 6Open the compensation flap between high pressure reference container and the Hi-pot test container, make Hi-pot test gas enter the Hi-pot test container from the high pressure reference container, treat high pressure reference container and Hi-pot test container internal pressure stable equilibrium after, record this moment equalized pressure P 4, obtain one group of data T, P this moment 4, P 5, P 6The high pressure content ratio juris has been adopted in the test of adsorbance, measuring and controlling instrument can be calculated the absorption variable quantity (Δ n) and the adsorbance (n) in this equilibrium pressure force by measuring the pressure and the temperature of high pressure reference container and Hi-pot test container adsorption equilibrium front and back by mass balance; Simultaneously in this course, Hi-pot test gas enters after the Hi-pot test container from the high pressure reference container, the coal petrography sample will be because absorption Hi-pot test gas will produce dilatational strain, make the displacement transducer measuring staff to top offset, displacement transducer is converted to electric signal with displacement deformation and sends into measuring and controlling instrument, the expansion height (Δ L) of coal petrography sample be can record simultaneously, adsorbance (n) and adsorption swelling amount (ε) calculated by following formula in this equilibrium pressure force; The computing formula of adsorbance is:
Δn = 1 G 0 [ ( ρ R 0 - ρ R 1 ) V R - ( ρ F 1 - ρ F 0 ) V F ] - - - ( 2 )
n＝Δn 1+Δn 2+Δn 3+....+Δn i ——(3)
Wherein: ρ R0=f (T, P 5) ρ F0=f (T, P 6)
ρ R1＝ρ F1＝f(T，P 4)
Adsorption swelling amount computing formula is:
ε＝ΔL/L 0×10 6 ——(4)
More than various in:
Δ n: represent the absorption variable quantity in each equilibrium pressure force, unit is the every gram of mM (mmol/g);
N: represent total adsorbance, unit is the every gram of mM (mmol/g);
G 0: the weight of expression coal petrography sample, unit is gram (g);
Δ L: the expansion height of expression coal petrography sample, unit is a millimeter (mm);
L 0: expression coal petrography sample elemental height, unit is a millimeter (mm);
ε: expression adsorption swelling amount, dimensionless;
V F: expression free space volumes, unit are cubic centimetre (cm 3);
V R: expression high pressure reference container volume (known), unit are cubic centimetre (cm 3);
P 4: pressure after the expression balance, unit is MPa (MPa);
P 5: expression high pressure reference container original pressure, unit is MPa (MPa);
P 6: expression Hi-pot test container original pressure, unit is MPa (MPa);
T: the expression experimental temperature, unit is (K);
ρ R0: expression high pressure reference container initial gas density, unit is every cubic centimetre of (mmol/cm of mM 3);
ρ F0: expression Hi-pot test container initial gas density, unit is every cubic centimetre of (mmol/cm of mM 3);
ρ R1: gas density after the expression high pressure reference container balance, unit is every cubic centimetre of (mmol/cm of mM 3);
ρ F1: gas density after the expression high pressure reference container balance, unit is every cubic centimetre of (mmol/cm of mM 3);
(6) after the adsorption swelling balance, close compensation flap, open gases at high pressure once more (as CH 4, N 2, CO 2Gas) valve, start the gases at high pressure supercharge pump, open gas admittance valve, continue to charge into Hi-pot test gas to high pressure reference container inside, regulate high pressure reference container pressure to next goal pressure, repeat (5) step, carry out the test of next experimental pressure point adsorbance and adsorption swelling amount, like this, test from low and high spot pressure one by one, until last spot pressure off-test, can obtain adsorbance and adsorption swelling amount under the different equalized pressures, i.e. adsorption isothermal and adsorption swelling isotherm; Change system temperature, can measure adsorption isothermal and adsorption swelling isotherm under the different temperatures.
Designed measurement mechanism for finishing the present invention.Measurement mechanism of the present invention is by the Hi-pot test container, the high pressure reference container, and displacement transducer, first pressure unit, second pressure unit, constant temperature bath cabinet and measuring and controlling instrument are formed; The wall that it is characterized in that the constant temperature bath cabinet is equipped with semiconductor chilling plate, in the constant temperature bath cabinet heating tube is housed, ebullator, thermometric thermal resistance, Hi-pot test container and high pressure reference container; The Hi-pot test container is by lower cylinder body, upper cylinder body, cutting ferrule, air intake opening and gas outlet are formed, between upper cylinder body and the lower cylinder body sealing gasket is installed, upper cylinder body and lower cylinder body are connected and sealed by cutting ferrule, at the upper cylinder body top displacement transducer is housed, between displacement transducer and the upper cylinder body sealing gasket is arranged, and be fixed together by fixed part, the measuring staff of displacement transducer passes through upper cylinder body, and be positioned at outside the upper cylinder body bottom, the bottom of upper cylinder body is equipped with sample tube and stay, the sample tube is to be threaded with the bottom of upper cylinder body, stay is fixed together the bottom of sample tube and upper cylinder body, the bleeder vent that is evenly distributed is arranged on the sample tube, lower cylinder body has air intake opening and gas outlet, at high pressure reference container top second pressure unit is arranged, between the high pressure reference container and second pressure unit air intake opening and gas outlet are arranged, air intake opening between the high pressure reference container and second pressure unit is equipped with gas admittance valve, vent valve is equipped with in gas outlet at lower cylinder body, and the equalizing valve and first pressure unit are housed between Hi-pot test container and high pressure reference container; Displacement transducer, first pressure unit, second pressure unit, heating tube, ebullator, semiconductor chilling plate is connected with measuring and controlling instrument by cable with the thermometric thermal resistance.
