CN105588782B - High/low temperature High Pressure Absorption test device for desorption and method - Google Patents

High/low temperature High Pressure Absorption test device for desorption and method Download PDF

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CN105588782B
CN105588782B CN201610167127.1A CN201610167127A CN105588782B CN 105588782 B CN105588782 B CN 105588782B CN 201610167127 A CN201610167127 A CN 201610167127A CN 105588782 B CN105588782 B CN 105588782B
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interface
gas
coal sample
desorption
pneumatic operated
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CN105588782A (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

Abstract

High/low temperature High Pressure Absorption test device for desorption, including inflation system, degassing system, adsorption system, desorption system, temperature control system and data collecting system, inflation system includes methane inflation unit and helium inflation unit, degassing system includes vacuum pump, vacuum tank, vacuum meter, temperature control system includes high temperature unit and cryogenic unit, adsorption system includes high temperature adsorption unit and low temperature adsorption unit, desorption system includes gas drainage metering device, electronic balance and stripping gas flowmeter body, and data collecting system includes computer and control unit.Test operation of the present invention is easy, test accuracy is high, the adsorption-desorption experiment under hot conditions and cryogenic conditions different pressures can be simulated respectively, and realize test data accurate automatic collection in real time, to study coal body gas adsorption adsorption law, relatively reliable data basis is provided, the efficient extraction and utilization to gas have important practical significance.

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, more particularly to a kind of high/low temperature High Pressure Absorption to desorb Experimental rig and method.
Background technology
Coal bed gas is resulted from coalification course, is mainly stored in adsorbed state in coal seam.With seam mining depth Increase, the micropore of Gas-bearing Coal Seams, hyposmosis, the bearing features of high absorption increasingly display.In coal and gas power phenomenon During, gas is difficult to mine safety accidents caused by extraction and energy waste problem annoyings the production in colliery.Therefore mould Intend deep fractures storage condition, carry out adsorption and desorption experiment, seek coal seam adsorption gas mechanism, deep fractures Gas Disaster is prevented Control has important theory significance with the exploration and development of coal bed gas.
Seam gas content is the important foundation data of shaft production and scientific research, and the accuracy of its value is gushed for gas Output prediction, coalbed gas geology evaluation, the coal mine gas comprehensive regulation and comprehensive utilization are of great significance.But surveyed in gas bearing capacity During fixed, drill hole sampling raises coal sample temperature, and coal core Methane Diffusion speed is accelerated, and causes gas bearing capacity measured value relatively low. At present, freezing sampling method becomes a new technological approaches of gas bearing capacity Accurate Determining, therefore, the gas of coal under low temperature environment The research of adsorption-desorption characteristics with regard to it is particularly important that.Meanwhile -82.6 DEG C of the critical-temperature of methane, critical pressure 4.5MPa.Critical Near point, methane has very strong compressibility, and appropriate increase pressure can make its density, and close to general liquid, methane is close at this time Violent change occurs for the properties such as degree, viscosity, solubility, thermal capacity, dielectric constant.Therefore research methane is under the environmental condition Phase-state change and adsorption-desorption characteristics, efficient extraction to gas and using having important practical significance.
At present, it has been disclosed that patent document " the high pressure adsorption isotherm experiment device of coal "（CN202502025U）, " become press strip Coal sample gas adsorption desorption experimental apparatus under part "（CN203705293U）, " a kind of gas adsorption test device for desorption " （CN103033442A）Deng all using heating water bath mode, it is impossible to carry out the experiment less than room temperature environment；A kind of " high temperature High Pressure Absorption desorption apparatus and its application method "（CN104062204A）Thermostatic oil bath mode of heating of the silicone oil for medium is used, Experimental situation is severe, complicated, cannot equally carry out the adsorption and desorption experiment under low temperature.And above device the degree of automation Relatively low, the pressure limit that can be born is small, and air-tightness deficiency, the laboratory sample amount that can be carried out at the same time is few, and conventional efficient is low.
The content of the invention
The present invention is in order to solve shortcoming of the prior art, there is provided a kind of test operation is easy, test accuracy is high, Test data is accurate, being capable of automatic data collection and the high high/low temperature High Pressure Absorption test device for desorption of test efficiency.
