CN105588782A - High-low-temperature high-pressure adsorption and desorption testing device and method - Google Patents

High-low-temperature high-pressure adsorption and desorption testing device and method Download PDF

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CN105588782A
CN105588782A CN201610167127.1A CN201610167127A CN105588782A CN 105588782 A CN105588782 A CN 105588782A CN 201610167127 A CN201610167127 A CN 201610167127A CN 105588782 A CN105588782 A CN 105588782A
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pneumatic operated
operated valve
interface
gas
coal sample
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CN105588782B (en
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温志辉
魏建平
王登科
李波
姚邦华
田宣
于世洋
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Henan University of Technology
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Henan University of Technology
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N7/00—Analysing materials by measuring the pressure or volume of a gas or vapour
    • G01N7/02—Analysing materials by measuring the pressure or volume of a gas or vapour by absorption, adsorption, or combustion of components and measurement of the change in pressure or volume of the remainder
    • G01N7/04—Analysing materials by measuring the pressure or volume of a gas or vapour by absorption, adsorption, or combustion of components and measurement of the change in pressure or volume of the remainder by absorption or adsorption alone
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N7/00—Analysing materials by measuring the pressure or volume of a gas or vapour
    • G01N7/14—Analysing materials by measuring the pressure or volume of a gas or vapour by allowing the material to emit a gas or vapour, e.g. water vapour, and measuring a pressure or volume difference

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Abstract

A high-low-temperature high-pressure adsorption and desorption testing device comprises an inflation system, a deflation system, an adsorption system, a desorption system, a temperature control system and a data collection system. The inflation system comprises a methane inflation unit and a helium inflation unit. The deflation system comprises a vacuum pump, a vacuum container and a vacuum gauge. The temperature control system comprises a high temperature unit and a low temperature unit. The adsorption system comprises a high temperature adsorption unit and a low temperature adsorption unit. The desorption system comprises a water drainage metering device, an electronic scale and a desorption gas flowmeter. The data collection system comprises a computer and a control unit. According to the high-low-temperature high-pressure adsorption and desorption testing device, test operations are easy and convenient, the test precision is high, adsorption and desorption tests under different pressures on the high-temperature and low-temperature conditions can be simulated respectively, real-time, accurate and automatic collection of test data is achieved, the more reliable data basis is provided for research on coal gas absorption and desorption rules, and the great practical significance is achieved for efficient gas exhausting, mining and utilization.

Description

High low temperature High Pressure Absorption test device for desorption and method
Technical field
The invention belongs to gas adsorption test device for desorption technical field, relate in particular to the desorb of a kind of high low temperature High Pressure AbsorptionExperimental rig and method.
Background technology
Coal bed gas results from coalification course, is mainly stored in coal seam with adsorbed state. Along with the seam mining degree of depthStrengthen, the micropore of Gas-bearing Coal Seams, hyposmosis, high tax of adsorbing are deposited feature and are more and more displayed. Adopt altogether at coal and gasIn process, gas is difficult to mine safety accidents that extraction causes and energy waste problem and is perplexing the production in colliery. Therefore mouldIntend coal seam, deep storage condition, carry out adsorption and desorption experiment, seek coal seam adsorption gas mechanism, anti-to deep coal-bed gas disasterControl with the exploration and development of coal bed gas and have important theory significance.
Seam gas content is the important foundation data of mine production and scientific research, and the accuracy of its value is gushed for gasOutput prediction, coalbed gas geology evaluation, the coal mine gas comprehensive regulation and fully utilize significant. But survey at gas bearing capacityDetermine in process, drill hole sampling raises coal sample temperature, and coal core Methane Diffusion speed is accelerated, and causes gas bearing capacity measured value on the low side.At present, freezing sampling method becomes a new technological approaches of gas bearing capacity Accurate Determining, therefore, and the gas of coal under low temperature environmentThe research of adsorption-desorption characteristics is just particularly important. Meanwhile, critical-temperature-82.6 DEG C of methane, critical pressure 4.5MPa. CriticalNear point, methane has very strong compressibility, suitably increases the density that pressure can make it and approaches general liquid, and now methane is closeThere is violent variation in the character such as degree, viscosity, solubility, thermal capacity, dielectric constant. Therefore study methane under this environmental conditionPhase-state change and adsorption-desorption characteristics, efficient extraction and the utilization of gas are had important practical significance.
At present, published patent documentation " the high pressure isothermal adsorption experimental provision of coal " (CN202502025U), " transformation barCoal sample gas adsorption desorption experimental apparatus under part " (CN203705293U), " a kind of gas adsorption test device for desorption "(CN103033442A) etc., what all adopt is heating water bath mode, can not carry out the experiment lower than room temperature environment; " a kind of high temperatureHigh Pressure Absorption desorption apparatus and using method thereof " (CN104062204A) to adopt silicone oil be medium thermostatic oil bath mode of heating,Experimental situation is severe, and complicated operation can not carry out the adsorption and desorption experiment under low temperature equally. And said apparatus automaticityLower, the pressure limit that can bear is little, air-tightness deficiency, and the laboratory sample amount that can simultaneously carry out is few, and conventional efficient is low.
Summary of the invention
The present invention is in order to solve weak point of the prior art, provide that a kind of test operation is easy, test accuracy is high,Test data is accurate, can automatic data collection and the high high low temperature High Pressure Absorption test device for desorption of test efficiency.
For solving the problems of the technologies described above, the present invention adopts following technical scheme: high low temperature High Pressure Absorption test device for desorption,Comprise gas charging system, degas system, adsorption system, desorption system, temperature control system and data collecting system;
Gas charging system comprises methane inflation unit and helium inflation unit, and methane inflation unit comprises high pressure methane gas cylinder, methaneAir accumulator and the first five-way valve, be communicated with by high-voltage tube between high pressure methane gas cylinder and methane air accumulator, high pressure methane gas cylinder andOn high-voltage tube between methane air accumulator, connect successively and be provided with the first gas pressure reducer and high pressure gas along methane gas circulating directionBody booster pump, the first five-way valve comprises the first valve body, the first valve body is provided with first interface, the second interface, the 3rd interface, the 4thInterface and the 5th interface, valve body is provided with five interface switches corresponding with the first to the 5th interface, and methane air accumulator passes throughHigh-voltage tube is connected with the 4th interface; Helium inflation unit comprises high pressure helium gas cylinder and the second gas pressure reducer, and high pressure helium gas cylinder is logicalCross high-voltage tube and be connected with the second interface, the second gas pressure reducer is arranged on the high-voltage tube between high pressure helium gas cylinder and the second interfaceOn;
Degas system comprises vavuum pump, vacuum tank, vacuum meter and the second five-way valve, and the second five-way valve comprises the second valve body, theTwo valve bodies are provided with the 6th interface, the 7th interface, the 8th interface, the 9th interface and the tenth interface, and the second valve body is provided with andFive interface switches that six to the tenth interfaces are corresponding, vavuum pump is connected with vacuum tank by high-voltage tube, and vacuum meter is located at veryOn empty, vacuum tank is connected with the 3rd interface by high-voltage tube, the first interface of the first five-way valve and the second five-way valveThe 8th interface connects by high-voltage tube, and the 5th interface of the first five-way valve and the 9th interface of the second five-way valve connect by high-voltage tubeConnect;
Temperature control system comprises high temperature unit and cryogenic unit, and high temperature unit comprises high-temperature incubator and is located at high-temperature incubatorOn the first control panel, the first control panel is provided with the first temperature controller, the first power switch, heater switch, indicator lamp and opensClose and by the heater of heater switch control; Cryogenic unit comprises cryostat and is located at second on cryostat to be controlledPanel, the second control panel is provided with the second temperature controller, second source switch, refrigeration switch and the refrigeration by the control of refrigeration switchUnit;
Adsorption system comprises high temperature adsorption unit and cryogenic absorption unit, and high temperature adsorption unit comprises and being arranged in high-temperature incubatorThe first gas buffer tank and some coal sample tanks, the first gas buffer tank and each coal sample tank are arranged in parallel by tube connector respectivelyOn the high-voltage tube between first interface and the 8th interface, on the high-voltage tube between first interface and the 8th interface along gas communicationDirection is connected successively and is provided with the first pneumatic operated valve and the first pressure sensor, and the first gas buffer tank is provided with the first temperature sensorWith the second pressure sensor, the tube connector connecting on the first gas buffer tank is provided with the second pneumatic operated valve, on each coal sample tank, dividesBe not provided with the second temperature sensor and the 3rd pressure sensor, on the tube connector connecting on each coal sample tank, be respectively equipped with the 3rd gasMoving valve;
Cryogenic absorption unit comprises the second gas buffer tank and the some coal sample tanks that are arranged in cryostat, and the second gas is slowRush tank and each coal sample tank and be arranged in parallel on the high-voltage tube between the 5th interface and the 9th interface by tube connector respectively, the 5thOn high-voltage tube between interface and the 9th interface, connect successively and be provided with the 4th pneumatic operated valve and the 4th pressure biography along gas communication directionSensor, the second gas buffer tank is provided with three-temperature sensor and the 5th pressure sensor, on the second gas buffer tank, connectsTube connector be provided with the 5th pneumatic operated valve, on each coal sample tank, be respectively equipped with the 4th temperature sensor and the 6th pressure sensor,On the tube connector connecting on each coal sample tank, be respectively equipped with the 6th pneumatic operated valve;
Desorption system comprises gas drainage metering device, electronic balance and some desorption gas flowmeters being connected in parallel, and respectively separatesThe range of air absorbing body flowmeter is different, and each desorption gas flowmeter is connected with the 7th interface by high-voltage tube respectively, everyOn high-voltage tube between individual desorption gas flowmeter and the 7th interface, be respectively equipped with the 7th pneumatic operated valve;
Gas drainage metering device comprises tank, drainpipe and collecting container, and tank upper end is by high-voltage tube and the 6thInterface connects, and the high-voltage tube between tank and the 6th interface is provided with the 8th pneumatic operated valve, drainpipe one end and tankBottom is communicated with, and the drainpipe other end is communicated with collecting container top, and collecting container is placed on electronic balance, on the tenth interface, connectsBe connected to evacuated tube, evacuated tube is provided with the 9th pneumatic operated valve;
Data collecting system comprises computer and control module, and control module comprises the 3rd control panel, on the 3rd control panelBe provided with pressure logging, temperature polling instrument, flowmeter display, for control second source switch cryostat switch,For controlling the high-temperature incubator switch of the first power switch, and for the 3rd of controlled pressure logging and temperature polling instrumentPower switch, computer control connect the first gas pressure reducer, the second gas pressure reducer, the first five-way valve, the second five-way valve andThe first to the 9th pneumatic operated valve.
