CN103994943A - Coal/shale isothermal adsorption experimental device - Google Patents

Coal/shale isothermal adsorption experimental device Download PDF

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Publication number
CN103994943A
CN103994943A CN201410222208.8A CN201410222208A CN103994943A CN 103994943 A CN103994943 A CN 103994943A CN 201410222208 A CN201410222208 A CN 201410222208A CN 103994943 A CN103994943 A CN 103994943A
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still
valve
gas
mesozone
sample
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CN103994943B (en
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宁正福
何斌
杨峰
王庆
赵天逸
孔德涛
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China University of Petroleum Beijing
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China University of Petroleum Beijing
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Abstract

The invention provides a coal/shale isothermal adsorption experimental device, wherein the output hole of a reference kettle and the first port of an intermediate area are connected through a first valve; the second port of the intermediate area and a gas storage tank are connected through a second valve; a third valve is arranged at the third port of the intermediate area; the fourth port of the intermediate area and a sample kettle are connected through a fourth valve; the reference kettle, the sample kettle, a temperature sensor, the gas storage tank and the intermediate area are arranged in a constant-temperature control box; a filter net is arranged at the output hole of the sample kettle; a first pressure sensor is used for obtaining the pressure value in the reference kettle; the second pressure sensor is used for obtaining the pressure valve in the sample kettle; the temperature sensor is used for precisely measuring the temperature value in the adsorption experimental process; the gas storage tank is used for pre-heating gas required in the adsorption experimental process before entering the reference kettle and the sample kettle; the intermediate area is used for gradually decreasing the pressure of the reference kettle and gradually increasing the pressure of the sample kettle, and therefore, the adsorption amount under different sample kettle pressures after adsorption equilibrium for many times is obtained.

Description

A kind of coal/shale isothermal adsorption experimental provision
Technical field
The present invention relates to adsorbance fields of measurement, particularly a kind of coal/shale isothermal adsorption experimental provision.
Background technology
At present, the experimental technique of measurement gas adsorption isothermal mainly contains volumetric method and the large class of gravimetric method two.Wherein, volumetric method is divided into constant volume type and constant-pressure type according to gas inject mode difference.
Constant volume type volumetric method, as the most conventional method, its experimental provision is mainly by gas cylinder, vacuum pump, supercharge pump, with reference to still, sample still, pressure and temperature sensor and constant temperature oven form, in experimentation, first to reference to injecting adsorbate gas in still, after pressure stability, record is with reference to still pressure, then open with reference to the intermediate valve between still and sample still, allow gas isothermal expansion enter sample still, after waiting for adsorption equilibrium, record equalized pressure, just can calculate each absorption increment according to the principle of mass conservation, Cumulative sum obtains the adsorbance under corresponding pressure.Repeat aforementioned process, just can obtain whole piece adsorption isothermal.
Constant-pressure type volumetric method is similar with it, and different is that the piston pump of a variable volume of reference still fixing volume is replaced, and adsorbate gas is that constant voltage is injected in sample still, same, utilizes the mass conservation to calculate adsorbance.But because variable volume piston pump is more complicated, sealing property is bad, be suitable for the shortcomings such as condition of high voltage is poor, operation inconvenience, there be limited evidence currently of uses, and people generally adopt constant volume type volumetric method, i.e. traditional volumetric method.
Gravimetric method is to calculate adsorbance according to the weight change of sample before and after absorption, and its main device is made up of electromagnetic suspension system balance, high-pressure sealed still and constant temperature oven.Wherein, airtight still is separated into two confined chambers, rock sample to be measured and gases at high pressure are placed in respectively in two confined chambers, in experimentation, first record the quality reading of sample still, then progressively in sample still, be filled with gas to be measured, the sample quality while recording adsorption equilibrium after wait balance reading is stable, the difference of front and back two inferior qualities is the quality of adsorbed gas.In gravimetric method experimentation, because gas exists buoyant weight, therefore before experiment, need to carry out buoyancy correction of weighing.
The required experimental facilities cost of gravimetric method is relatively costly, and there be limited evidence currently of uses.