In order to solve the above technical problems, the present invention adopts the following technical scheme that：High/low temperature High Pressure Absorption test device for desorption, Including inflation system, degassing system, adsorption system, desorption system, temperature control system and data collecting system；
Inflation system includes methane inflation unit and helium inflation unit, methane inflation unit include high pressure methane gas cylinder, Methane air accumulator and the first five-way valve, are connected between high pressure methane gas cylinder and methane air accumulator by high-voltage tube, high pressure methane gas It is sequentially connected in series on high-voltage tube between bottle and methane air accumulator along methane gas circulating direction equipped with first gas pressure reducing valve and height Calm the anger body booster pump, the first five-way valve includes the first valve body, the first valve body be equipped with first interface, second interface, the 3rd interface, 4th interface and the 5th interface, valve body are equipped with and corresponding five interface switches of the first to the 5th interface, methane air accumulator It is connected by high-voltage tube with the 4th interface；Helium inflation unit includes high pressure helium gas cylinder and second gas pressure reducing valve, high-pressure helium Bottle is connected by high-voltage tube with second interface, and second gas pressure reducing valve is arranged on the high pressure between high pressure helium gas cylinder and second interface Guan Shang；
Degassing system includes vacuum pump, vacuum tank, vacuum meter and the second five-way valve, and the second five-way valve includes the second valve Body, the second valve body are equipped with the 6th interface, the 7th interface, the 8th interface, the 9th interface and the tenth interface, and the second valve body is equipped with With corresponding five interface switches of the 6th to the tenth interface, vacuum pump is connected by high-voltage tube with vacuum tank, and vacuum meter is set On vacuum tank, vacuum tank is connected by high-voltage tube with the 3rd interface, and the first interface of the first five-way valve and the two or five leads to 8th interface of valve is connected by high-voltage tube, and the 5th interface of the first five-way valve and the 9th interface of the second five-way valve pass through high pressure Pipe connects；
Temperature control system includes high temperature unit and cryogenic unit, and high temperature unit includes high-temperature incubator and is located at high-temperature constant The first control panel on incubator, the first control panel are equipped with the first temperature controller, the first power switch, heater switch, instruction Lamp switch and the heater controlled by heater switch；Cryogenic unit includes cryostat and be located on cryostat second Control panel, the second control panel are equipped with the second temperature controller, second source switch, refrigeration and switch and by refrigeration switch control Refrigeration unit；
Adsorption system includes high temperature adsorption unit and low temperature adsorption unit, and high temperature adsorption unit includes being arranged on high temperature constant temperature First gas surge tank and some coal sample tanks in case, first gas surge tank and each coal sample tank are in parallel by connecting tube respectively It is arranged on the high-voltage tube between first interface and the 8th interface, along gas on the high-voltage tube between first interface and the 8th interface Circulating direction is sequentially connected in series to be passed equipped with the first pneumatic operated valve and first pressure sensor, first gas surge tank equipped with the first temperature Sensor and second pressure sensor, the connecting tube connected on first gas surge tank are equipped with the second pneumatic operated valve, each coal sample tank On be respectively equipped with second temperature sensor and the 3rd pressure sensor, is respectively equipped with the connecting tube connected on each coal sample tank Three pneumatic operated valves；
Low temperature adsorption unit includes second gas surge tank and some coal sample tanks being arranged in cryostat, the second gas Body surge tank and each coal sample tank are arranged in parallel on the high-voltage tube between the 5th interface and the 9th interface by connecting tube respectively, It is sequentially connected in series along gas circulating direction on high-voltage tube between 5th interface and the 9th interface and is pressed equipped with the 4th pneumatic operated valve and the 4th Force snesor, second gas surge tank are equipped with three-temperature sensor and the 5th pressure sensor, on second gas surge tank The connecting tube of connection is equipped with the 5th pneumatic operated valve, and the 4th temperature sensor and the 6th pressure sensing are respectively equipped with each coal sample tank Device, is respectively equipped with the 6th pneumatic operated valve in the connecting tube connected on each coal sample tank；
Desorption system includes gas drainage metering device, electronic balance and some desorption gas flowmeters being connected in parallel, The range of each desorption gas flowmeter is different, and each desorption gas flowmeter is connected by high-voltage tube and the 7th interface respectively Connect, the 7th pneumatic operated valve is respectively equipped with the high-voltage tube between each desorption gas flowmeter and the 7th interface；
Gas drainage metering device includes tank, drainpipe and collecting container, tank upper end by high-voltage tube with 6th interface connects, and the high-voltage tube between tank and the 6th interface is equipped with the 8th pneumatic operated valve, drainpipe one end and water storage Container bottom connects, and the drainpipe other end at the top of collecting container with connecting, and collecting container is placed on electronic balance, the tenth interface On be connected with evacuated tube, evacuated tube is equipped with the 9th pneumatic operated valve；
Data collecting system includes computer and control unit, and control unit includes the 3rd control panel, the 3rd chain of command Plate is equipped with pressure logging, temperature polling instrument, flow meter display, the cryostat for controlling second source to switch and opens Close, the high-temperature incubator switch for controlling the first power switch, and for control pressure logging and temperature polling instrument 3rd power switch, computer control connection first gas pressure reducing valve, second gas pressure reducing valve, the first five-way valve, the two or five lead to Valve and the first to the 9th pneumatic operated valve.