In high temperature adsorption unit, described coal sample tank is five, is respectively the first coal sample tank, the second coal sample tank, the 3rd coal sampleTank, the 4th coal sample tank and the 5th coal sample tank, in cryogenic absorption unit, described coal sample tank is five, is respectively the 6th coal sample tank,Seven coal sample tanks, the 8th coal sample tank, the 9th coal sample tank and the tenth coal sample tank.
In desorption system, described desorption gas flow is counted three, is respectively the first desorption gas flowmeter, the second desorbGas flowmeter and the 3rd desorption gas flowmeter, the range of the first desorption gas flowmeter is 0-2000ml/min, second separatesThe range of air absorbing body flowmeter is 0-500ml/min, and the range of the 3rd desorption gas flowmeter is 0-100ml/min; Described streamAmount meter display is three, is respectively and the first desorption gas flowmeter, the second desorption gas flowmeter, the 3rd desorption gas streamThe first desorption gas flowmeter, the second desorption gas flowmeter, the 3rd desorption gas flowmeter that amount meter is corresponding.
The present invention also aims to provide a kind of test method of high low temperature High Pressure Absorption test device for desorption, respectively mouldIntend the adsorption-desorption test under hot conditions and cryogenic conditions different pressures, and realize test data accurate automatic collection in real time,For research coal body gas adsorption adsorption law, data basis more is reliably provided, efficient extraction and the utilization of gas are hadImportant realistic meaning.
For achieving the above object, the test method of high low temperature High Pressure Absorption test device for desorption of the present invention is wrapped successivelyDraw together following steps:
(1) on down-hole mining working face, drill through block fresh coal sample, after tightly encapsulating, deliver to ground experiment chamber, will be newFresh coal sample is pulverized, is sieved into different granularities, chooses respectively the coal sample of corresponding granularity and carries out real density and measurement of apparent density;
(2) to guarantee that experimental rig connects reliable for checkout facility device, open the second gas pressure reducer, first interface, the second interface,The 5th interface, the first pneumatic operated valve, the second pneumatic operated valve, the 3rd pneumatic operated valve, the 4th pneumatic operated valve, the 5th pneumatic operated valve and the 6th pneumatic operated valve,Helium is filled with to the first gas buffer tank, the second gas buffer tank and the first to the tenth coal sample tank, checkout facility device airtightProperty guarantees that experimental rig air-tightness is good, then closes all gas pressure-reducing valve, pneumatic operated valve and interface; Open first interface,Three interfaces and the 5th interface, open the first pneumatic operated valve, the second pneumatic operated valve, the 3rd pneumatic operated valve, the 4th pneumatic operated valve, the 5th pneumatic operated valve andThe 6th pneumatic operated valve, starts vavuum pump high temperature adsorption unit and cryogenic absorption unit is carried out to degassed processing, until vacuum gauge pressureShow that 20Pa is following more than three hours, then close vavuum pump and all gas pressure-reducing valve, pneumatic operated valve and interface, by electronics skyPlacing flat, at evacuated tube place, is placed on electronic balance and injected water by collecting container, and the port of export of evacuated tube is extend into collectionBelow the water receptacle water surface, record the registration g of electronic balance1, open the 8th interface and the tenth interface, open the 9th pneumatic operated valve,Water in collecting container flows into and fills the high-voltage tube between the first pneumatic operated valve and the 8th interface, records the registration of electronic balanceg2，g1With g2The volume of the corresponding water of difference be the volume of the high-voltage tube between the first pneumatic operated valve and the 8th interface, successivelyOpen the 3rd pneumatic operated valve on the second pneumatic operated valve and the first to the 5th coal sample tank, treat electronic balance after opening corresponding pneumatic operated valve at every turnRegistration stable after, record the registration of electronic balance now and close this pneumatic operated valve, record respectively the quality that flows into water, draw theOne gas buffer tank and the first volume to the 5th coal sample tank, close total interface and pneumatic operated valve, then open the 9th interface andThe tenth interface, opens the 9th pneumatic operated valve, and the water in collecting container flows into and fill the height between the 4th pneumatic operated valve and the 9th interfacePressure pipe, records the registration of electronic balance, calculates the volume of the high-voltage tube between the 4th pneumatic operated valve and the 9th interface, then complies withInferior the 6th pneumatic operated valve of opening on the 5th pneumatic operated valve and the 6th to the tenth coal sample tank is treated electronics sky after opening corresponding pneumatic operated valve at every turnAfter flat registration is stable, records the registration of electronic balance now and close this pneumatic operated valve, recording respectively the quality that flows into water, drawingThe second gas buffer tank and the 6th volume to the tenth coal sample tank;
(3) in the first to the tenth coal sample tank, load coal sample, set in high-temperature incubator by the first temperature controller control heaterTest temperature, set the test temperature in cryostat, high-temperature incubator temperature by the second temperature controller control refrigeration unitIt is 20 DEG C to 80 DEG C that degree arranges scope, and cryostat temperature arranges scope and is-100 DEG C to 20 DEG C, opens on the first five-way valveFirst interface, the 3rd interface and the 5th interface, open the first to the 6th pneumatic operated valve, close all the other interfaces and pneumatic operated valve, startVavuum pump carries out degassed processing to high temperature adsorption unit and cryogenic absorption unit, until vacuum gauge pressure shows that 20Pa is following and protectsHold more than three hours, then close vavuum pump and all pneumatic operated valves and interface, open first interface and the second interface, openOne pneumatic operated valve, open high pressure helium gas cylinder, and high-pressure helium enters high temperature adsorption unit after the second gas pressure reducer reduced pressure treatmentIn high-voltage tube, after the first pressure sensor reading is stable, close the first pneumatic operated valve, open successively on the first to the 5th coal sample tankThe 3rd pneumatic operated valve, treat the 3rd pressure sensor reading and the first pressure on corresponding coal sample tank after opening the 3rd pneumatic operated valve at every turnWhen the registration of sensor is consistent, closes the 3rd pneumatic operated valve on this coal sample tank and record the 3rd pressure sensing on this coal sample tankThe registration of device, and again open the first pneumatic operated valve, open high pressure helium gas cylinder, high-pressure helium is through the second gas pressure reducer decompression placeAfter reason, enter in the high-voltage tube of high temperature adsorption unit, after the first pressure sensor reading is stable, close the first pneumatic operated valve, therebyDraw the first free space volumes to the 5th coal sample tank; Close first interface, open the 5th interface, open the 4th pneumatic operated valve,Open high pressure helium gas cylinder, high-pressure helium enters in the high-voltage tube of cryogenic absorption unit after the second gas pressure reducer reduced pressure treatment,After the 4th pressure sensor reading is stable, close the 4th pneumatic operated valve, open successively the 6th gas on the 6th to the tenth coal sample tankMoving valve is opened the 6th pressure sensor reading treated after the 6th pneumatic operated valve on corresponding coal sample tank and the 4th pressure sensor at every turnWhen registration is consistent, closes the 6th pneumatic operated valve on this coal sample tank and record showing of the 6th pressure sensor on this coal sample tankNumber, and again open the 4th pneumatic operated valve, open high pressure helium gas cylinder, high-pressure helium is laggard through the second gas pressure reducer reduced pressure treatmentEnter in the high-voltage tube of cryogenic absorption unit, after the 4th pressure sensor reading is stable, close the 4th pneumatic operated valve, thereby draw theSix free space volumes to the tenth coal sample tank, close all pneumatic operated valves and interface;
(4) open first interface, the 3rd interface and the 5th interface, open the first pneumatic operated valve, the 3rd pneumatic operated valve, the 4th pneumatic operated valve andThe 6th pneumatic operated valve, starts vavuum pump high temperature adsorption unit and cryogenic absorption unit is carried out to degassed processing, until vacuum gauge pressureShow that 20Pa is following and keep more than three hours, then closing vavuum pump and all pneumatic operated valves and interface, opening high pressure methaneGas cylinder, high pressure methane gas after the first gas pressure reducer reduced pressure treatment again through gases at high pressure booster pump be pressurized to test before by testingThe predetermined adsorptive pressure value that personnel determine is stored in methane air accumulator, opens first interface and the 4th interface, opens the first gasMove valve and the second pneumatic operated valve, the methane gas of predetermined adsorptive pressure value is filled with to the high-voltage tube of the first gas buffer tank and connection thereofIn, after the registration of the first pressure sensor and the second pressure sensor is stablized, close the first pneumatic operated valve and the second pneumatic operated valve, soAfter record the now registration of the first pressure sensor, open successively the 3rd pneumatic operated valve on the first to the 5th coal sample tank, eachOpen the 3rd pressure sensor reading treated after the 3rd pneumatic operated valve on corresponding coal sample tank and the registration of the first pressure sensorAfter relatively stable, close the 3rd pneumatic operated valve on this coal sample tank, and now the 3rd pressure sensor on this coal sample tank of recordRegistration is also closed the 3rd pneumatic operated valve, keeps seven hours, coal sample is fully adsorbed and reach balance, and record is now on this coal sample tankThe registration of the 3rd pressure sensor, and open the second pneumatic operated valve, treat the first pressure sensor and the second pressure sensorAfter registration is stable, closes the second pneumatic operated valve, thereby calculate respectively the methane gas volume being filled with in the first to the 5th coal sample tankAnd methane gas volume under free state, finally obtain adsorbed methane gas volume in the first to the 5th coal sample tank; CloseOne interface, opens the 5th interface, opens the 4th pneumatic operated valve and the 5th pneumatic operated valve, and the methane gas of predetermined adsorptive pressure value is filled withIn the high-voltage tube of the second gas buffer tank and connection thereof, treat that the registration of the 4th pressure sensor and the 5th pressure sensor is stableAfter, close the 4th pneumatic operated valve and the 5th pneumatic operated valve, then record the now registration of the 4th pressure sensor, open successively the 6thTo the 6th pneumatic operated valve on the tenth coal sample tank, treat that the 6th pressure on corresponding coal sample tank passes after opening the 6th pneumatic operated valve at every turnAfter the registration of sensor registration and the 4th pressure sensor is relatively stable, closes the 6th pneumatic operated valve on this coal sample tank, and record thisTime the 6th pressure sensor on this coal sample tank registration and close the 6th pneumatic operated valve, keep seven hours, make coal sample abundantAbsorption reaches balance, and record is the registration of the 6th pressure sensor on this coal sample tank now, and opens the 5th pneumatic operated valve, treats theAfter the registration of four pressure sensors and the 6th pressure sensor is stable, close the 5th pneumatic operated valve, be filled with the thereby calculate respectivelyMethane gas volume in six to the tenth coal sample tanks and the methane gas volume under free state, finally obtain the 6th to the tenth coalAdsorbed methane gas volume in sample tank, closes all pneumatic operated valves and interface;