Described Hi-pot test container and high pressure reference container, its material are stainless steel, and be withstand voltage greater than 30MPa.
Described displacement transducer is that model is a kind of high pressure resistant linear variable differential transformer (LVDT) formula displacement transducer (LVDT) of GA-2, this displacement transducer body and iron core measuring staff are integral structure, have guiding and resilience function, the back springing type structure can avoid measuring staff owing to friction can't reliably contact the measuring error that causes with measuring samples, improves measuring accuracy; This displacement transducer is withstand voltage greater than 30MPa, and measuring accuracy is 0.05%, and measurement range is 0-2mm, and displacement transducer is converted to electric signal with the expansion or the drawdown deformation of measured coal petrography sample, delivers to measuring and controlling instrument and carries out signal Processing and analog to digital conversion.
Described pressure unit is that model is a kind of high-voltage intelligent pressure unit of MPM421, it is withstand voltage greater than 30MPa, measuring accuracy is 0.1%FS, and measurement range is-0.1-20MPa that pressure unit is used to measure the internal pressure of Hi-pot test container and high pressure reference container.
Used heating medium is water or glycerine in the described constant temperature bath cabinet; The working temperature of thermostatic bath is 0-80 ℃, and temperature-controlled precision is 0.1 ℃.
Described thermometric thermal resistance is the Pt100 platinum resistance.
Described measuring and controlling instrument has been used the single chip computer measurement control technology, includes the displacement transducer signal data acquisition circuit, thermometric thermal resistance signal data acquisition circuit, pressure unit signal data acquisition circuit, temperature-control circuit, display circuit, data communication circuit and single-chip microcomputer; Pressure unit, the electric signal of displacement transducer and thermometric thermal resistance is delivered to data acquisition circuit separately, under the control of single-chip microcomputer, by data acquisition circuit to displacement transducer, the thermometric thermal resistance, the electric signal of pressure unit carries out signal transformation and analog to digital conversion, shows the temperature of thermostatic bath in real time by display circuit, the expansion height of Hi-pot test container and high pressure reference container internal pressure and coal petrography sample; Wherein the PID control technology is adopted in temperature control, by temperature-control circuit control heating tube 8, and semiconductor chilling plate, the work of ebullator is carried out temperature control to thermostatic bath; The temperature of being gathered simultaneously, pressure and displacement data are directly sent into computing machine through the data communication circuit, and the RS232 serial communication mode is used in Computer Data Communication, and this measuring and controlling instrument is connected with the RS232 serial line interface of computing machine by RS232 communication lead.
The computing machine automatic reception is from the experimental temperature of measuring and controlling instrument, pressure and displacement signal data, the data that receive are write down and preserve, automatically calculate adsorbance and adsorption swelling amount, and on computer screen, show the temperature in the experimentation in real time, pressure, adsorbance and swell increment data, and show pressure in real time, temperature and swell increment be law curve over time.
Coal petrography gases at high pressure adsorbance provided by the present invention and simultaneously-measured method of adsorption swelling amount and measurement mechanism can be at pressure 0-20MPa, in temperature 0-80 ℃ the scope, measure automatically simultaneously coal petrography at gases at high pressure (as CH 4, N 2, CO 2Gas) adsorbance in and adsorption swelling amount.In measuring process, measuring and controlling instrument is to displacement transducer, the thermometric thermal resistance, and the electric signal of pressure unit carries out signal transformation and analog to digital conversion, shows experimental pressure in real time, the displacement signal data that the expansion of temperature and sample changes.The computing machine automatic reception is from the pressure of measuring and controlling instrument, temperature and displacement signal data, the data that receive are write down and preserve, automatically calculate adsorbance and adsorption swelling amount, on computer screen, show the pressure in the experimentation in real time, temperature, adsorbance and swell increment data, and show pressure in real time, temperature and swell increment be law curve over time.
Coal petrography gases at high pressure adsorbance provided by the present invention and simultaneously-measured method of adsorption swelling amount and measurement mechanism also can be widely used in other field, are used for test and the research of other porous mass in the adsorbance and the adsorption swelling amount of gases at high pressure.