The coal sample tank is five in high temperature adsorption unit, 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 sample tank, the coal sample tank is five in low temperature adsorption unit, is respectively the 6th coal sample tank, the Seven coal sample tanks, the 8th coal sample tank, the 9th coal sample tank and the tenth coal sample tank.
The desorption gas flow is calculated as three in desorption system, is respectively the first desorption gas flowmeter, the second desorption Gas flowmeter and the 3rd desorption gas flowmeter, the range of the first desorption gas flowmeter is 0-2000ml/min, and second solves The range of air-breathing flowmeter body is 0-500ml/min, and the range of the 3rd desorption gas flowmeter is 0-100ml/min；The stream Gauge display be three, respectively with the first desorption gas flowmeter, the second desorption gas flowmeter, the 3rd desorption gas stream The corresponding first desorption gas flowmeter of gauge, the second desorption gas flowmeter, the 3rd desorption gas flowmeter.
The present invention also aims to provide a kind of test method of high/low temperature High Pressure Absorption test device for desorption, difference mould Intend the adsorption-desorption experiment under hot conditions and cryogenic conditions different pressures, and realize test data accurate automatic collection in real time, To study coal body gas adsorption adsorption law, there is provided relatively reliable data basis, efficient extraction and utilization to gas have Important realistic meaning.
For achieving the above object, the test method of high/low temperature High Pressure Absorption test device for desorption of the invention is wrapped successively Include following steps：
（1）Block fresh coal sample is drilled through on down-hole mining working face, sent after tightly encapsulating to ground experiment room, Fresh coal sample is crushed, is sieved into different granularities, the coal sample for choosing corresponding granularity respectively carries out the survey of real density and apparent density It is fixed；
（2）Checkout facility device ensures that experimental rig connection is reliable, opens second gas pressure reducing valve, first interface, 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 gas Dynamic valve, first gas surge tank, second gas surge tank and the first to the tenth coal sample tank are filled with by helium, checkout facility device Air-tightness ensures that experimental rig air-tightness is good, is then shut off all gas pressure reducing valve, pneumatic operated valve and interface；First is opened to connect Mouth, the 3rd interface 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 gas Dynamic valve and the 6th pneumatic operated valve, start vacuum pump and are de-gassed processing to high temperature adsorption unit and low temperature adsorption unit, until vacuum Count pressure and show that below 20Pa three more than hour, is then shut off vacuum pump and all gas pressure reducing valve, pneumatic operated valve and interface, will Electronic balance is placed at evacuated tube, and collecting container is placed on electronic balance and injects water, the port of export of evacuated tube is stretched Enter to below the collecting container water surface, record the registration g of electronic balance1, the 8th interface and the tenth interface are opened, opens the 9th gas Dynamic valve, the water in collecting container flow into and fill the high-voltage tube between the first pneumatic operated valve and the 8th interface, record electronic balance Registration g2, g1With g2Difference corresponding to water volume be the high-voltage tube between the first pneumatic operated valve and the 8th interface body Product, opens the 3rd pneumatic operated valve on the second pneumatic operated valve and the first to the 5th coal sample tank, is treated after opening corresponding pneumatic operated valve every time successively After the registration of electronic balance is stablized, record the registration of electronic balance at this time and close the pneumatic operated valve, measure the matter for flowing into water respectively Amount, draws the volume of first gas surge tank and the first to the 5th coal sample tank, closes total interface and pneumatic operated valve, then opens the Nine interfaces and the tenth interface, open the 9th pneumatic operated valve, and the water in collecting container flows into and fills the 4th pneumatic operated valve and the 9th interface Between high-voltage tube, record the registration of electronic balance, calculate the body of the high-voltage tube between the 4th pneumatic operated valve and the 9th interface Product, then opens the 6th pneumatic operated valve on the 5th pneumatic operated valve and the 6th to the tenth coal sample tank, opens corresponding pneumatic operated valve every time successively Afterwards after the registration of electronic balance is stablized, record the registration of electronic balance at this time and close the pneumatic operated valve, measure inflow water respectively Quality, draw the volume of second gas surge tank and the 6th to the tenth coal sample tank；