(5) step (3) and step (4) are adsorbed methane gas volume measuring method, use the method to measure adsorbed methane gasBefore volume, determine in the method the first gas buffer tank and second in high temperature adsorption unit and cryogenic absorption unit by testing crewThe N of a gas buffer tank predetermined adsorptive pressure value, N is less than 10 positive integer, uses adsorbed methane gas volume measuring methodCarry out N step (3) and step (4), under minimum predetermined adsorptive pressure value condition, adopt described adsorbed methane gas volumeMeasuring method operates, and obtains the methane gas volume that adsorbs in the first to the tenth coal sample tank, then increases by gases at high pressureThe force value of the first gas buffer tank and the second gas buffer tank is increased to next predetermined adsorptive pressure value by press pump; Pre-at nextDetermine recuperation under the condition of adsorptive pressure value and carry out step (3) and step (4), until the operation of N step (3) and step (4) is completeCheng Hou, obtains the methane gas volume adsorbing in N the first to the tenth coal sample tank under predetermined adsorptive pressure value;
(6) open first interface, the 3rd interface and the 5th interface, open the first pneumatic operated valve, the 3rd pneumatic operated valve, the 4th pneumatic operated valve andThe 6th pneumatic operated valve, starts vavuum pump high temperature adsorption unit and cryogenic absorption unit is carried out to degassed processing, until vacuum gauge pressureShow that 20Pa is following and keep more than three hours, then closing vavuum pump and all pneumatic operated valves and interface, opening high pressure methaneGas cylinder, high pressure methane gas after the first gas pressure reducer reduced pressure treatment again through gases at high pressure booster pump be pressurized to test before by testingThe predetermined desorption pressures value that personnel determine is stored in methane air accumulator, opens first interface and the 4th interface, opens the first gasMove valve and the second pneumatic operated valve, the methane gas of predetermined desorption pressures value is filled with to the high-voltage tube of the first gas buffer tank and connection thereofIn, after the registration of the first pressure sensor and the second pressure sensor is stablized, close the first pneumatic operated valve and the second pneumatic operated valve, soAfter record the now registration of the first pressure sensor, open successively the 3rd pneumatic operated valve on the first to the 5th coal sample tank, eachOpen the 3rd pressure sensor reading treated after the 3rd pneumatic operated valve on corresponding coal sample tank and the registration of the first pressure sensorAfter relatively stable, close the 3rd pneumatic operated valve on this coal sample tank, and now the 3rd pressure sensor on this coal sample tank of recordRegistration is also closed the 3rd pneumatic operated valve, keeps seven hours, coal sample is fully adsorbed and reach balance, and record is now on this coal sample tankThe registration of the 3rd pressure sensor, and open the second pneumatic operated valve, treat the first pressure sensor and the second pressure sensorAfter registration is stable, closes the second pneumatic operated valve, thereby calculate respectively the methane gas volume being filled with in the first to the 5th coal sample tankAnd methane gas volume under free state, finally obtain adsorbed methane gas volume in the first to the 5th coal sample tank; CloseOne interface, opens the 5th interface, opens the 4th pneumatic operated valve and the 5th pneumatic operated valve, and the methane gas of predetermined desorption pressures value is filled withIn the high-voltage tube of the second gas buffer tank and connection thereof, treat that the registration of the 4th pressure sensor and the 5th pressure sensor is stableAfter, close the 4th pneumatic operated valve and the 5th pneumatic operated valve, then record the now registration of the 4th pressure sensor, open successively the 6thTo the 6th pneumatic operated valve on the tenth coal sample tank, treat that the 6th pressure on corresponding coal sample tank passes after opening the 6th pneumatic operated valve at every turnAfter the registration of sensor registration and the 4th pressure sensor is relatively stable, closes the 6th pneumatic operated valve on this coal sample tank, and record thisTime the 6th pressure sensor on this coal sample tank registration and close the 6th pneumatic operated valve, keep seven hours, make coal sample abundantAbsorption reaches balance, and record is the registration of the 6th pressure sensor on this coal sample tank now, and opens the 5th pneumatic operated valve, treats theAfter the registration of four pressure sensors and the 6th pressure sensor is stable, close the 5th pneumatic operated valve, be filled with the thereby calculate respectivelyMethane gas volume in six to the tenth coal sample tanks and the methane gas volume under free state, finally obtain the 6th to the tenth coalAdsorbed methane gas volume in sample tank, closes all pneumatic operated valves and interface, and coal sample reaches after adsorption equilibrium, open the 6th interface,The 7th interface, the 8th interface, the tenth interface and the 9th pneumatic operated valve, open the 3rd pneumatic on the first to the 5th coal sample tank successivelyValve, respectively the methane gas under free state in the first to the 5th coal sample tank is carried out emptying, open at every turn one the 3rd pneumaticThe 3rd pressure sensor reading after valve on corresponding coal sample tank is 1 o'clock, closes the 9th pneumatic operated valve, adopts computer automatically to controlMake the 7th pneumatic operated valve on the first desorption gas flowmeter, the second desorption gas flowmeter, the 3rd desorption gas flowmeter andThe 8th pneumatic operated valve, first chooses the first desorption gas flowmeter, in the time that methane gas flow is greater than 450ml/min, computer controlledSystem is opened the 7th pneumatic operated valve on the first desorption gas flowmeter, records by the first desorption gas flowmeter the first that desorb goes outAlkane gas volume, in the time that methane gas flow is between 80ml/min-450ml/min, computer is by the second desorption gas flowThe 7th pneumatic operated valve on meter is opened, and records by the second desorption gas flowmeter the methane gas volume that desorb goes out, and works as methane gasBody flow is between 20ml/min-80ml/min time, and computer is opened the 7th pneumatic operated valve on the 3rd desorption gas flowmeter,Record by the 3rd desorption gas flowmeter the methane gas volume that desorb goes out, when methane gas flow is less than 20ml/min, meterCalculation machine is opened the 8th pneumatic operated valve, records the methane gas volume of separating sucking-off, thereby record first by gas drainage metering deviceTo the methane gas volume of separating sucking-off in the 5th coal sample tank; Then close the 8th interface, open the 9th interface and the 9th pneumatic operated valve,Open successively the 6th pneumatic operated valve on the 6th to the tenth coal sample tank, respectively to the first under free state in the 6th to the tenth coal sample tankAlkane gas carries out emptying, treats that the 6th pressure sensor reading on corresponding coal sample tank is zero after opening the 6th pneumatic operated valve at every turnTime, close the 9th pneumatic operated valve, adopt computer controlled automatic the first desorption gas flowmeter, the second desorption gas flowmeter, theThe 7th pneumatic operated valve on three desorption gas flowmeters and the 8th pneumatic operated valve, by the first desorption gas flowmeter, the second desorbGas flowmeter, the gentle drainage metering device of the 3rd desorption gas flowmeter, record and in the 6th to the tenth coal sample tank, separate sucking-offMethane gas volume, whole desorption process Computer Real-time Collection instantaneous delivery and integrated flux, and generated data form andCurve;
(7) step (6) is desorption of methane gas volume measuring method, uses the method to measure before desorption of methane gas volume, byTesting crew is determined in the method the first gas buffer tank and the second gas buffer in high temperature adsorption unit and cryogenic absorption unitThe N of a tank predetermined desorption pressures value, N is less than 10 positive integer, uses desorption of methane gas volume measuring method to carry out N timeStep (6), under minimum predetermined desorption pressures value condition, adopts described desorption of methane gas volume measuring method to graspDo, obtain separating in the first to the tenth coal sample tank the methane gas volume of sucking-off, then pass through gases at high pressure booster pump by the first gasThe force value of body surge tank and the second gas buffer tank is increased to next predetermined desorption pressures value; In next predetermined desorption pressures valueCondition under recuperation carry out step (6), until after the operation of N step (6) completes, obtain under N predetermined desorption pressures valueThe methane gas volume adsorbing in the first to the tenth coal sample tank.
Adopt technique scheme, tool of the present invention has the following advantages:
1, high low temperature High Pressure Absorption test device for desorption of the present invention comprises gas charging system, degas system, adsorption system, desorb systemSystem, temperature control system and data collecting system, gas charging system comprises methane inflation unit and helium inflation unit, methane inflationUnit by using high pressure methane gas cylinder is first by the first gas pressure reducer decompression, then through gases at high pressure booster pump by methane gas pressureBe adjusted to the required pressure of test, and the methane gas that sets force value is filled in methane air accumulator, by methane gas storageTank is to the methane gas that scheduled pressure value is provided in adsorption system, and helium inflation unit utilizes high pressure helium gas cylinder to subtract through the second gasAfter pressure valve reduced pressure treatment, pass in adsorption system, for demarcating the free space volumes of each coal sample tank; Degas system adopts trueEmpty pump carries out degassed processing to adsorption system, guarantees to only have methane gas to participate in test in process of the test, thereby gets rid of itHis interference of gas to result of the test; Temperature control system utilizes high temperature unit in conjunction with the high temperature adsorption unit mould in adsorption systemIntend the methane adsorption-desorption test under hot environment, and utilize cryogenic unit in conjunction with the cryogenic absorption unit simulation in adsorption systemMethane adsorption-desorption test under low temperature environment;
2, desorption system of the present invention adopts desorption gas flowmeter and the gas drainage metering device of three different ranges, is separatingThe suction test initial stage adopts the first desorption gas flowmeter to measure, and along with the flow of desorption gas reduces, adopts successively secondDesorption gas flowmeter, the 3rd desorption gas flowmeter and gas drainage metering device measure, in whole desorption experiment mistakeCheng Zhong, switches according to the big or small automatic control interface of desorption gas flow by computer, and real-time automatic collecting data, hasEffect ground has improved test accuracy, and has reduced operation easier, and test operation is easy, effectively improves test efficiency;
3, high low temperature High Pressure Absorption test device for desorption of the present invention adopts cryogenic unit that the low temperature environment of-100 DEG C can be provided, forThe adsorption-desorption characteristics of research methane under low temperature environment provides experimental condition with the supercritical adsorption of simulation methane;
4, the test method of high low temperature High Pressure Absorption test device for desorption of the present invention, the data acquisition in process of the test and connecingMouth is controlled all computer control, and instrument workflow is presented on interface, and operating personnel set after parameter, and computer canAutomatically gather all pressure, temperature, flow, and treated generation initial data form, analytical table and curve map, effectively avoidThe test error brought of artificial reading and manual record, promoted accuracy and the test efficiency of test, reduced test peopleMember's operation easier;
5, the test method of high low temperature High Pressure Absorption test device for desorption of the present invention can be carried out the not equality of temperature of five groups of coal samples simultaneouslyMethane gas adsorbance under degree, different pressures under condition and the mensuration of methane desorbing gas amount, effectively improved test efficiency,And simulating respectively the methane adsorption-desorption test under hot conditions and cryogenic conditions different pressures, is research coal body gas adsorptionAdsorption law especially under low temperature environment coal gas adsorption-desorption characteristics data basis more is reliably provided, to gasEfficient extraction and utilization have important practical significance.