The present invention has the following advantages:
1, can disposablely finish the measurement of adsorbance and adsorption swelling amount, more easy than existing additive method, quick.
2, use same specimen to measure adsorbance and adsorption swelling amount simultaneously, can reflect the relation of influencing each other between them better.
3, adopt the bulk sample coal sample of cylindrical or rectangular build, test findings helps comparing with conventional rock mechanics standard, has higher utility.
4, displacement sensor adsorption swelling amount, what the measurement of adsorbance was adopted is the high pressure content ratio juris, directly utilizes the swell increment test container as the sample cylinder in the high pressure content method absorption measurement, measures the adsorption swelling amount when measuring adsorbance.
Measure when 5, not only can be used for adsorbance and adsorption swelling amount, obtain adsorption isothermal and adsorption swelling isotherm.Measure when also can be used for desorption rate and desorption amount of contraction, obtain desorption isotherm and desorption and shrink isotherm.
Measure when 6, not only can be used for adsorbance and adsorption swelling amount, also can be used for independent measurement adsorbance or independent measurement adsorption swelling amount.
7, have simple in structurely, high pressure sealing is reliable and secure, easy operating, measuring accuracy height, withstand voltage height, the advantage of measuring automatically.
Description of drawings:
Fig. 1, be coal petrography gases at high pressure adsorbance and the adsorption swelling amount structural representation of measurement mechanism simultaneously
Fig. 2, be coal petrography gases at high pressure adsorbance and the adsorption swelling amount circuit diagram of measurement mechanism simultaneously
Fig. 3, be coal petrography gases at high pressure adsorbance and adsorption swelling amount simultaneously measurement mechanism use synoptic diagram
Fig. 4, be temperature under 45 ℃ of conditions, a kind of Yangquan coal petrography sample of surveying at CO 2The relation curve of the adsorbance in the gas and adsorption swelling amount and equalized pressure.
Fig. 5, be under 65 ℃ of conditions, a kind of Yangquan coal petrography sample of surveying at CH 4The relation curve of the adsorbance in the gas and adsorption swelling amount and equalized pressure.
Fig. 6, be under 25 ℃ of conditions, a kind of Yangquan coal petrography sample of surveying at N 2The relation curve of the adsorbance in the gas and adsorption swelling amount and equalized pressure.
As shown in the figure: the 1st, Hi-pot test container, the 2nd, high pressure reference container, the 3rd, displacement transducer, 4 second pressure units, 5 is first pressure units, the 6th, and column type sample tube, the 7th, stay, the 8th, heating tube, the 9th, thermometric thermal resistance, the 10th, bottom cylinder body, the 11st, top cylinder body, the 12nd, cutting ferrule, the 13rd, fixed part, the 14th, sealing gasket, the 15th, coal petrography sample, the 16th, semiconductor chilling plate, the 17th, ebullator, the 18th, thermostatic bath, the 19th, constant temperature bath cabinet, the 20th, gas admittance valve, the 21st, equalizing valve, the 22nd, vent valve, the 23rd, measuring and controlling instrument, 24,25,29,31st, by-pass valve control, the 26th, vacuum pump, the 27th, computing machine, the 28th, high-pressure helium (He) steel cylinder, the 30th, Hi-pot test gas bomb, the 32nd, supercharge pump, the 33rd, fixed head, the 34th, sealing gasket.
Embodiment
Be described in detail below in conjunction with embodiment illustrated in fig. 3 the specific embodiment of the present invention is done further.
Embodiment 1:
Measurement mechanism is by Hi-pot test container 1, high pressure reference container 2, displacement transducer 3, the first pressure units 5, the second pressure units 4, constant temperature bath cabinet 19 and measuring and controlling instrument 23 are formed, the wall of constant temperature bath cabinet 19 is equipped with semiconductor chilling plate 16, and heating tube 8 is equipped with in constant temperature oven 19 inside, thermometric thermal resistance 9, ebullator 17, Hi-pot test container 1 and high pressure reference container 2; Hi-pot test container 1 is by lower cylinder body 10, upper cylinder body 11, cutting ferrule 12, air intake opening and gas outlet are formed, between upper cylinder body 11 and the lower cylinder body 10 sealing gasket 14 is installed, upper cylinder body 11 is connected and fixed by cutting ferrule 12 with lower cylinder body 10, at upper cylinder body 11 tops displacement transducer 3 is housed, sealing gasket 34 is housed between displacement transducer 3 and the upper cylinder body 11 and is fixed together by fixed part 13, the bottom of upper cylinder body 11 is equipped with column type sample tube 6 and stay 7, column type sample tube 6 is to be threaded with the bottom of upper cylinder body 11, and stay 7 is connected and fixed the bottom of column type sample tube 6 with upper cylinder body 11, on the column type sample tube 6 bleeder vent that is evenly distributed is arranged; At high pressure reference container 2 tops second pressure unit 4 is arranged, between the high pressure reference container 2 and second pressure unit 4 air intake opening and gas outlet are arranged, air intake opening between the high pressure reference container 2 and second pressure unit 4 is equipped with gas admittance valve 20, in the gas outlet of lower cylinder body 10 vent valve 22 is housed, the equalizing valve 21 and first pressure unit 5 are housed between Hi-pot test container 1 and high pressure reference container 2; Displacement transducer 3, the first pressure units 5, the second pressure units 4, heating tube 8, ebullator 17, semiconductor chilling plate 11 is connected with measuring and controlling instrument 23 by cable with thermometric thermal resistance 9.