（3）Coal sample is loaded in the first to the tenth coal sample tank, controls heater to set high temperature constant temperature by the first temperature controller Test temperature in case, controls refrigeration unit to set the test temperature in cryostat, high temperature constant temperature by the second temperature controller Case temperature setting scope is 20 DEG C to 80 DEG C, and cryostat temperature setting scope is -100 DEG C to 20 DEG C, and it is logical to open the one or five First interface, the 3rd interface and the 5th interface on valve, open the first to the 6th pneumatic operated valve, close remaining interface and pneumatic operated valve, Start vacuum pump and processing is de-gassed to high temperature adsorption unit and low temperature adsorption unit, until vacuum gauge pressure shows below 20Pa And it is more than hour to be kept for three, vacuum pump and all pneumatic operated valves and interface are then shut off, first interface and second interface is opened, beats The first pneumatic operated valve is driven, opens high pressure helium gas cylinder, high-pressure helium enters high temperature adsorption list after second gas pressure reducing valve reduced pressure treatment In the high-voltage tube of member, after first pressure sensor registration stabilization, the first pneumatic operated valve is closed, opens the first to the 5th coal sample successively The 3rd pneumatic operated valve on tank, treats the 3rd pressure sensor reading and first on corresponding coal sample tank every time after the 3rd pneumatic operated valve of opening When the registration of pressure sensor is consistent, the 3rd pneumatic operated valve closed on the coal sample tank simultaneously records the 3rd pressure on the coal sample tank The registration of sensor, and the first pneumatic operated valve is again turned on, high pressure helium gas cylinder is opened, high-pressure helium subtracts through second gas pressure reducing valve Enter after pressure processing in the high-voltage tube of high temperature adsorption unit, after first pressure sensor registration stabilization, close the first pneumatic operated valve, So as to draw the free space volumes of the first to the 5th coal sample tank；First interface is closed, opens the 5th interface, it is pneumatic to open the 4th Valve, opens high pressure helium gas cylinder, and high-pressure helium enters the high-voltage tube of low temperature adsorption unit after second gas pressure reducing valve reduced pressure treatment It is interior, after the 4th pressure sensor reading stabilization, the 4th pneumatic operated valve is closed, opens the 6th on the 6th to the tenth coal sample tank successively Pneumatic operated valve, treats the 6th pressure sensor reading and the 4th pressure sensor on corresponding coal sample tank every time after the 6th pneumatic operated valve of opening Registration it is consistent when, the 6th pneumatic operated valve closed on the coal sample tank simultaneously records showing for the 6th pressure sensor on the coal sample tank Number, and the 4th pneumatic operated valve is again turned on, high pressure helium gas cylinder is opened, high-pressure helium is laggard through second gas pressure reducing valve reduced pressure treatment Enter in the high-voltage tube of low temperature adsorption unit, after the 4th pressure sensor reading stabilization, close the 4th pneumatic operated valve, so as to draw the The free space volumes of six to the tenth coal sample tanks, close all pneumatic operated valves and interface；
（4）First interface, the 3rd interface and the 5th interface are opened, opens the first pneumatic operated valve, the 3rd pneumatic operated valve, the 4th pneumatic Valve and the 6th pneumatic operated valve, start vacuum pump and are de-gassed processing to high temperature adsorption unit and low temperature adsorption unit, until vacuum meter Pressure shows below 20Pa and it is more than hour to be kept for three, is then shut off vacuum pump and all pneumatic operated valves and interface, opens high pressure Methane gas cylinder, high pressure methane gas after first gas pressure reducing valve reduced pressure treatment again through gases at high pressure booster pump be pressurized to experiment before by The predetermined adsorption pressure force value that testing crew determines is stored in methane air accumulator, opens first interface and the 4th interface, opens the