Brief description of the drawings
Fig. 1 is structural representation of the present invention.
Detailed description of the invention
As shown in Figure 1, high low temperature High Pressure Absorption test device for desorption of the present invention, comprises gas charging system, degas system, suctionAttached system, desorption system, temperature control system and data collecting system.
Gas charging system comprises methane inflation unit and helium inflation unit, methane inflation unit comprise high pressure methane gas cylinder 1,Methane air accumulator 2 and the first five-way valve, be communicated with high pressure first by high-voltage tube 3 between high pressure methane gas cylinder 1 and methane air accumulator 2On high-voltage tube 3 between alkane gas cylinder 1 and methane air accumulator 2, connect successively and be provided with the first gas decompression along methane gas circulating directionValve 4 and gases at high pressure booster pump 5, the first five-way valves comprise that the first valve body 6, the first valve bodies 6 are provided with first interface 7, second and connectMouthfuls 8, the 3rd interface 9, the 4th interface 10 and the 5th interface 11, the first valve bodies 6 be provided with the first to the 5th interface 7,8,9,10,11 corresponding five interface switches (five-way valve is existing conventional components, and its concrete structure no longer describes in detail), methane air accumulator 2 is logicalCrossing high-voltage tube 3 is connected with the 4th interface 10; Helium inflation unit comprises high pressure helium gas cylinder 12 and the second gas pressure reducer 13, high pressureHelium tank 12 is connected with the second interface 8 by high-voltage tube 3, and the second gas pressure reducer 13 is arranged on high pressure helium gas cylinder 12 and second and connectsOn high-voltage tube 3 between mouth 8.
Degas system comprises vavuum pump 14, vacuum tank 15, vacuum meter 16 and the second five-way valve, and the second five-way valve comprisesTwo valve body 17, the second valve bodies 17 are provided with the 6th interface 18, the 7th interface 19, the 8th interface 20, the 9th interface 21 and the tenth and connectMouth 22, the second valve bodies 17 are provided with five interface switches corresponding with the 6th to the tenth interface 18,19,20,21,22,
Vavuum pump 14 is connected with vacuum tank 15 by high-voltage tube 3, and vacuum meter 16 is located on vacuum tank 15, and vacuum tank 15 is logicalCross high-voltage tube 3 and be connected with the 3rd interface 9, the 8th interface 20 of the first interface 7 of the first five-way valve and the second five-way valve is by highPressure pipe 3 connects, and the 5th interface 11 of the first five-way valve is connected by high-voltage tube 3 with the 9th interface 21 of the second five-way valve.
Temperature control system comprises high temperature unit and cryogenic unit, and high temperature unit comprises high-temperature incubator 23 and is located at high temperatureThe first control panel 24, the first control panels 24 on insulating box 23 are provided with the first temperature controller 25, the first power switch 26, addThermal switch 27, indicator light switch 28 and the heater of being controlled by heater switch 27; Cryogenic unit comprises cryostat 29 and establishesThe second control panel 30, the second control panels 30 on cryostat 29 are provided with the second temperature controller 31, second source is openedThe refrigeration unit that closes 32, freezes switch 33 and controlled by refrigeration switch 33; In high temperature unit and cryogenic unit, each several part is existingHave routine techniques, figure does not show heater and refrigeration unit. It is 20 DEG C to 80 DEG C that the temperature of high-temperature incubator 23 arranges scope, high temperatureInsulating box 23 fronts are designed with the rotating single open-door with observation window, and ray lamp is housed in operating room, box outer surface plastic-blasting, interior tableFace adopts stainless steel material, and endless form is hot air convection circulation, and uses the first temperature controller 25 to regulate temperature, for test providesRequired isoperibol; Cryostat 29 adopts three grades of automatic cascaded circulation refrigeration unit refrigeration, can provide-100 DEG C to 20DEG C experimental enviroment, box outer surface plastic-blasting, inner surface adopt stainless steel material, interior wall is provided with refrigerating evaporator, internal stepLadder support is used for placing cryogenic absorption chamber, adopts horizontal type structure to guarantee that ultralow temperature state temperature keeps constant.
Adsorption system comprises high temperature adsorption unit and cryogenic absorption unit, and high temperature adsorption unit comprises and is arranged on high temperature constant temperatureThe first gas buffer tank 34 in case 23 and some coal sample tanks, the first gas buffer tank 34 with each coal sample tank respectively by being connectedPipe 83 is arranged in parallel on the high-voltage tube 3 between first interface 7 and the 8th interface 20, between first interface 7 and the 8th interface 20High-voltage tube 3 on connect successively and be provided with the first pneumatic operated valve 35 and the first pressure sensor 36, the first gases along gas communication directionSurge tank 34 is provided with the connection connecting on the first temperature sensor 37 and the second pressure sensor 38, the first gas buffer tanks 34Pipe 83 is provided with the second pneumatic operated valve 39, is respectively equipped with the second temperature sensor 40 and the 3rd pressure sensor on each coal sample tank41, on the tube connector 83 connecting on each coal sample tank, be respectively equipped with the 3rd pneumatic operated valve 42.
Cryogenic absorption unit comprises the second gas buffer tank 43 and the some coal sample tanks that are arranged in cryostat 29, theTwo gas buffer tanks 43 and each coal sample tank respectively by tube connector 83 be arranged in parallel the 5th interface 11 and the 9th interface 21 itBetween high-voltage tube 3 on, on the high-voltage tube 3 between the 5th interface 11 and the 9th interface 21, connect and be provided with successively along gas communication directionThe 4th pneumatic operated valve 44 and the 4th pressure sensor 45, the second gas buffer tanks 43 are provided with three-temperature sensor 46 and the 5th pressureThe tube connector 83 connecting on power sensor 47, the second gas buffer tanks 43 is provided with the 5th pneumatic operated valve 48, on each coal sample tank, dividesBe not provided with the 4th temperature sensor 49 and the 6th pressure sensor 50, on the tube connector 83 connecting on each coal sample tank, be respectively equipped withThe 6th pneumatic operated valve 51.
Desorption system comprises gas drainage metering device, electronic balance 52 and some desorption gas flows being connected in parallelMeter, the range of each desorption gas flowmeter is different, and each desorption gas flowmeter is respectively by high-voltage tube 3 and the 7th interface19 connect, and on the high-voltage tube 3 between each desorption gas flowmeter and the 7th interface 19, are respectively equipped with the 7th pneumatic operated valve 53.
Gas drainage metering device comprises tank 54, drainpipe 55 and collecting container 56, and tank 54 upper ends are passed throughHigh-voltage tube 3 is connected with the 6th interface 18, and the high-voltage tube 3 between tank 54 and the 6th interface 18 is provided with the 8th pneumatic operated valve57, drainpipe 55 one end are communicated with tank 54 bottoms, and drainpipe 55 other ends are communicated with collecting container 56 tops, the appearance of catchmentingDevice 56 is placed on electronic balance 52, on the tenth interface 22, is connected with evacuated tube 58, and evacuated tube 58 is provided with the 9th pneumatic operated valve 59.
Data collecting system comprises computer 60 and control module, and control module comprises the 3rd control panel 61, the three controlsPanel 61 processed is provided with pressure logging 62, temperature polling instrument 63, flowmeter display, for controlling second source switch 32Cryostat switch 64, for controlling the high-temperature incubator switch 65 of the first power switch 26, and patrol for controlled pressureThe 3rd power switch 66 of inspection instrument 62 and temperature polling instrument 63, computer control connects the first gas pressure reducer 4, the second gas subtractsPressure valve 13, the first five-way valve, the second five-way valve and the first to the 9th pneumatic operated valve 35,39,42,44,48,51,53,57,59. CalculateMachine 60 adopts DelPhi programming, has gas parameter conversion, data analysis function, and instrument workflow is presented on interface, canRealize human-computer dialogue, operating personnel set after parameter, and computer can gather all pressure, temperature, flow automatically, and through locatingReason generates initial data form, analytical statement and curve map.
The methane gas being filled with in high pressure methane gas cylinder 1 is commercially available methane Standard Gases, and volume is 40L/ bottle, purity >=99.99%, the helium being filled with in high pressure helium gas cylinder 12 is commercially available standard helium, and pressure is 15MPa, and volume is 40L/ bottle, high-voltage tube3 withstand voltage is more than 50MPa.
In high temperature adsorption unit, described coal sample tank is five, is respectively the first coal sample tank 67, the second coal sample tank 68, the 3rd coalSample tank 69, the 4th coal sample tank 70 and the 5th coal sample tank 71, in cryogenic absorption unit, described coal sample tank is five, is respectively the 6th coalSample tank 72, the 7th coal sample tank 73, the 8th coal sample tank 74, the 9th coal sample tank 75 and the tenth coal sample tank 76.
In desorption system, described desorption gas flow is counted three, is respectively the first desorption gas flowmeter 77, the second solutionThe range of air absorbing body flowmeter 78 and the 3rd desorption gas flowmeter 79, the first desorption gas flowmeters 77 is 0-2000ml/Min, the range of the second desorption gas flowmeter 78 is 0-500ml/min, the range of the 3rd desorption gas flowmeter 79 is 0-100ml/min; Described flowmeter display is three, is respectively and the first desorption gas flowmeter 77, the second desorption gas streamThe corresponding first flow meter display of amount meter 78, the 3rd desorption gas flowmeter 79 80, the second flowmeter display 81, the 3rdFlowmeter display 82.
Wherein, vavuum pump 14, vacuum tank 15, vacuum meter 16, gases at high pressure booster pump 5, gas pressure reducer, pneumatic operated valve,Five-way valve, temperature sensor, pressure sensor, high-temperature incubator 23, cryostat 29 and desorption gas flowmeter etc. areThe existing routine techniques in this area, its concrete structure no longer describes in detail.