At present, the experimental provision of robotization control is few, is to need people manually to control mostly, and on the one hand, manually control need to be opened constant temperature oven, causes the temperature fluctuation of experimental situation larger, has extended pressure balance time, needs to wait for the longer adsorption experiment time; On the other hand, manually control and need manpower, and pressure control is not accurate enough.And if adopt automation control system, the problem of these two aspects all can be well solved.
At present, people be all based on traditional volumetric method principle design different adsorption experimental apparatus, the experiment flow of volumetric method is not had to too many research, also the error in experimentation and error effect factor are not carried out to detailed analysis.The high pressure isothermal adsorption test method (with reference to standard GB/T/T19560-2008) of coal is also the experimental principle based on traditional volumetric method, and experiment flow does not change.Chinese invention patent CN102607991A is coal/shale adsorbance determinator, though this device possesses the absorbed natural gas process of the actual geology Coal Under/shale of simulation and the ability of its absorption is evaluated, measuring method is still traditional volumetric method.
The needed experimental provision of tradition volumetric method is simple, easy to operate, but the experimental implementation of multiple injection gas can be brought the repeatedly accumulation of measuring error, cause the experimental error of measurement result very large, finally may cause that adsorption isothermal is abnormal, therefore this method is only applicable to the adsorbent (as activated charcoal etc.) of adsorbance large (measuring error impact is little), measurement for the very low coal/shale of absorption tolerance produces very large error, has a strong impact on experimental result.Although patent CN102607991A possesses the ability that coal/shale adsorbance is measured, and propose to utilize pneumatic valve to carry out procedure auto-control, simulation reservoir pressure is higher, but its principle is constant volume type volumetric method, the error of measurement result is still very large, can not ensure accurately to measure the adsorptive power of gas with various in the actual formation Coal Under/shale such as High Temperature High Pressure.
Summary of the invention
In order to eliminate the error accumulation in traditional volumetric method measuring process, reduce the experimental error of measurement result, the invention provides a kind of coal/shale isothermal adsorption experimental provision, by improving experimental provision, make accurately to measure the adsorptive power of gas with various in the actual formation Coal Under/shale such as High Temperature High Pressure.
For achieving the above object, the invention provides a kind of coal/shale isothermal adsorption experimental provision, described experimental provision comprises: with reference to still, sample still, the first pressure transducer, the second pressure transducer, temperature sensor, constant temperature control box, gas-holder and filter screen; Described experimental provision also comprises: mesozone; Wherein,
The described delivery outlet with reference to still is connected by the first valve with the first port of described mesozone, the second port of described mesozone is connected by the second valve with described gas-holder, the 3rd port of described mesozone arranges the 3rd valve, and the 4th port of described mesozone is connected by the 4th valve with described sample still;
Describedly all be arranged in described constant temperature control box with reference to still, described sample still, described temperature sensor, described gas-holder and described mesozone;
The equipped at outlet port of described sample still arranges described filter screen;
Described the first pressure transducer, described with reference to the force value in still for obtaining;
Described the second pressure transducer, for obtaining the force value in described sample still;
Described temperature sensor, for accurately measuring the temperature value of adsorption experiment process;
Described gas-holder carried out thermal pretreatment before entering with reference to still and sample still at the required gas of adsorption experiment process;
Described mesozone, with reference to the progressively step-down of still and the progressively supercharging of described sample still, realizes the adsorbance obtaining under sample still pressure different after multiple adsorb balance for described.
Optionally, in an embodiment of the present invention, described experimental provision also comprises: gas chromatograph;
Described gas chromatograph, in the time carrying out multicomponent gas experiment, gets gas by the 3rd valve of described mesozone, then carries out gas composition analysis.
Optionally, in an embodiment of the present invention, the volume of described mesozone is the described volume with reference to still 1 20 ~ 1 15 .
Optionally, in an embodiment of the present invention, described the first valve, described the second valve, described the 3rd valve and described the 4th valve are pneumatic valve.
Optionally, in an embodiment of the present invention, described experimental provision also comprises flow-limiting valve;
In pipeline between the described delivery outlet with reference to still and described the first valve, described flow-limiting valve is set, described with reference to progressively step-down of still for accurately controlling.