The material of Hi-pot test container 1 is a stainless steel, and is withstand voltage greater than 30MPa.Displacement transducer 3 is that model is the high pressure resistant linear variable differential transformer (LVDT) formula displacement transducer of GA-2, first pressure unit 5 and second pressure unit 4 are that model is the high-voltage intelligent pressure unit of MPM421, thermometric thermal resistance 9 is the Pt100 platinum resistance, and constant temperature bath cabinet 19 used heating mediums are water or glycerine.
Measuring and controlling instrument 23 has been used the single chip computer measurement control technology, comprises the displacement transducer signal data acquisition circuit, thermometric thermal resistance signal data acquisition circuit, pressure unit signal data acquisition circuit, temperature-control circuit, display circuit, data communication circuit and single-chip microcomputer; First pressure unit 5, second pressure unit 4, the electric signal of displacement transducer 3 and thermometric thermal resistance 9 is delivered to data acquisition circuit separately, under the control of single-chip microcomputer, data acquisition circuit is with first pressure unit, 5, the second pressure units 4, and the electric signal of displacement transducer 3 and thermometric thermal resistance 9 carries out signal transformation and analog to digital conversion, show the temperature of thermostatic bath in real time by display circuit, the expansion height of high pressure reference container 2 and Hi-pot test container 1 internal pressure and sample; Wherein the PID control technology is adopted in temperature control, by temperature-control circuit control heating tube 8, and ebullator 17, the work of semiconductor chilling plate 16 is carried out temperature control to thermostatic bath 18; The temperature of being gathered simultaneously, pressure and displacement data are directly sent into computing machine 27 through the data communication circuit, the RS232 serial communication mode is used in Computer Data Communication, and measuring and controlling instrument 23 is connected with the RS232 serial line interface of computing machine 27 by RS232 communication lead.
Narrate adsorbance and adsorption swelling amount measuring process simultaneously below:
Earlier measurement mechanism is connected according to mode shown in Figure 3.
At first Yangquan to be measured coal petrography is processed into the bulk sample of column type or rectangular build, and guarantees that coal petrography sample 15 upper and lower end faces are parallel and smooth,, accurately measure the height (L of coal petrography sample coal petrography sample dry 12h under 110 ℃ of vacuum conditions of temperature 0), and accurately take by weighing the weight (G of coal petrography sample 0), sealing is preserved stand-by.
Open measuring and controlling instrument 23 power supplys, start computing machine 27.With the coal petrography sample 15 column type sample tube 6 of packing into fast, column type sample tube 6 is connected with the top cylinder body 11 of Hi-pot test container 1, guarantee that coal petrography sample 15 reliably contacts with the measuring staff of displacement transducer 3, regulate the height of column type sample tube 6, observe the displacement data that shows on measuring and controlling instrument or the computer screen simultaneously, accurately regulate the zero point of displacement transducer, with stay 7 fixed cylinder type sample tubes 6, the bottom cylinder body 10 of then top cylinder body 11 being packed into will be gone up lower cylinder body with cutting ferrule 12 and be connected and fixed.
Design temperature is 45 ℃ (T) for experiment is temperature required, start and add heat control, thermostatic bath 18 is heated, treat that thermostatic bath 18 temperature arrive design temperature (45 ℃), close all valves, open equalizing valve 21, air release 22 and vacuum valve 25 start vacuum pump 26 and extract high pressure reference container 2 and Hi-pot test container 1 and internal system air.Close equalizing valve 21 then, air release 22 and vacuum valve 25 stop vacuum pump 26.