The test method of high low temperature High Pressure Absorption test device for desorption comprises the following steps successively:
(1) on down-hole mining working face, drill through block fresh coal sample, after tightly encapsulating, deliver to ground experiment chamber, by freshCoal sample is pulverized, is sieved into different granularities, chooses respectively the coal sample of corresponding granularity and carries out Industrial Analysis, real density and apparent density etc.The mensuration of parameter;
(2) to guarantee that experimental rig connects reliable for checkout facility device, opens the second gas pressure reducer 13, first interface 7, second connectsMouth 8, the 5th interface 11, the first pneumatic operated valve 35, the second pneumatic operated valve 39, the 3rd pneumatic operated valve 42, the 4th pneumatic operated valve 44, the 5th pneumatic operated valve48 and the 6th pneumatic operated valve 51, helium is filled with to the first gas buffer tank 34, the second gas buffer tank 43 and the first to the tenth coal sampleTank 67,68,69,70,71,72,73,74,75,76, the air-tightness of checkout facility device guarantees that experimental rig air-tightness is good, soAfter close all gas pressure-reducing valve, pneumatic operated valve and interface; Open first interface 7, the 3rd interface 9 and the 5th interface 11, openOne pneumatic operated valve 35, the second pneumatic operated valve 39, the 3rd pneumatic operated valve 42, the 4th pneumatic operated valve 44, the 5th pneumatic operated valve 48 and the 6th pneumatic operated valve 51,Start vavuum pump 14 high temperature adsorption unit and cryogenic absorption unit are carried out to degassed processing, until vacuum meter 16 pressure show 20PaMore than three hours, then close vavuum pump 14 and all gas pressure-reducing valve, pneumatic operated valve and interface below, electronic balance 52 is putPut at evacuated tube 58 places, collecting container 56 is placed on electronic balance 52 and injected water, the port of export of evacuated tube 58 is stretched intoTo below collecting container 56 waters surface, record the registration g of electronic balance 521, open the 8th interface 20 and the tenth interface 22, openThe 9th pneumatic operated valve 59, the water in collecting container 56 flows into and fills the high-voltage tube 3 between the first pneumatic operated valve 35 and the 8th interface 20,Record the registration g of electronic balance 522，g1With g2The volume of the corresponding water of difference be the first pneumatic operated valve 35 and the 8th and connectThe volume of the high-voltage tube 3 between mouth 20, opens the second pneumatic operated valve 39 and the first to the 5th coal sample tank 67,68,69,70,71 successivelyOn the 3rd pneumatic operated valve 42, open after corresponding pneumatic operated valve at every turn registration until electronic balance 52 stable after, record now electronics skyFlat 52 registration is also closed this pneumatic operated valve, records respectively the quality that flows into water, draws the first gas buffer tank 34 and first to theThe volume of five coal sample tanks 67,68,69,70,71, closes total interface and pneumatic operated valve, then opens the 9th interface 21 and the tenth and connectsMouth 22, opens the 9th pneumatic operated valve 59, and the water in collecting container 56 flows into and fills between the 4th pneumatic operated valve 44 and the 9th interface 21High-voltage tube 3, record the registration of electronic balance 52, calculate the high-voltage tube 3 between the 4th pneumatic operated valve 44 and the 9th interface 21Volume, then open successively the 6th pneumatic operated valve on the 5th pneumatic operated valve 48 and the 6th to the tenth coal sample tank 72,73,74,75,7651, open after corresponding pneumatic operated valve at every turn registration until electronic balance 52 stable after, record the registration of electronic balance 52 now and closeClose this pneumatic operated valve, record respectively and flow into the quality of water, draw the second gas buffer tank 43 and the 6th to the tenth coal sample tank 72,73,74,75,76 volume;
(3) in the first to the tenth coal sample tank 67,68,69,70,71,72,73,74,75,76 interior filling coal samples, by the first temperature controlInstrument 25 control heaters are set the test temperature in high-temperature incubator 23, control refrigeration unit set low by the second temperature controller 31Test temperature in temperature insulating box 29, it is 20 DEG C to 80 DEG C that high-temperature incubator 23 temperature arrange scope, cryostat 29 temperatureThe scope that arranges is-100 DEG C to 20 DEG C, opens first interface 7, the 3rd interface 9 and the 5th interface 11, opens first to the 6th pneumaticValve 35,39,42,44,48,51, cuts out all the other interfaces and pneumatic operated valve, starts vavuum pump 14 to high temperature adsorption unit and cryogenic absorptionUnit carries out degassed processing, until vacuum meter 16 pressure show that 20Pa are following and keep more than three hours, then closes vacuumPump 14 and all pneumatic operated valves and interface, open first interface 7 and the second interface 8, opens the first pneumatic operated valve 35, opens high-pressure heliumBottle 12, high-pressure helium enters in the high-voltage tube 3 of high temperature adsorption unit after the second gas pressure reducer 13 reduced pressure treatment, treats the first pressureAfter power sensor 36 registrations are stable, close the first pneumatic operated valve 35, open successively the first to the 5th coal sample tank 67,68,69,70,71On the 3rd pneumatic operated valve 42, open at every turn the 3rd pressure sensor 41 registrations treated after the 3rd pneumatic operated valve 42 on corresponding coal sample tank andWhen the registration of the first pressure sensor 36 is consistent, closes the 3rd pneumatic operated valve 42 on this coal sample tank and record on this coal sample tankThe registration of the 3rd pressure sensor 41, and again open the first pneumatic operated valve 35, opens high pressure helium gas cylinder 12, and high-pressure helium is through theAfter two gas pressure reducer 13 reduced pressure treatment, enter in the high-voltage tube 3 of high temperature adsorption unit, treat that the first pressure sensor 36 registrations are steadyAfter fixed, close the first pneumatic operated valve 35, thereby draw the free space volumes of the first to the 5th coal sample tank 67,68,69,70,71; CloseClose first interface 7, open the 5th interface 11, open the 4th pneumatic operated valve 44, open high pressure helium gas cylinder 12, high-pressure helium is through the second gasAfter body pressure-reducing valve 13 reduced pressure treatment, enter in the high-voltage tube 3 of cryogenic absorption unit, after the 4th pressure sensor 45 registrations are stable,Close the 4th pneumatic operated valve 44, open successively the 6th pneumatic operated valve 51 on the 6th to the tenth coal sample tank 72,73,74,75,76, eachOpen showing of the 6th pressure sensor 50 registrations treated after the 6th pneumatic operated valve 51 on corresponding coal sample tank and the 4th pressure sensor 45Number is when consistent, closes the 6th pneumatic operated valve 51 on this coal sample tank and records showing of the 6th pressure sensor 50 on this coal sample tankNumber, and again open the 4th pneumatic operated valve 44, open high pressure helium gas cylinder 12, high-pressure helium is through the second gas pressure reducer 13 decompressions placeAfter reason, enter in the high-voltage tube 3 of cryogenic absorption unit, after the 4th pressure sensor 45 registrations are stable, close the 4th pneumatic operated valve44, thus draw the free space volumes of the 6th to the tenth coal sample tank 72,73,74,75,76, close all pneumatic operated valves and interface;
(4) open first interface 7, the 3rd interface 9 and the 5th interface 11, open the first pneumatic operated valve 35, the 3rd pneumatic operated valve 42, the 4thPneumatic operated valve 44 and the 6th pneumatic operated valve 51, start vavuum pump 14 high temperature adsorption unit and cryogenic absorption unit carried out to degassed processing,Until vacuum meter 16 pressure show that 20Pa are following and keep more than three hours, then close vavuum pump 14 and all pneumatic operated valves andInterface, opens high pressure methane gas cylinder 1, high pressure methane gas after the first gas pressure reducer 4 reduced pressure treatment again through gases at high pressure superchargingPump 5 is pressurized to the predetermined adsorptive pressure value of being determined by testing crew before test and is stored in methane air accumulator 2, opens first interface7 and the 4th interface 10, open the first pneumatic operated valve 35 and the second pneumatic operated valve 39, the methane gas of predetermined adsorptive pressure value is filled with toIn the high-voltage tube 3 of one gas buffer tank 34 and connection thereof, treat the registration of the first pressure sensor 36 and the second pressure sensor 38After stable, close the first pneumatic operated valve 35 and the second pneumatic operated valve 39, then record the now registration of the first pressure sensor 36, comply withInferior the 3rd pneumatic operated valve 42 of opening on the first to the 5th coal sample tank 67,68,69,70,71 is opened the 3rd pneumatic operated valve 42 at every turnAfter after the registration of the 3rd pressure sensor 41 registrations on corresponding coal sample tank and the first pressure sensor 36 is relatively stable, closeThe 3rd pneumatic operated valve 42 on this coal sample tank, and record now the 3rd pressure sensor 41 on this coal sample tank registration and close thisThe 3rd pneumatic operated valve 42, keeps seven hours, coal sample is fully adsorbed and reach balance, and record is the 3rd pressure on this coal sample tank nowThe registration of sensor 41, and open the second pneumatic operated valve 39, treat showing of the first pressure sensor 36 and the second pressure sensor 38After number is stable, close the second pneumatic operated valve 39, be filled with in the first to the 5th coal sample tank 67,68,69,70,71 thereby calculate respectivelyMethane gas volume and free state under methane gas volume, finally obtain the first to the 5th coal sample tank 67,68,69,70,71 interior adsorbed methane gas volumes; Close first interface 7, open the 5th interface 11, open the 4th pneumatic operated valve 44 and the 5th pneumaticValve 48, is filled with the methane gas of predetermined adsorptive pressure value in the high-voltage tube 3 of the second gas buffer tank 43 and connection thereof, treats the 4thThe registration of pressure sensor 45 and the 5th pressure sensor 47 is closed the 4th pneumatic operated valve 44 and the 5th pneumatic operated valve 48 after stablizing, soAfter record the now registration of the 4th pressure sensor 45, open successively on the 6th to the tenth coal sample tank 72,73,74,75,76The 6th pneumatic operated valve 51, open at every turn the 6th pressure sensor 50 registrations treated after the 6th pneumatic operated valve 51 on corresponding coal sample tank withAfter the registration of the 4th pressure sensor 45 is relatively stable, close the 6th pneumatic operated valve 51 on this coal sample tank, and now this coal of recordThe registration of the 6th pressure sensor 50 on sample tank is also closed the 6th pneumatic operated valve 51, keeps seven hours, and coal sample is fully inhaledThe attached balance that reaches, record is the registration of the 6th pressure sensor 50 on this coal sample tank now, and opens the 5th pneumatic operated valve 48, treatsThe registration of the 4th pressure sensor 45 and the 6th pressure sensor 50 is closed the 5th pneumatic operated valve 48 after stablizing, thereby calculates respectivelyGo out to be filled with methane gas volume in the 6th to the tenth coal sample tank 72,73,74,75,76 and the methane gas body under free stateLong-pending, finally obtain the 6th to the tenth coal sample tank 72,73,74,75,76 interior adsorbed methane gas volumes, close all pneumatic operated valves andInterface;