Compared with traditional device, the effect of this device and advantage applies are in the following aspects:
1, this device is provided with mesozone between with reference to still and sample still, be connected by valve, and ultimate principle based on volumetric method, propose isothermal adsorption and tested new measuring method, can effectively reduce gas injection number of times, shorten the adsorption experiment time.
2, owing to being provided with mesozone, can realize with reference to the progressively step-down of still, the progressively supercharging of sample still, solved in prior art, face from a slowly difficult problem for step-down progressively of high pressure, and provide one to solve clearly thinking.
3, the experimental provision after improvement can effectively reduce the experimental error of measurement result, has improved measuring accuracy.
4, in the time carrying out multicomponent gas experiment, can get gas by mesozone, carry out gas composition analysis by gas chromatograph, reduce the risk of getting gas under conventional art.
Brief description of the drawings
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, to the accompanying drawing of required use in embodiment or description of the Prior Art be briefly described below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, do not paying under the prerequisite of creative work, can also obtain according to these accompanying drawings other accompanying drawing.
Fig. 1 is a kind of coal/shale isothermal adsorption experimental provision schematic diagram that the present invention proposes;
Fig. 2 is the measurement result of the present embodiment and the error of traditional volumetric method measurement result contrast schematic diagram.
Accompanying drawing mark:
1, gas bomb, 2, helium steel cylinder, 3, gas boosting pump, 4, vacuum meter, 5, six-way valve, 6, vacuum pump, 7, the first hand valve, 8, the second hand valve, 9, the 3rd hand valve, 10, the 4th hand valve, 11, the 5th hand valve, 12, the 6th hand valve, 13, temperature sensor, 14, gas-holder, 15, with reference to still, 16, the first pressure transducer, 17, flow-limiting valve, 18, the first pneumatic valve, 19, the second pneumatic valve, 20, the 3rd pneumatic valve, 21, the 4th pneumatic valve, 22, gas chromatograph, 23, the second pressure transducer, 24, filter screen, 25, sample still, 26, constant temperature control box, 27, mesozone.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described.Obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiment.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtaining under creative work prerequisite, belong to the scope of protection of the invention.
Record known according to background technology part, owing to completing, the needed gas flow of whole adsorption experiment is more, therefore after the adsorbate gas of disposable injection q.s, original pressure with reference to still is very high, and the original pressure of sample still is approximately vacuum, in adsorption experiment process, need progressively step-down with reference to still, the in the situation that of prior art, be difficult to accurately control by valve, in order to realize the progressively step-down process with reference to still, the technical program is provided with mesozone on experimental provision, utilizes mesozone to carry out the method for progressively step-down.Simultaneously for better controlled pressure, at the pipeline installing after still a flow-limiting valve 17.
Concrete technical thought is: in the middle of with reference to still and experiment still, the mesozone of a volume very little (1-2ml) is set, because mesozone volume is long-pending little a lot of with reference to kettle, therefore, even under high-pressure situations, the each pressure increase of sample still is also certain, can be by the gas of valve control mesozone to progressively supercharging in sample still.Like this, in the technical program, mesozone has the effect of following two aspects:
1, utilize mesozone smaller size smaller to realize with reference to the progressively step-down of still, the progressively pressurization of sample still, the method is simple and convenient, pressure controllability is strong; And, in adsorption experiment process, while carrying out single-component gas experiment, due to by mesozone to the adsorbate gas with reference to the disposable injection q.s of still, and by mesozone to progressively reducing pressure with reference to still, sample still is progressively increased to pressure, obtain after multiple different adsorption equilibriums adsorbance corresponding under sample still internal pressure.If conventional art will obtain after 5 different adsorption equilibriums adsorbance corresponding under sample still internal pressure, just need successively 5 times to reference to injecting adsorbate gas in still, technical scheme of the present invention the experimental error of measurement result accumulated, so can reduce the experimental error of measurement result.
2,, in adsorption experiment process, in the time carrying out multicomponent gas experiment, after adsorption equilibrium, utilize mesozone to get gas, and carry out gas composition analysis by gas chromatograph.