Open helium (He) steel cylinder 28 valves and helium stop valve 29, start gases at high pressure supercharge pump 32 and charge into helium to system.Open gas admittance valve 20, charge into a certain amount of helium to high pressure reference container 2, second pressure unit 4 is used to measure high pressure reference container 2 internal pressures, regulate high pressure reference container 2 pressure to goal pressure, close gas admittance valve 20 then, treat pressure stability, record high pressure reference container this moment 2 internal pressure (P 2) and Hi-pot test container 1 internal pressure (P 3); Open the equalizing valve 21 between high pressure reference container 2 and the Hi-pot test container 1, make helium enter Hi-pot test container 1 from high pressure reference container 2, first pressure unit 5 is used to measure Hi-pot test container 1 internal pressure, after treating high pressure reference container 2 and Hi-pot test container 1 internal pressure stabilises balance, record pressure (P this moment 1), by measuring and controlling instrument 23 acquisition system temperature (T) and pressure (P 1), (P 2) and (P 3) signal, carry out data processing by computing machine 27, calculate the Hi-pot test container 1 internal freedom spatial volume (V that places behind the coal petrography sample F); Emptying system then, start vacuum pump 26 once more and extract high pressure reference container 2 and Hi-pot test container 1 and internal system gas, make high pressure reference container 2 and Hi-pot test container 1 and internal system be in vacuum state, stop vacuum pump 26 then, closeall valve.Free space volumes specifically calculates:
The data that record:
T＝45+273.15＝318.45(K) P 1＝0.965(MPa) P 2＝1.280(MPa)
P 3＝0.000(MPa) V R＝176.74(cm 3)
ρ R1＝ρ F1＝f(T，P 1)＝0.3633(mmol/cm 3)
ρ R0＝f(T，P 2)＝0.4813(mmol/cm 3)
ρ F0＝f(T，P 3)＝0.0000(mmol/cm 3)
Calculate and can get by formula (1):
V F＝V R(ρ R0-ρ R1)/(ρ F1-ρ F0)＝57.41(cm 3)
Open Hi-pot test gas (CO 2Gas) steel cylinder 30 valves and stop valve 31 start gases at high pressure supercharge pump 32, charge into Hi-pot test gas (CO to internal system 2Gas); Open gas admittance valve 20, charge into a certain amount of Hi-pot test gas to high pressure reference container 2, second pressure unit 4 is used to measure high pressure reference container 2 internal pressures, regulates high pressure reference container 2 pressure to goal pressure, closes gas admittance valve 20 then; Treat pressure stability, record high pressure reference container this moment 2 internal pressure (P 5) and Hi-pot test container 1 internal pressure (P 6); Open the equalizing valve 21 between high pressure reference container 2 and the Hi-pot test container 1, make Hi-pot test gas enter Hi-pot test container 1 from high pressure reference container 2, first pressure unit 5 is used to measure Hi-pot test container 1 internal pressure, after treating high pressure reference container 2 and Hi-pot test container 1 internal pressure stabilises balance, record equalized pressure (P this moment 4); This moment is by measuring and controlling instrument 23 acquisition system temperature (T) and pressure (P 4), (P 5) and (P 6) signal, carry out data processing by computing machine 27.According to pressure and the temperature before and after high pressure reference container 2 and Hi-pot test container 1 balance, can obtain adsorbance (the Δ n in this equilibrium pressure force 1) and adsorbance (n).
In this course, Hi-pot test gas enters from high pressure reference container 2 after the Hi-pot test container 1, and coal petrography sample 15 is because absorption Hi-pot test gas (CO 2Gas) will produce dilatational strain, and make displacement transducer 3 measuring staffs to top offset, displacement transducer 3 is converted to electric signal with displacement deformation, delivers to measuring and controlling instrument 23 and carries out signal Processing and analog to digital conversion.Computing machine 27 automatic receptions are from the experimental pressure of measuring and controlling instrument 23, temperature and displacement signal data, the data that receive are write down and preserve, and on computer screen, show the pressure in the experimentation in real time, temperature and expansion data, and swell increment law curve over time.After the adsorption swelling balance, can record expansion height (the Δ L of coal petrography sample simultaneously in this equilibrium pressure force 1) and adsorption swelling amount (ε).
The concrete calculating of adsorbance and adsorption swelling amount:
T＝45+273.15＝318.45(K) L 0＝68.70(mm) G 0＝18.8527(g)
P 4＝0.425(MPa) P 5＝0.780(MPa) P 6＝0.000(MPa)
V R＝176.74(cm 3) ρ R1＝ρ F1＝f(T，P 4)＝0.1635(mmol/cm 3)
ρ R0＝f(T，P 5)＝0.3046(mmol/cm 3) ρ F0＝f(T，P 6)＝0.0000(mmol/cm 3)
V F＝57.41(cm 3) ΔL 1＝0.1308(mm)
Calculate and can get by formula (2):
Δ n 1 = 1 G 0 [ ( ρ R 0 - ρ R 1 ) V R - ( ρ F 1 - ρ F 0 ) V F ] = 0.8249 ( mmol / g )
Calculate and can get by formula (3):
n＝Δn 1＝0.8249(mmol/g)
Calculate and can get by formula (4):
ε＝ΔL 1/L 0×10 6＝1904
After the adsorption swelling balance, close equalizing valve 21; Open gases at high pressure (CO once more 2Gas) steel cylinder 30 valves and valve 31, start gases at high pressure supercharge pump 32, open gas admittance valve 20, continue to charge into Hi-pot test gas to high pressure reference container 2 inside, regulate high pressure reference container 2 pressure to next goal pressure, repeat above step, carry out the test of next experimental pressure point adsorbance and adsorption swelling amount., test, until last spot pressure off-test from low and high spot pressure one by one like this.Can obtain adsorbance and adsorption swelling amount under the different pressures, i.e. adsorption isothermal and adsorption swelling isotherm.Change system temperature, can measure adsorption isothermal and adsorption swelling isotherm under the different temperatures.