(5) step (3) and step (4) are adsorbed methane gas volume measuring method, use the method to measure adsorbed methane gasBefore volume, determine in the method the first gas buffer tank 34 and in high temperature adsorption unit and cryogenic absorption unit by testing crewThe N of a two gas buffer tanks 43 predetermined adsorptive pressure value, N is less than 10 positive integer, uses adsorbed methane gas volume to measureMethod is carried out N step (3) and step (4), under minimum predetermined adsorptive pressure value condition, adopts described adsorbed methane gasVolume measuring method operates, and obtains the first to the tenth coal sample tank 67,68,69,70,71,72,73,74,75,76 interior absorptionMethane gas volume, then by gases at high pressure booster pump 5 by the first gas buffer tank 34 and the second gas buffer tank 43Force value is increased to next predetermined adsorptive pressure value; Under the condition of next predetermined adsorptive pressure value recuperation carry out step (3) andStep (4), until after the operation of N step (3) and step (4) completes, obtain first under N predetermined adsorptive pressure value toThe methane gas volume of the tenth coal sample tank 67,68,69,70,71,72,73,74,75,76 interior absorption;
(6) open first interface 7, the 3rd interface 9 and the 5th interface 11, open the first pneumatic operated valve 35, the 3rd pneumatic operated valve 42, the 4thPneumatic operated valve 44 and the 6th pneumatic operated valve 51, start vavuum pump 14 high temperature adsorption unit and cryogenic absorption unit carried out to degassed processing,Until vacuum meter 16 pressure show that 20Pa are following and keep more than three hours, then close vavuum pump 14 and all pneumatic operated valves andInterface, opens high pressure methane gas cylinder 1, high pressure methane gas after the first gas pressure reducer 4 reduced pressure treatment again through gases at high pressure superchargingPump 5 is pressurized to the predetermined desorption pressures value of being determined by testing crew before test and is stored in methane air accumulator 2, opens first interface7 and the 4th interface 10, open the first pneumatic operated valve 35 and the second pneumatic operated valve 39, the methane gas of predetermined desorption pressures value is filled with toIn the high-voltage tube 3 of one gas buffer tank 34 and connection thereof, treat the registration of the first pressure sensor 36 and the second pressure sensor 38After stable, close the first pneumatic operated valve 35 and the second pneumatic operated valve 39, then record the now registration of the first pressure sensor 36, comply withInferior the 3rd pneumatic operated valve 42 of opening on the first to the 5th coal sample tank 67,68,69,70,71 is opened the 3rd pneumatic operated valve 42 at every turnAfter after the registration of the 3rd pressure sensor 41 registrations on corresponding coal sample tank and the first pressure sensor 36 is relatively stable, closeThe 3rd pneumatic operated valve 42 on this coal sample tank, and record now the 3rd pressure sensor 41 on this coal sample tank registration and close thisThe 3rd pneumatic operated valve 42, keeps seven hours, coal sample is fully adsorbed and reach balance, and record is the 3rd pressure on this coal sample tank nowThe registration of sensor 41, and open the second pneumatic operated valve 39, treat showing of the first pressure sensor 36 and the second pressure sensor 38After number is stable, close the second pneumatic operated valve 39, be filled with in the first to the 5th coal sample tank 67,68,69,70,71 thereby calculate respectivelyMethane gas volume and free state under methane gas volume, finally obtain the first to the 5th coal sample tank 67,68,69,70,71 interior adsorbed methane gas volumes; Close first interface 7, open the 5th interface 11, open the 4th pneumatic operated valve 44 and the 5th pneumaticValve 48, is filled with the methane gas of predetermined desorption pressures value in the high-voltage tube 3 of the second gas buffer tank 43 and connection thereof, treats the 4thThe registration of pressure sensor 45 and the 5th pressure sensor 47 is closed the 4th pneumatic operated valve 44 and the 5th pneumatic operated valve 48 after stablizing, soAfter record the now registration of the 4th pressure sensor 45, open successively on the 6th to the tenth coal sample tank 72,73,74,75,76The 6th pneumatic operated valve 51, open at every turn the 6th pressure sensor 50 registrations treated after the 6th pneumatic operated valve 51 on corresponding coal sample tank withAfter the registration of the 4th pressure sensor 45 is relatively stable, close the 6th pneumatic operated valve 51 on this coal sample tank, and now this coal of recordThe registration of the 6th pressure sensor 50 on sample tank is also closed the 6th pneumatic operated valve 51, keeps seven hours, and coal sample is fully inhaledThe attached balance that reaches, record is the registration of the 6th pressure sensor 50 on this coal sample tank now, and opens the 5th pneumatic operated valve 48, treatsThe registration of the 4th pressure sensor 45 and the 6th pressure sensor 50 is closed the 5th pneumatic operated valve 48 after stablizing, thereby calculates respectivelyGo out to be filled with methane gas volume in the 6th to the tenth coal sample tank 72,73,74,75,76 and the methane gas body under free stateLong-pending, finally obtain the 6th to the tenth coal sample tank 72,73,74,75,76 interior adsorbed methane gas volumes, close all pneumatic operated valves andInterface, coal sample reaches after adsorption equilibrium, opens the 6th interface 18, the 7th interface 19, the 8th interface 20, the tenth interface 22 and the 9thPneumatic operated valve 59, opens the 3rd pneumatic operated valve 42 on the first to the 5th coal sample tank 67,68,69,70,71 successively, respectively to first toMethane gas under the 5th coal sample tank 67,68,69,70,71 interior free states carries out emptying, opens the 3rd pneumatic operated valve at every turnThe 3rd pressure sensor 41 registrations after 42 on corresponding coal sample tank are 1 o'clock, close the 9th pneumatic operated valve 59, adopt computer 60Automatically control the on the first desorption gas flowmeter 77, the second desorption gas flowmeter 78, the 3rd desorption gas flowmeter 79Seven pneumatic operated valves 53 and the 8th pneumatic operated valve 57, first choose the first desorption gas flowmeter 77, when methane gas flow is greater thanWhen 450ml/min, computer 60 is controlled the 7th pneumatic operated valve 53 on the first desorption gas flowmeter 77 is opened, by the first solutionAir absorbing body flowmeter 77 records the methane gas volume of separating sucking-off, when methane gas flow is between 80ml/min-450ml/minTime, computer 60 is opened the 7th pneumatic operated valve 53 on the second desorption gas flowmeter 78, by the second desorption gas flowmeter78 record the methane gas volume of separating sucking-off, and in the time that methane gas flow is between 20ml/min-80ml/min, computer 60 willThe 7th pneumatic operated valve 53 on the 3rd desorption gas flowmeter 79 opens, and recorded and separated sucking-off by the 3rd desorption gas flowmeter 79Methane gas volume, when methane gas flow is less than 20ml/min, computer 60 is opened the 8th pneumatic operated valve 57, by gas drainingMetering device records the methane gas volume of separating sucking-off, thereby records the first to the 5th coal sample tank 67,68,69,70,71 interior desorbsThe methane gas volume going out; Then close the 8th interface 20, open the 9th interface 21 and the 9th pneumatic operated valve 59, open successively the 6thTo the 6th pneumatic operated valve 51 on the tenth coal sample tank 72,73,74,75,76, respectively to the 6th to the tenth coal sample tank 72,73,74,75,Methane gas under 76 interior free states carries out emptying, treats on corresponding coal sample tank after opening the 6th pneumatic operated valve 51 at every turnSix pressure sensor 50 registrations are 1 o'clock, close the 9th pneumatic operated valve 59, adopt computer 60 automatically to control the first desorption gas streamThe 7th pneumatic operated valve 53 on amount meter 77, the second desorption gas flowmeter 78, the 3rd desorption gas flowmeter 79 and the 8th pneumaticValve 57, by the first desorption gas flowmeter 77, the second desorption gas flowmeter 78, the gentle row of the 3rd desorption gas flowmeter 79Water metering device, records the methane gas volume of the 6th to the tenth coal sample tank 72,73,74,75,76 interior solution sucking-offs, whole desorbProcess Computer 60 Real-time Collection instantaneous delivery and integrated fluxs, and generated data form and curve;
(7) step (6) is desorption of methane gas volume measuring method, uses the method to measure before desorption of methane gas volume, byTesting crew determines in the method that in high temperature adsorption unit and cryogenic absorption unit, the first gas buffer tank 34 and the second gas are slowN the predetermined desorption pressures value of rushing tank 43, N is less than 10 positive integer, uses desorption of methane gas volume measuring method to carry outN step (6), under minimum predetermined desorption pressures value condition, adopts described desorption of methane gas volume measuring method to carry outOperate, obtain the methane gas volume of the first to the tenth coal sample tank 67,68,69,70,71,72,73,74,75,76 interior solution sucking-offs,Then by gases at high pressure booster pump 5, the force value of the first gas buffer tank 34 and the second gas buffer tank 43 is increased to nextPredetermined desorption pressures value; Under the condition of next predetermined desorption pressures value, step (6) is carried out in recuperation, until N step (6)After having operated, obtain the first to the tenth coal sample tank 67,68,69,70,71,72,73,74 under N predetermined desorption pressures value,75, the methane gas volume of 76 interior absorption.
The present embodiment is not done any pro forma restriction to shape of the present invention, material, structure etc., every according to thisAny simple modification, equivalent variations and modification that bright technical spirit is done above embodiment, all belong to the technology of the present invention sideThe protection domain of case.