As shown in Figure 1, a kind of coal/shale isothermal adsorption experimental provision schematic diagram proposing for the present invention.Described experimental provision comprises: with reference to still 15, sample still 25, the first pressure transducer 16, the second pressure transducer 23, temperature sensor 13, constant temperature control box 26, gas-holder 14 and filter screen 24; Wherein, described experimental provision also comprises: mesozone 27;
The described delivery outlet with reference to still 15 is connected by the first valve 18 with the first port of described mesozone 27, the second port of described mesozone 27 is connected by the second valve 19 with described gas-holder 14, the 3rd port of described mesozone 27 arranges the 3rd valve 20, and the 4th port of described mesozone 27 is connected by the 4th valve 21 with described sample still 25;
Describedly all be arranged in described constant temperature control box 26 with reference to still 15, described sample still 25, described temperature sensor 13, described gas-holder 14 and described mesozone 27;
The equipped at outlet port of described sample still 25 arranges described filter screen 24;
Described the first pressure transducer 16, described with reference to the force value in still 15 for obtaining;
Described the second pressure transducer 23, for obtaining the force value in described sample still 25;
Described temperature sensor 13, for accurately measuring the temperature value of adsorption experiment process;
Described gas-holder 14, describedly carries out thermal pretreatment before with reference to still 15 and described sample still 25 for entering at the required gas of adsorption experiment process;
Described mesozone 27, for described with reference to the progressively step-down of still 15 and the progressively pressurization of described sample still 25.
Optionally, in an embodiment of the present invention, described experimental provision also comprises: gas chromatograph 22;
Described gas chromatograph 22, in the time carrying out multicomponent gas experiment, gets gas by the 3rd valve 20 of described mesozone 27, then carries out gas composition analysis.
Optionally, in an embodiment of the present invention, the volume of described mesozone 27 is the described volume with reference to still 15 1 20 ~ 1 15 .
Optionally, in an embodiment of the present invention, described the first valve 18, described the second valve 19, described the 3rd valve 20 and described the 4th valve 21 are pneumatic valve.
Optionally, in an embodiment of the present invention, described experimental provision also comprises flow-limiting valve 17;
In pipeline between the described delivery outlet with reference to still 15 and described the first valve 18, described flow-limiting valve 17 is set, for controlling the described progressively step-down with reference to still 15.
Taking the adsorption experiment of methane (purity >99.99%) gas on shale as example, the technical program is described in detail below.But these examples can not be understood to the restriction that the present invention can practical range.
In an embodiment of the present invention, adopt experimental provision as shown in Figure 1.The volume of mesozone is 2ml, is 30ml with reference to the volume of still, and the volume of sample still is 60ml.Also can only know the volume sum with reference to still and mesozone, in the time carrying out multicomponent gas experiment, adopt this device to obtain the volume with reference to still by standardization, just can indirectly obtain the volume of mesozone.
In adsorption experiment process, testing sample can be rock core, also can be the particle powder (granularity is generally 80 order~100 orders) after grinding, enter pressure line for fear of rock particles from sample still 25, in the lid of the upper end of sample still 25, be provided with the filter screen 24 of 2 μ m.In order to carry out multicomponent gas adsorption experiment, gas chromatograph 22 can utilize the 3rd port of mesozone 27 to get gas operation, then carries out gas composition analysis.