Embodiment 2:
Design temperature is at 65 ℃, and Hi-pot test gas is CH 4Under the condition of gas, all the other are with embodiment 1.
Embodiment 3:
Design temperature is at 25 ℃, and Hi-pot test gas is N 2Under the condition of gas, all the other are with embodiment 1.

Claims (8)

1. coal petrography gases at high pressure adsorbance and the simultaneously-measured method of adsorption swelling amount is characterized in that comprising the steps:
(1) preparation of test coal petrography sample:
At first coal petrography to be measured is processed into the bulk sample of column type or rectangular build, and guarantees that coal petrography sample upper and lower end face is parallel and smooth, as required the coal petrography sample is carried out equilibrium moisture then and handle or dried, accurately measure the height L of coal petrography sample 0, and accurately take by weighing the weight G of coal petrography sample 0
(2) installation of test coal petrography sample:
At first open measuring and controlling instrument (23) power supply, start computing machine (27) and operation;
With pack into the sample tube (6) of measurement mechanism of coal petrography sample, the bottom of sample tube (6) with the upper cylinder body (11) of Hi-pot test container (1) is connected, by regulating the position of sample tube (6), guarantee that the coal petrography sample reliably contacts with the displacement transducer that is contained in upper cylinder body (11) (3) measuring staff; Observe the displacement data that shows on measuring and controlling instrument (23) or computing machine (27) screen simultaneously, accurately regulate the zero point of displacement transducer, with stay (7) that the bottom and the sample tube (6) of upper cylinder body (11) is fixing, then sample tube (6) is packed into the lower cylinder body (10) of Hi-pot test container (1) is tightly connected with lower cylinder body (10) with the upper cylinder body (11) of cutting ferrule (12) with Hi-pot test container (1);
(3) work is prepared before the test:
According to experimental program, set the temperature required T of experiment, start and add heat control, thermostatic bath (18) is heated, when treating that thermostatic bath (18) temperature arrives design temperature T, start vacuum pump and extract high pressure reference container (2) and Hi-pot test container (1) and measuring system inner air, make high pressure reference container (2) and Hi-pot test container (1) and measuring system inside be in vacuum state, stop vacuum pump then, closeall valve;
(4) free space volumes is measured:
Open the high-pressure helium valve, in system, charge into helium, open gas admittance valve (20), the helium that charges into to high pressure reference container (2), regulate high pressure reference container (2) pressure to goal pressure, close gas admittance valve (20) then, treat after the pressure stability, record high pressure reference container (2) internal pressure P this moment 2With Hi-pot test container (1) internal pressure P 3Open the equalizing valve (21) between high pressure reference container (2) and the Hi-pot test container (1), make helium enter Hi-pot test container (1) from high pressure reference container (2), treat high pressure reference container (2) and Hi-pot test container (1) internal pressure stabilises balance after, record this moment pressure P 1, obtain one group of data T, P this moment 1, P 2, P 3, calculate the volume V that places Hi-pot test container (1) the internal freedom space behind the coal petrography sample by following formula F
The free space volumes computing formula is:
V F＝V R(ρ R0-ρ R1)/(ρ F1-ρ F0) ——(1)
Wherein: ρ R0=f (T, P 2) ρ F0=f (T, P 3)
ρ R1＝ρ F1＝f(T，P 1)
In the formula:
V F: expression free space volumes, unit are cubic centimetre;
V R: expression high pressure reference container (2) volume, unit is a cubic centimetre);
P 1: pressure after the expression balance, unit is a MPa;
P 2: expression high pressure reference container (2) original pressure, unit is a MPa;
P 3: expression Hi-pot test container (1) original pressure, unit is a MPa;
T: the expression experimental temperature, unit is K;
ρ R0:Expression high pressure reference container (2) initial gas density, unit is every cubic centimetre of a mM;
ρ F0: expression Hi-pot test container (1) initial gas density, unit is every cubic centimetre of a mM;
ρ R1: gas density after expression high pressure reference container (2) balance, unit is every cubic centimetre of a mM;
ρ F1: gas density after expression Hi-pot test container (1) balance, unit is every cubic centimetre of a mM;
After free space volumes has been measured, with the gas emptying, start vacuum pump once more and extract high pressure reference container (2) and Hi-pot test container (1) and measuring system internal gas, make high pressure reference container (2) and Hi-pot test container (1) and measuring system inside be in vacuum state, stop vacuum pump then, closeall valve;
(5) adsorbance and adsorption swelling amount are measured simultaneously:
Open the Hi-pot test gas valve, start the gases at high pressure supercharge pump as required, at first open gas admittance valve (20), the Hi-pot test gas that charges into to high pressure reference container (2), regulate high pressure reference container (2) pressure to goal pressure, close gas admittance valve (20) then, treat pressure stability after, record this moment high pressure reference container (2) internal pressure P 5With Hi-pot test container (1) internal pressure P 6Open the equalizing valve (21) between high pressure reference container (2) and the Hi-pot test container (1), make Hi-pot test gas enter Hi-pot test container (1) from high pressure reference container (2), after treating high pressure reference container (2) and Hi-pot test container (1) internal pressure stabilises balance, record equalized pressure P this moment 4, obtain one group of data T, P this moment 4, P 5, P 6Calculate adsorbance n and adsorption swelling amount ε by following formula;
The computing formula of adsorbance is:
n＝Δn 1+Δn 2+Δn 3+....+Δn i ——(3)
Wherein: ρ R0=f (T, P 5) ρ F0=f (T, P 6)
ρ R1＝ρ F1＝f(T，P 4)
Adsorption swelling amount computing formula is:
ε＝ΔL/L 0×10 6 ——(4)
More than various in:
Δ n: represent the absorption variable quantity in each equilibrium pressure force, unit is the every gram of mM;
R: represent total adsorbance, unit is the every gram of mM;
G 0: the weight of expression coal petrography sample, unit is gram;
Δ L: the expansion height of expression coal petrography sample, unit is a millimeter;
L 0: expression coal petrography sample elemental height, unit is a millimeter;
ε: expression adsorption swelling amount, dimensionless;
V F: expression free space volumes, unit are cubic centimetre;
V R: expression high pressure reference container (2) volume, unit is a cubic centimetre;
P 4: pressure after the expression balance, unit is a MPa;
P 5: expression high pressure reference container (2) original pressure, unit is a MPa;
P 6: expression Hi-pot test container (1) original pressure, unit is a MPa;
T: the expression experimental temperature, unit is K;
ρ R0: expression high pressure reference container (2) initial gas density, unit is every cubic centimetre of a mM;
ρ F0: expression Hi-pot test container (1) initial gas density, unit is every cubic centimetre of a mM;
ρ R1: gas density after expression high pressure reference container (2) balance, unit is every cubic centimetre of a mM;
ρ F1: gas density after expression high pressure reference container (1) balance, unit is every cubic centimetre of a mM;
(6) after the adsorption swelling balance, close equalizing valve (21), open high pressure gas valve once more, start the gases at high pressure supercharge pump, open gas admittance valve (20), continue to charge into Hi-pot test gas to high pressure reference container (2) inside, regulate high pressure reference container (2) pressure to next goal pressure, repeat (5) step, carry out the test of next experimental pressure point adsorbance and adsorption swelling amount, like this, test from low and high spot pressure one by one, until last spot pressure off-test, can obtain adsorbance and adsorption swelling amount under the different equalized pressures, i.e. adsorption isothermal and adsorption swelling isotherm; Change system temperature, can measure adsorption isothermal and adsorption swelling isotherm under the different temperatures.
2. a kind of coal petrography gases at high pressure adsorbance as claimed in claim 1 and the simultaneously-measured measurement mechanism of adsorption swelling amount, it is by Hi-pot test container (1), high pressure reference container (2), displacement transducer (3), first pressure unit (5), second pressure unit (4), constant temperature bath cabinet (19) and measuring and controlling instrument (23) are formed; The wall of constant temperature bath cabinet (19) is equipped with semiconductor chilling plate (16), and heating tube (8) is equipped with in constant temperature bath cabinet (19) inside, thermometric thermal resistance (9), ebullator (17), Hi-pot test container (1) and high pressure reference container (2); Hi-pot test container (1) is by lower cylinder body (10), upper cylinder body (11), cutting ferrule (12), air intake opening and gas outlet are formed, between upper cylinder body (11) and the lower cylinder body (10) sealing gasket (14) is installed, upper cylinder body (11) is connected and fixed by cutting ferrule (12) with lower cylinder body (10), at upper cylinder body (11) top displacement transducer (3) is housed, between displacement transducer (3) and the upper cylinder body (11) sealing gasket (34) is housed, and be fixed together by fixed part (13), the bottom of upper cylinder body (11) is equipped with sample tube (6) and stay (7), sample tube (6) is to be threaded with the bottom of upper cylinder body (11), stay (7) is connected and fixed the bottom of sample tube (6) with upper cylinder body (11), and the sample tube has the bleeder vent that is evenly distributed on (6); At high pressure reference container (2) top second pressure unit (4) is arranged, between high pressure reference container (2) and second pressure unit (4) air intake opening and gas outlet are arranged, air intake opening between high pressure reference container (2) and second pressure unit (4) is equipped with gas admittance valve (20), in the gas outlet of lower cylinder body (10) vent valve (22) is housed, equalizing valve (21) and first pressure unit (5) are housed between Hi-pot test container (1) and high pressure reference container (2); Displacement transducer (3), first pressure unit (5), second pressure unit (4), heating tube (8), ebullator (17), semiconductor chilling plate (11) is connected with measuring and controlling instrument (23) by cable with thermometric thermal resistance (9).