Claims (4)

1. high low temperature High Pressure Absorption test device for desorption, is characterized in that: comprise gas charging system, degas system, adsorption system, solutionDesorption system, temperature control system and data collecting system;
Gas charging system comprises methane inflation unit and helium inflation unit, and methane inflation unit comprises high pressure methane gas cylinder, methaneAir accumulator and the first five-way valve, be communicated with by high-voltage tube between high pressure methane gas cylinder and methane air accumulator, high pressure methane gas cylinder andOn high-voltage tube between methane air accumulator, connect successively and be provided with the first gas pressure reducer and high pressure gas along methane gas circulating directionBody booster pump, the first five-way valve comprises the first valve body, the first valve body is provided with first interface, the second interface, the 3rd interface, the 4thInterface and the 5th interface, valve body is provided with five interface switches corresponding with the first to the 5th interface, and methane air accumulator passes throughHigh-voltage tube is connected with the 4th interface; Helium inflation unit comprises high pressure helium gas cylinder and the second gas pressure reducer, and high pressure helium gas cylinder is logicalCross high-voltage tube and be connected with the second interface, the second gas pressure reducer is arranged on the high-voltage tube between high pressure helium gas cylinder and the second interfaceOn;
Degas system comprises vavuum pump, vacuum tank, vacuum meter and the second five-way valve, and the second five-way valve comprises the second valve body, theTwo valve bodies are provided with the 6th interface, the 7th interface, the 8th interface, the 9th interface and the tenth interface, and the second valve body is provided with andFive interface switches that six to the tenth interfaces are corresponding, vavuum pump is connected with vacuum tank by high-voltage tube, and vacuum meter is located at veryOn empty, vacuum tank is connected with the 3rd interface by high-voltage tube, the first interface of the first five-way valve and the second five-way valveThe 8th interface connects by high-voltage tube, and the 5th interface of the first five-way valve and the 9th interface of the second five-way valve connect by high-voltage tubeConnect;
Temperature control system comprises high temperature unit and cryogenic unit, and high temperature unit comprises high-temperature incubator and is located at high-temperature incubatorOn the first control panel, the first control panel is provided with the first temperature controller, the first power switch, heater switch, indicator lamp and opensClose and by the heater of heater switch control; Cryogenic unit comprises cryostat and is located at second on cryostat to be controlledPanel, the second control panel is provided with the second temperature controller, second source switch, refrigeration switch and the refrigeration by the control of refrigeration switchUnit;
Adsorption system comprises high temperature adsorption unit and cryogenic absorption unit, and high temperature adsorption unit comprises and being arranged in high-temperature incubatorThe first gas buffer tank and some coal sample tanks, the first gas buffer tank and each coal sample tank are arranged in parallel by tube connector respectivelyOn the high-voltage tube between first interface and the 8th interface, on the high-voltage tube between first interface and the 8th interface along gas communicationDirection is connected successively and is provided with the first pneumatic operated valve and the first pressure sensor, and the first gas buffer tank is provided with the first temperature sensorWith the second pressure sensor, the tube connector connecting on the first gas buffer tank is provided with the second pneumatic operated valve, on each coal sample tank, dividesBe not provided with the second temperature sensor and the 3rd pressure sensor, on the tube connector connecting on each coal sample tank, be respectively equipped with the 3rd gasMoving valve;
Cryogenic absorption unit comprises the second gas buffer tank and the some coal sample tanks that are arranged in cryostat, and the second gas is slowRush tank and each coal sample tank and be arranged in parallel on the high-voltage tube between the 5th interface and the 9th interface by tube connector respectively, the 5thOn high-voltage tube between interface and the 9th interface, connect successively and be provided with the 4th pneumatic operated valve and the 4th pressure biography along gas communication directionSensor, the second gas buffer tank is provided with three-temperature sensor and the 5th pressure sensor, on the second gas buffer tank, connectsTube connector be provided with the 5th pneumatic operated valve, on each coal sample tank, be respectively equipped with the 4th temperature sensor and the 6th pressure sensor,On the tube connector connecting on each coal sample tank, be respectively equipped with the 6th pneumatic operated valve;
Desorption system comprises gas drainage metering device, electronic balance and some desorption gas flowmeters being connected in parallel, and respectively separatesThe range of air absorbing body flowmeter is different, and each desorption gas flowmeter is connected with the 7th interface by high-voltage tube respectively, everyOn high-voltage tube between individual desorption gas flowmeter and the 7th interface, be respectively equipped with the 7th pneumatic operated valve;
Gas drainage metering device comprises tank, drainpipe and collecting container, and tank upper end is by high-voltage tube and the 6thInterface connects, and the high-voltage tube between tank and the 6th interface is provided with the 8th pneumatic operated valve, drainpipe one end and tankBottom is communicated with, and the drainpipe other end is communicated with collecting container top, and collecting container is placed on electronic balance, on the tenth interface, connectsBe connected to evacuated tube, evacuated tube is provided with the 9th pneumatic operated valve;
Data collecting system comprises computer and control module, and control module comprises the 3rd control panel, on the 3rd control panelBe provided with pressure logging, temperature polling instrument, flowmeter display, for control second source switch cryostat switch,For controlling the high-temperature incubator switch of the first power switch, and for the 3rd of controlled pressure logging and temperature polling instrumentPower switch, computer control connect the first gas pressure reducer, the second gas pressure reducer, the first five-way valve, the second five-way valve andThe first to the 9th pneumatic operated valve.
2. high low temperature High Pressure Absorption test device for desorption according to claim 1, is characterized in that: in high temperature adsorption unitDescribed coal sample tank is five, is respectively the first coal sample tank, the second coal sample tank, the 3rd coal sample tank, the 4th coal sample tank and the 5th coal sampleTank, in cryogenic absorption unit, described coal sample tank is five, is respectively the 6th coal sample tank, the 7th coal sample tank, the 8th coal sample tank, the 9thCoal sample tank and the tenth coal sample tank.
3. high low temperature High Pressure Absorption test device for desorption according to claim 1 and 2, is characterized in that: in desorption systemDescribed desorption gas flow is counted three, is respectively the first desorption gas flowmeter, the second desorption gas flowmeter and the 3rd solutionAir absorbing body flowmeter, the range of the first desorption gas flowmeter is 0-2000ml/min, the range of the second desorption gas flowmeterFor 0-500ml/min, the range of the 3rd desorption gas flowmeter is 0-100ml/min; Described flowmeter display is three, pointWei be not corresponding with the first desorption gas flowmeter, the second desorption gas flowmeter, the 3rd desorption gas flowmeter first separateAir absorbing body flowmeter, the second desorption gas flowmeter, the 3rd desorption gas flowmeter.
4. the test method that adopts high low temperature High Pressure Absorption test device for desorption claimed in claim 3, is characterized in that: successivelyComprise the following steps:
(1) on down-hole mining working face, drill through block fresh coal sample, after tightly encapsulating, deliver to ground experiment chamber, by freshCoal sample is pulverized, is sieved into different granularities, chooses respectively the coal sample of corresponding granularity and carries out real density and measurement of apparent density;
(2) to guarantee that experimental rig connects reliable for checkout facility device, open the second gas pressure reducer, first interface, the second interface,The 5th interface, the first pneumatic operated valve, the second pneumatic operated valve, the 3rd pneumatic operated valve, the 4th pneumatic operated valve, the 5th pneumatic operated valve and the 6th pneumatic operated valve,Helium is filled with to the first gas buffer tank, the second gas buffer tank and the first to the tenth coal sample tank, checkout facility device airtightProperty guarantees that experimental rig air-tightness is good, then closes all gas pressure-reducing valve, pneumatic operated valve and interface; Open first interface,Three interfaces and the 5th interface, open the first pneumatic operated valve, the second pneumatic operated valve, the 3rd pneumatic operated valve, the 4th pneumatic operated valve, the 5th pneumatic operated valve andThe 6th pneumatic operated valve, starts vavuum pump high temperature adsorption unit and cryogenic absorption unit is carried out to degassed processing, until vacuum gauge pressureShow that 20Pa is following more than three hours, then close vavuum pump and all gas pressure-reducing valve, pneumatic operated valve and interface, by electronics skyPlacing flat, at evacuated tube place, is placed on electronic balance and injected water by collecting container, and the port of export of evacuated tube is extend into collectionBelow the water receptacle water surface, record the registration g of electronic balance1, open the 8th interface and the tenth interface, open the 9th pneumatic operated valve,Water in collecting container flows into and fills the high-voltage tube between the first pneumatic operated valve and the 8th interface, records the registration of electronic balanceg2，g1With g2The volume of the corresponding water of difference be the volume of the high-voltage tube between the first pneumatic operated valve and the 8th interface, successivelyOpen the 3rd pneumatic operated valve on the second pneumatic operated valve and the first to the 5th coal sample tank, treat electronic balance after opening corresponding pneumatic operated valve at every turnRegistration stable after, record the registration of electronic balance now and close this pneumatic operated valve, record respectively the quality that flows into water, draw theOne gas buffer tank and the first volume to the 5th coal sample tank, close total interface and pneumatic operated valve, then open the 9th interface andThe tenth interface, opens the 9th pneumatic operated valve, and the water in collecting container flows into and fill the height between the 4th pneumatic operated valve and the 9th interfacePressure pipe, records the registration of electronic balance, calculates the volume of the high-voltage tube between the 4th pneumatic operated valve and the 9th interface, then complies withInferior the 6th pneumatic operated valve of opening on the 5th pneumatic operated valve and the 6th to the tenth coal sample tank is treated electronics sky after opening corresponding pneumatic operated valve at every turnAfter flat registration is stable, records the registration of electronic balance now and close this pneumatic operated valve, recording respectively the quality that flows into water, drawingThe second gas buffer tank and the 6th volume to the tenth coal sample tank;
(3) in the first to the tenth coal sample tank, load coal sample, set in high-temperature incubator by the first temperature controller control heaterTest temperature, set the test temperature in cryostat, high-temperature incubator temperature by the second temperature controller control refrigeration unitIt is 20 DEG C to 80 DEG C that degree arranges scope, and cryostat temperature arranges scope and is-100 DEG C to 20 DEG C, opens on the first five-way valveFirst interface, the 3rd interface and the 5th interface, open the first to the 6th pneumatic operated valve, close all the other interfaces and pneumatic operated valve, startVavuum pump carries out degassed processing to high temperature adsorption unit and cryogenic absorption unit, until vacuum gauge pressure shows that 20Pa is following and protectsHold more than three hours, then close vavuum pump and all pneumatic operated valves and interface, open first interface and the second interface, openOne pneumatic operated valve, open high pressure helium gas cylinder, and high-pressure helium enters high temperature adsorption unit after the second gas pressure reducer reduced pressure treatmentIn high-voltage tube, after the first pressure sensor reading is stable, close the first pneumatic operated valve, open successively on the first to the 5th coal sample tankThe 3rd pneumatic operated valve, treat the 3rd pressure sensor reading and the first pressure on corresponding coal sample tank after opening the 3rd pneumatic operated valve at every turnWhen the registration of sensor is consistent, closes the 3rd pneumatic operated valve on this coal sample tank and record the 3rd pressure sensing on this coal sample tankThe registration of device, and again open the first pneumatic operated valve, open high pressure helium gas cylinder, high-pressure helium is through the second gas pressure reducer decompression placeAfter reason, enter in the high-voltage tube of high temperature adsorption unit, after the first pressure sensor reading is stable, close the first pneumatic operated valve, therebyDraw the first free space volumes to the 5th coal sample tank; Close first interface, open the 5th interface, open the 4th pneumatic operated valve,Open high pressure helium gas cylinder, high-pressure helium enters in the high-voltage tube of cryogenic absorption unit after the second gas pressure reducer reduced pressure treatment,After the 4th pressure sensor reading is stable, close the 4th pneumatic operated valve, open successively the 6th gas on the 6th to the tenth coal sample tankMoving valve is opened the 6th pressure sensor reading treated after the 6th pneumatic operated valve on corresponding coal sample tank and the 4th pressure sensor at every turnWhen registration is consistent, closes the 6th pneumatic operated valve on this coal sample tank and record showing of the 6th pressure sensor on this coal sample tankNumber, and again open the 4th pneumatic operated valve, open high pressure helium gas cylinder, high-pressure helium is laggard through the second gas pressure reducer reduced pressure treatmentEnter in the high-voltage tube of cryogenic absorption unit, after the 4th pressure sensor reading is stable, close the 4th pneumatic operated valve, thereby draw theSix free space volumes to the tenth coal sample tank, close all pneumatic operated valves and interface;