The detailed process of experiment is as follows: first according to actual formation condition, testing sample is carried out to water balance processing or be put in the drying box of 110 DEG C drying and reaching 12 hours, then utilize micro-electronic balance weighing equilibrium water or dried testing sample quality, rapidly testing sample is positioned in sample still 25, the temperature that constant temperature control box 26 is set is required experimental temperature, next the free space volumes carrying out in sample still 25 is demarcated, and concrete steps are as follows:
1, close the 3rd pneumatic valve 20, close the 4th hand valve 10 and the 6th hand valve 12, open vacuum pump 6, the 5th hand valve 11 and vacuum meter 4, experimental provision system in constant temperature control box 26 is vacuumized, about 1 hour duration, close the 5th hand valve 11 and vacuum pump 6, utilize temperature sensor 13 and vacuum meter 4 to obtain initial temperature and the original pressure of sample still 25;
2, close the second pneumatic valve 19, open the second hand valve 8, the 3rd hand valve 9 and the 4th hand valve 10, gas inject gas-holder in helium steel cylinder 2 14 is carried out to preheating, close the 4th pneumatic valve 21, open the first pneumatic valve 18 and the second pneumatic valve 19, to reference to injecting quantitative helium in still 15, close the second pneumatic valve 19, wait for after pressure stability, obtain the original pressure with reference to still 15 by the first pressure transducer 16, obtain the initial temperature with reference to still 15 by temperature sensor 13;
3, open the 4th pneumatic valve 21, under the effect of pressure, allow helium isothermal enter after sample still 25, close the 4th pneumatic valve 21, wait for pressure equilibrium in two stills and stable after, utilize the first pressure transducer 16 to obtain to demarcate after balances with reference to still pressure, utilize the second pressure transducer 23 to obtain to demarcate sample still pressure after balances, meanwhile, utilize temperature sensor 13 to obtain respectively and demarcate the temperature with reference to still and sample still after balance;
4, in the case of the volume sum of known reference still 15 and mesozone 27, known sample still 25 volumes, according to the principle of mass conservation, calculate the free space volumes in sample still 25.Computing formula is as follows:
V void = ( P 1 Z 1 - P 2 Z 2 ) ( P 3 Z 3 - P 0 Z 0 ) V ref
In formula, P 0for the original pressure of sample still, P 1for the original pressure with reference to still, unit is MPa; P 2for the pressure with reference to still after demarcation balance, P 3for the pressure of sample still after demarcation balance, unit is MPa; Z 0for the compressibility factor of helium under the original pressure of sample still, Z 1for the compressibility factor of helium under the original pressure with reference to still, Z 2for the compressibility factor of helium under the pressure of sample still after demarcation balance, Z 3for the compressibility factor with reference to the helium under the pressure of still after demarcation balance; V refbe the volume sum with reference to still and mesozone, unit is ml; V voidbe free space volumes in sample still, unit is ml.
Next, carry out isothermal adsorption experiment, detailed operation steps is as follows:
1, close the 3rd pneumatic valve 20, the 4th hand valve 10 and the 6th hand valve 12, open vacuum pump 6, the 5th hand valve 11 and vacuum meter 4, experimental provision system in constant temperature control box 26 is vacuumized, about 1 hour duration, close the 5th hand valve 11 and vacuum pump 6, utilize vacuum meter 4 to obtain the original pressure P of sample still 25 0 sam;
2, close the second pneumatic valve 19, open the first hand valve 7, the 3rd hand valve 9 and the 4th hand valve 10, utilize supercharge pump 3 that the methane gas in gas bomb 1 is pressurized to the required pressure of experiment, and inject gas-holder 14 and carry out thermal pretreatment, close the 4th pneumatic valve 21, open the first pneumatic valve 18 and the second pneumatic valve 19, to the methane gas with reference to disposable injection q.s in still 15, close the second pneumatic valve 19, wait for after pressure stability, obtain the original pressure P with reference to still 15 by the first pressure transducer 16 0 ref, obtain the initial temperature with reference to still 15 by temperature sensor 13;
3, close the first pneumatic valve 18, open the 4th pneumatic valve 21, under the effect of pressure, gas isothermal expansion in mesozone 27 enters in sample still 25, after the pressure equilibrium in the pressure in mesozone 27 and sample still 25, close the 4th pneumatic valve 21, open the first pneumatic valve 18, until the pressure in mesozone 27 with reference to after the pressure equilibrium in still 15 stablizing, obtain the pressure P with reference to still 15 by the first pressure transducer 16 1 ref, obtain the pressure P of sample still 25 by the second pressure transducer 23 1 sam;
4, repeat above-mentioned steps 3 i time, record is respectively P with reference to the pressure in still 15 and sample still 25 i ref, P i sam, just can calculate the adsorbance (m mol) of unit testing sample quality corresponding under the pressure of sample still after the i time adsorption equilibrium according to the mass conservation, computing formula is as follows:
n a ( i ) = ( P 0 ref Z 0 ref - P i ref Z i ref ) V ref RT - ( P i sam Z i sam - P 0 sam Z 0 sam ) V void RT
In formula, R is ideal gas constant, is 8.31451J/mol/k; T is experimental temperature, and unit is K; V refthe volume sum with reference to still and mesozone, ml; V voidbe free space volumes in sample still, unit is ml; with reference to still original pressure P 0 refunder the compressibility factor of methane; with reference to still pressure P i refunder the compressibility factor of methane; it is sample still pressure P i samunder methane compressibility factor; the original pressure P of sample still 0 samunder the compressibility factor of methane.