3. a kind of coal petrography gases at high pressure adsorbance as claimed in claim 2 and the simultaneously-measured measurement mechanism of adsorption swelling amount is characterized in that the material of described Hi-pot test container (1) and high pressure reference container (2) is a stainless steel, and be withstand voltage greater than 30Mpa.
4. a kind of coal petrography gases at high pressure adsorbance as claimed in claim 2 and the simultaneously-measured measurement mechanism of adsorption swelling amount, it is characterized in that described displacement transducer (3) is that model is a kind of high pressure resistant linear variable differential transformer (LVDT) formula displacement transducer of GA-2, withstand voltage greater than 30MPa, measuring accuracy is 0.05%, and measurement range is 0-2mm.
5. a kind of coal petrography gases at high pressure adsorbance as claimed in claim 2 and the simultaneously-measured measurement mechanism of adsorption swelling amount, it is characterized in that described first pressure unit (5) and second pressure unit (4) are that model is the high-voltage intelligent pressure unit of MPM421, it is withstand voltage greater than 30MPa, measuring accuracy is 0.1%FS, and measurement range is-0.1-20Mpa.
6. a kind of coal petrography gases at high pressure adsorbance as claimed in claim 2 and the simultaneously-measured measurement mechanism of adsorption swelling amount, it is characterized in that used heating medium is water or glycerine in the described constant temperature bath cabinet (19), the working temperature of the interior heating medium of constant temperature bath cabinet (19) is 0-80 ℃, and temperature-controlled precision is 0.1 ℃.
7. a kind of coal petrography gases at high pressure adsorbance as claimed in claim 2 and the simultaneously-measured measurement mechanism of adsorption swelling amount is characterized in that described thermometric thermal resistance is Pt 100 platinum resistance.
8. a kind of coal petrography gases at high pressure adsorbance as claimed in claim 2 and the simultaneously-measured measurement mechanism of adsorption swelling amount, it is characterized in that described measuring and controlling instrument (23) includes the displacement transducer signal data acquisition circuit, thermometric thermal resistance signal data acquisition circuit, pressure unit signal data acquisition circuit, temperature-control circuit, display circuit, data communication circuit and single-chip microcomputer; First pressure unit (5), the electric signal of second pressure unit (4) displacement transducer (3) and thermometric thermal resistance (9) is delivered to data acquisition circuit separately, under the control of single-chip microcomputer, by data acquisition circuit to displacement transducer (3), thermometric thermal resistance (9), the electric signal of first pressure unit (5) and second pressure unit (4) carries out signal transformation and analog to digital conversion, show the temperature of thermostatic bath in real time by display circuit, the expansion height of Hi-pot test container (1) and high pressure reference container (2) internal pressure and coal petrography sample; Wherein the PID control technology is adopted in temperature control, by temperature-control circuit control heating tube (8), and semiconductor chilling plate (16), the work of ebullator (17) is carried out temperature control to thermostatic bath (18); The temperature of being gathered simultaneously, pressure and displacement data are directly sent into computing machine (27) through the data communication circuit, the RS232 serial communication mode is used in Computer Data Communication, and measuring and controlling instrument (23) is connected with the RS232 serial line interface of computing machine (27) by RS232 communication lead.
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CN109708993A (en) * 2018-11-14 2019-05-03 中国石油天然气股份有限公司 A kind of mud shale high pressure gas isothermal adsorption quantity measuring method and device
CN110196206A (en) * 2019-05-15 2019-09-03 中国矿业大学 A kind of more gas competitive Adsorption test devices of Residual coal in goaf and its application method
CN110455670A (en) * 2019-09-09 2019-11-15 中国矿业大学(北京) It is a kind of to consider the coal dust test device for desorption of mash gas that initially desorbs and method
CN110455670B (en) * 2019-09-09 2020-07-17 中国矿业大学(北京) Pulverized coal gas desorption test device and method considering initial desorption
CN110927203A (en) * 2019-12-25 2020-03-27 重庆大学 Long coal petrography sample gas-liquid temperature rise adsorption expansion test chamber
CN110927203B (en) * 2019-12-25 2020-10-27 重庆大学 Long coal petrography sample gas-liquid temperature rise adsorption expansion test chamber

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