(4) open first interface, the 3rd interface and the 5th interface, open the first pneumatic operated valve, the 3rd pneumatic operated valve, the 4th pneumatic operated valve andThe 6th pneumatic operated valve, starts vavuum pump high temperature adsorption unit and cryogenic absorption unit is carried out to degassed processing, until vacuum gauge pressureShow that 20Pa is following and keep more than three hours, then closing vavuum pump and all pneumatic operated valves and interface, opening high pressure methaneGas cylinder, high pressure methane gas after the first gas pressure reducer reduced pressure treatment again through gases at high pressure booster pump be pressurized to test before by testingThe predetermined adsorptive pressure value that personnel determine is stored in methane air accumulator, opens first interface and the 4th interface, opens the first gasMove valve and the second pneumatic operated valve, the methane gas of predetermined adsorptive pressure value is filled with to the high-voltage tube of the first gas buffer tank and connection thereofIn, after the registration of the first pressure sensor and the second pressure sensor is stablized, close the first pneumatic operated valve and the second pneumatic operated valve, soAfter record the now registration of the first pressure sensor, open successively the 3rd pneumatic operated valve on the first to the 5th coal sample tank, eachOpen the 3rd pressure sensor reading treated after the 3rd pneumatic operated valve on corresponding coal sample tank and the registration of the first pressure sensorAfter relatively stable, close the 3rd pneumatic operated valve on this coal sample tank, and now the 3rd pressure sensor on this coal sample tank of recordRegistration is also closed the 3rd pneumatic operated valve, keeps seven hours, coal sample is fully adsorbed and reach balance, and record is now on this coal sample tankThe registration of the 3rd pressure sensor, and open the second pneumatic operated valve, treat the first pressure sensor and the second pressure sensorAfter registration is stable, closes the second pneumatic operated valve, thereby calculate respectively the methane gas volume being filled with in the first to the 5th coal sample tankAnd methane gas volume under free state, finally obtain adsorbed methane gas volume in the first to the 5th coal sample tank; CloseOne interface, opens the 5th interface, opens the 4th pneumatic operated valve and the 5th pneumatic operated valve, and the methane gas of predetermined adsorptive pressure value is filled withIn the high-voltage tube of the second gas buffer tank and connection thereof, treat that the registration of the 4th pressure sensor and the 5th pressure sensor is stableAfter, close the 4th pneumatic operated valve and the 5th pneumatic operated valve, then record the now registration of the 4th pressure sensor, open successively the 6thTo the 6th pneumatic operated valve on the tenth coal sample tank, treat that the 6th pressure on corresponding coal sample tank passes after opening the 6th pneumatic operated valve at every turnAfter the registration of sensor registration and the 4th pressure sensor is relatively stable, closes the 6th pneumatic operated valve on this coal sample tank, and record thisTime the 6th pressure sensor on this coal sample tank registration and close the 6th pneumatic operated valve, keep seven hours, make coal sample abundantAbsorption reaches balance, and record is the registration of the 6th pressure sensor on this coal sample tank now, and opens the 5th pneumatic operated valve, treats theAfter the registration of four pressure sensors and the 6th pressure sensor is stable, close the 5th pneumatic operated valve, be filled with the thereby calculate respectivelyMethane gas volume in six to the tenth coal sample tanks and the methane gas volume under free state, finally obtain the 6th to the tenth coalAdsorbed methane gas volume in sample tank, closes all pneumatic operated valves and interface;
(5) step (3) and step (4) are adsorbed methane gas volume measuring method, use the method to measure adsorbed methane gasBefore volume, determine in the method the first gas buffer tank and second in high temperature adsorption unit and cryogenic absorption unit by testing crewThe N of a gas buffer tank predetermined adsorptive pressure value, N is less than 10 positive integer, uses adsorbed methane gas volume measuring methodCarry out N step (3) and step (4), under minimum predetermined adsorptive pressure value condition, adopt described adsorbed methane gas volumeMeasuring method operates, and obtains the methane gas volume that adsorbs in the first to the tenth coal sample tank, then increases by gases at high pressureThe force value of the first gas buffer tank and the second gas buffer tank is increased to next predetermined adsorptive pressure value by press pump; Pre-at nextDetermine recuperation under the condition of adsorptive pressure value and carry out step (3) and step (4), until the operation of N step (3) and step (4) is completeCheng Hou, obtains the methane gas volume adsorbing in N the first to the tenth coal sample tank under predetermined adsorptive pressure value;
(6) open first interface, the 3rd interface and the 5th interface, open the first pneumatic operated valve, the 3rd pneumatic operated valve, the 4th pneumatic operated valve andThe 6th pneumatic operated valve, starts vavuum pump high temperature adsorption unit and cryogenic absorption unit is carried out to degassed processing, until vacuum gauge pressureShow that 20Pa is following and keep more than three hours, then closing vavuum pump and all pneumatic operated valves and interface, opening high pressure methaneGas cylinder, high pressure methane gas after the first gas pressure reducer reduced pressure treatment again through gases at high pressure booster pump be pressurized to test before by testingThe predetermined desorption pressures value that personnel determine is stored in methane air accumulator, opens first interface and the 4th interface, opens the first gasMove valve and the second pneumatic operated valve, the methane gas of predetermined desorption pressures value is filled with to the high-voltage tube of the first gas buffer tank and connection thereofIn, after the registration of the first pressure sensor and the second pressure sensor is stablized, close the first pneumatic operated valve and the second pneumatic operated valve, soAfter record the now registration of the first pressure sensor, open successively the 3rd pneumatic operated valve on the first to the 5th coal sample tank, eachOpen the 3rd pressure sensor reading treated after the 3rd pneumatic operated valve on corresponding coal sample tank and the registration of the first pressure sensorAfter relatively stable, close the 3rd pneumatic operated valve on this coal sample tank, and now the 3rd pressure sensor on this coal sample tank of recordRegistration is also closed the 3rd pneumatic operated valve, keeps seven hours, coal sample is fully adsorbed and reach balance, and record is now on this coal sample tankThe registration of the 3rd pressure sensor, and open the second pneumatic operated valve, treat the first pressure sensor and the second pressure sensorAfter registration is stable, closes the second pneumatic operated valve, thereby calculate respectively the methane gas volume being filled with in the first to the 5th coal sample tankAnd methane gas volume under free state, finally obtain adsorbed methane gas volume in the first to the 5th coal sample tank; CloseOne interface, opens the 5th interface, opens the 4th pneumatic operated valve and the 5th pneumatic operated valve, and the methane gas of predetermined desorption pressures value is filled withIn the high-voltage tube of the second gas buffer tank and connection thereof, treat that the registration of the 4th pressure sensor and the 5th pressure sensor is stableAfter, close the 4th pneumatic operated valve and the 5th pneumatic operated valve, then record the now registration of the 4th pressure sensor, open successively the 6thTo the 6th pneumatic operated valve on the tenth coal sample tank, treat that the 6th pressure on corresponding coal sample tank passes after opening the 6th pneumatic operated valve at every turnAfter the registration of sensor registration and the 4th pressure sensor is relatively stable, closes the 6th pneumatic operated valve on this coal sample tank, and record thisTime the 6th pressure sensor on this coal sample tank registration and close the 6th pneumatic operated valve, keep seven hours, make coal sample abundantAbsorption reaches balance, and record is the registration of the 6th pressure sensor on this coal sample tank now, and opens the 5th pneumatic operated valve, treats theAfter the registration of four pressure sensors and the 6th pressure sensor is stable, close the 5th pneumatic operated valve, be filled with the thereby calculate respectivelyMethane gas volume in six to the tenth coal sample tanks and the methane gas volume under free state, finally obtain the 6th to the tenth coalAdsorbed methane gas volume in sample tank, closes all pneumatic operated valves and interface, and coal sample reaches after adsorption equilibrium, open the 6th interface,The 7th interface, the 8th interface, the tenth interface and the 9th pneumatic operated valve, open the 3rd pneumatic on the first to the 5th coal sample tank successivelyValve, respectively the methane gas under free state in the first to the 5th coal sample tank is carried out emptying, open at every turn one the 3rd pneumaticThe 3rd pressure sensor reading after valve on corresponding coal sample tank is 1 o'clock, closes the 9th pneumatic operated valve, adopts computer automatically to controlMake the 7th pneumatic operated valve on the first desorption gas flowmeter, the second desorption gas flowmeter, the 3rd desorption gas flowmeter andThe 8th pneumatic operated valve, first chooses the first desorption gas flowmeter, in the time that methane gas flow is greater than 450ml/min, computer controlledSystem is opened the 7th pneumatic operated valve on the first desorption gas flowmeter, records by the first desorption gas flowmeter the first that desorb goes outAlkane gas volume, in the time that methane gas flow is between 80ml/min-450ml/min, computer is by the second desorption gas flowThe 7th pneumatic operated valve on meter is opened, and records by the second desorption gas flowmeter the methane gas volume that desorb goes out, and works as methane gasBody flow is between 20ml/min-80ml/min time, and computer is opened the 7th pneumatic operated valve on the 3rd desorption gas flowmeter,Record by the 3rd desorption gas flowmeter the methane gas volume that desorb goes out, when methane gas flow is less than 20ml/min, meterCalculation machine is opened the 8th pneumatic operated valve, records the methane gas volume of separating sucking-off, thereby record first by gas drainage metering deviceTo the methane gas volume of separating sucking-off in the 5th coal sample tank; Then close the 8th interface, open the 9th interface and the 9th pneumatic operated valve,Open successively the 6th pneumatic operated valve on the 6th to the tenth coal sample tank, respectively to the first under free state in the 6th to the tenth coal sample tankAlkane gas carries out emptying, treats that the 6th pressure sensor reading on corresponding coal sample tank is zero after opening the 6th pneumatic operated valve at every turnTime, close the 9th pneumatic operated valve, adopt computer controlled automatic the first desorption gas flowmeter, the second desorption gas flowmeter, theThe 7th pneumatic operated valve on three desorption gas flowmeters and the 8th pneumatic operated valve, by the first desorption gas flowmeter, the second desorbGas flowmeter, the gentle drainage metering device of the 3rd desorption gas flowmeter, record and in the 6th to the tenth coal sample tank, separate sucking-offMethane gas volume, whole desorption process Computer Real-time Collection instantaneous delivery and integrated flux, and generated data form andCurve;
(7) step (6) is desorption of methane gas volume measuring method, uses the method to measure before desorption of methane gas volume, byTesting crew is determined in the method the first gas buffer tank and the second gas buffer in high temperature adsorption unit and cryogenic absorption unitThe N of a tank predetermined desorption pressures value, N is less than 10 positive integer, uses desorption of methane gas volume measuring method to carry out N timeStep (6), under minimum predetermined desorption pressures value condition, adopts described desorption of methane gas volume measuring method to graspDo, obtain separating in the first to the tenth coal sample tank the methane gas volume of sucking-off, then pass through gases at high pressure booster pump by the first gasThe force value of body surge tank and the second gas buffer tank is increased to next predetermined desorption pressures value; In next predetermined desorption pressures valueCondition under recuperation carry out step (6), until after the operation of N step (6) completes, obtain under N predetermined desorption pressures valueThe methane gas volume adsorbing in the first to the tenth coal sample tank.
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