5, obtain the adsorbance (mmol/g) of unit testing sample quality corresponding under the pressure of sample still after adsorption equilibrium according to testing sample Mass Calculation, can draw the adsorption isothermal of shale.
As shown in Figure 2, be the measurement result of the present embodiment and the error of traditional volumetric method measurement result contrast schematic diagram.If carry out adsorption experiment by traditional volumetric method, calculating when adsorbance, be first to calculate single absorption increment, then obtain after adsorption equilibrium corresponding adsorbance under sample still internal pressure by cumulative summation.By the derivation of equation and error analysis, show that the uncertainty of the measurement result of traditional volumetric method is:
σ n a ( i ) = Σ k = 1 i σ Δ n a ( k ) 2 = σ Δn a ( 1 ) 2 + σ Δn a ( 2 ) 2 + . . . + σ Δn a ( i ) 2
Wherein:
σ Δn a ( i ) 2 = ( ρ 2 i - 1 - ρ 2 i ) 2 σ V ref 2 + ( σ ρ 2 i - 1 2 + σ ρ 2 i 2 ) V ref 2 + ( ρ 2 i - ρ 2 i - 2 ) 2 σ V void 2 + ( σ ρ 2 i 2 + σ ρ 2 i - 2 2 ) V viod 2
In formula, Δ n a(i) the single absorption increment while being the i time absorption, unit is mol; ρ 2i-2be the gas density in sample still before the i time adsorption equilibrium, unit is mol/ml; ρ 2i-1be that the i time adsorption equilibrium is front with reference to the gas density in still, unit is mol/ml; ρ 2ibe the gas density in sample still after the i time adsorption equilibrium, unit is mol/ml; σ ρ 2i-2gas density ρ 2i-2standard deviation, unit is mol/ml; σ ρ 2i-1gas density ρ 2i-1standard deviation, unit is mol/ml; σ ρ 2igas density ρ 2istandard deviation, unit is mol/ml; v refstandard deviation, unit is ml; v voidstandard deviation, unit is ml.V refbe the volume sum with reference to still and mesozone, unit is ml; V voidbe free space volumes in sample still, unit is ml.
And for the technical scheme of the present embodiment, in the time calculating adsorbance, be directly to calculate after adsorption equilibrium corresponding adsorbance under sample still internal pressure, by the derivation of equation and error analysis, show that the uncertainty of the measurement result of the technical program is:
σ n a ( i ) = ( ρ 0 ref - ρ i ref ) 2 σ V ref 2 + ( σ ρ 0 ref 2 + σ ρ i ref 2 ) V ref 2 + ( ρ i sam - ρ 0 sam ) 2 σ V void 2 + ( σ ρ i sam 2 + σ ρ 0 sam 2 ) V void 2
In formula, with reference to still original pressure P 0 refunder gas density, unit is mol/ml; with reference to still pressure P i refunder gas density, unit is mol/ml; sample still original pressure P 0 samunder gas density, unit is mol/ml; it is sample still pressure P i samunder gas density, unit is mol/ml; it is gas density standard deviation, unit is mol/ml; it is gas density standard deviation, unit is mol/ml; it is gas density standard deviation, unit is mol/ml; it is gas density standard deviation, unit is mol/ml.
In Fig. 2, numerical value on horizontal ordinate is the force value in sample still after adsorption equilibrium, and unit is MPa, and the numerical value on ordinate is the adsorbance of unit testing sample quality corresponding under the pressure of sample still after adsorption equilibrium, unit is mmol/g, and the line of I shape is experimental error line.Wherein, in Fig. 2, the minimum value of experimental error line is that the uncertainty that absorption value that after adsorption equilibrium, under sample still internal pressure, experiment measuring obtains deducts measurement result obtains, in like manner, in Fig. 2, the maximal value of experimental error line is that the absorption value that after adsorption equilibrium, under sample still internal pressure, experiment measuring obtains adds that the uncertainty of measurement result obtains.By relatively finding, under force value after identical adsorption equilibrium in sample still, the experimental error line at round dot place is shorter than the experimental error line at triangle place, can draw: the experimental error of measurement result of the present invention is far smaller than the experimental error that traditional volumetric method is measured.
Further, the uncertainty formula of more above-mentioned two measurement results is found: the present invention has eliminated error accumulation, under the condition of the equipment of same precision, can make measurement result more accurate, greatly reduces the experimental error of measurement result.
Also have, in the time that the device that adopts Fig. 1 is implemented the experiment flow of the present embodiment, mesozone can be realized with reference to the progressively step-down of still, the progressively supercharging of sample still, solved in prior art, face from a slowly difficult problem for step-down progressively of high pressure, and provide one to solve clearly thinking.And, can effectively reduce gas injection number of times, shorten the adsorption experiment time.
Separately, in the time carrying out multicomponent gas experiment, can get gas by mesozone, carry out gas composition analysis by gas chromatograph, reduce the risk of getting gas under conventional art.
Finally it should be noted that: above-mentioned only in order to the present invention to be described and unrestricted technical scheme described in the invention; Although this instructions has been described in detail to the present invention, but, those skilled in the art still can modify or be equal to replacement the present invention, and all do not depart from technical scheme and the improvement thereof of the spirit and scope of the present invention, and it all should be encompassed in claim scope of the present invention.

Claims (5)

1. coal/shale isothermal adsorption experimental provision, described experimental provision comprises: with reference to still, sample still, the first pressure transducer, the second pressure transducer, temperature sensor, constant temperature control box, gas-holder and filter screen; It is characterized in that, described experimental provision also comprises: mesozone; Wherein,
The described delivery outlet with reference to still is connected by the first valve with the first port of described mesozone, the second port of described mesozone is connected by the second valve with described gas-holder, the 3rd port of described mesozone arranges the 3rd valve, and the 4th port of described mesozone is connected by the 4th valve with described sample still;
Describedly all be arranged in described constant temperature control box with reference to still, described sample still, described temperature sensor, described gas-holder and described mesozone;
The equipped at outlet port of described sample still arranges described filter screen;
Described the first pressure transducer, described with reference to the force value in still for obtaining;
Described the second pressure transducer, for obtaining the force value in described sample still;
Described temperature sensor, for accurately measuring the temperature value of adsorption experiment process;
Described gas-holder carried out thermal pretreatment before entering with reference to still and sample still at the required gas of adsorption experiment process;
Described mesozone, with reference to the progressively step-down of still and the progressively supercharging of described sample still, obtains the adsorbance under sample still pressure different after multiple adsorb balance for described.
2. device as claimed in claim 1, is characterized in that, described experimental provision also comprises: gas chromatograph;
Described gas chromatograph, in the time carrying out multicomponent gas experiment, is got gas by the 3rd valve of described mesozone, then carries out gas composition analysis.
3. device as claimed in claim 1 or 2, is characterized in that, the volume of described mesozone is the described volume with reference to still 1 20 ~ 1 15 .
4. device as claimed in claim 1 or 2, is characterized in that, described the first valve, described the second valve, described the 3rd valve and described the 4th valve are pneumatic valve.
5. device as claimed in claim 1 or 2, is characterized in that, described experimental provision also comprises flow-limiting valve;
In pipeline between the described delivery outlet with reference to still and described the first valve, described flow-limiting valve is set, described with reference to progressively step-down of still for accurately controlling.
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CN106018165A (en) * 2016-07-27 2016-10-12 中国石油大学(北京) Shale multi-component adsorption experimental calculation method
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