One pneumatic operated valve and the second pneumatic operated valve, first gas surge tank and its height of connection are filled with by the methane gas of predetermined adsorption pressure force value In pressure pipe, after the registration of first pressure sensor and second pressure sensor stabilization, the first pneumatic operated valve and second pneumatic is closed Valve, then records the registration of first pressure sensor at this time, opens the 3rd pneumatic operated valve on the first to the 5th coal sample tank successively, The 3rd pressure sensor reading and first pressure sensor on corresponding coal sample tank are treated after one the 3rd pneumatic operated valve of opening every time After registration is stablized relatively, the 3rd pneumatic operated valve on the coal sample tank is closed, and record the 3rd pressure sensing on the coal sample tank at this time The registration of device simultaneously closes the 3rd pneumatic operated valve, is kept for seven hours, coal sample is fully adsorbed and reach balance, records the coal sample at this time The registration of the 3rd pressure sensor on tank, and the second pneumatic operated valve is opened, treat first pressure sensor and second pressure sensing After the registration of device is stablized, the second pneumatic operated valve is closed, so as to calculate the methane gas being filled with the first to the 5th coal sample tank respectively Methane gas volume under volume and free state, finally obtains adsorbed methane gas volume in the first to the 5th coal sample tank；Close First interface is closed, opens the 5th interface, the 4th pneumatic operated valve and the 5th pneumatic operated valve are opened, by the methane gas of predetermined adsorption pressure force value It is filled with second gas surge tank and its high-voltage tube of connection, treats that the registration of the 4th pressure sensor and the 5th pressure sensor is steady After fixed, the 4th pneumatic operated valve and the 5th pneumatic operated valve are closed, then records the registration of the 4th pressure sensor at this time, opens the successively The 6th pneumatic operated valve on six to the tenth coal sample tanks, treats the 6th pressure on corresponding coal sample tank every time after one the 6th pneumatic operated valve of opening Sensor registration it is opposite with the registration of the 4th pressure sensor stablize after, close the 6th pneumatic operated valve on the coal sample tank, and record The registration of the 6th pressure sensor on the coal sample tank and the 6th pneumatic operated valve is closed at this time, kept for seven hours, fill coal sample Divide absorption to reach balance, record the registration of the 6th pressure sensor on the coal sample tank at this time, and open the 5th pneumatic operated valve, treat After the registration of 4th pressure sensor and the 6th pressure sensor is stablized, the 5th pneumatic operated valve is closed, is filled with so as to calculate respectively The methane gas volume under methane gas volume and free state in 6th to the tenth coal sample tank, finally obtains the 6th to the tenth Adsorbed methane gas volume in coal sample tank, closes all pneumatic operated valves and interface；
（5）Step（3）And step（4）For adsorbed methane gas volume measuring method, adsorbed methane is measured using this method Before gas volume, by testing crew determine in this method high temperature absorbing unit and low temperature adsorption unit first gas surge tank and N number of predetermined adsorption pressure force value of second gas surge tank, N are the positive integer less than 10, are measured using adsorbed methane gas volume Method carries out n times step（3）And step（4）, under the conditions of minimum predetermined adsorption pressure force value, using the adsorbed methane gas Volume measuring method is operated, and is obtained the methane gas volume adsorbed in the first to the tenth coal sample tank, is then passed through high pressure gas The pressure value of first gas surge tank and second gas surge tank is increased to next predetermined adsorption pressure force value by body booster pump；Under Restored under conditions of one predetermined adsorption pressure force value and carry out step（3）And step（4）, until n times step（3）And step（4）Behaviour After the completion of work, the methane gas volume adsorbed in the first to the tenth coal sample tank under N number of predetermined adsorption pressure force value is obtained；
（6）First interface, the 3rd interface and the 5th interface are opened, opens the first pneumatic operated valve, the 3rd pneumatic operated valve, the 4th pneumatic Valve and the 6th pneumatic operated valve, start vacuum pump and are de-gassed processing to high temperature adsorption unit and low temperature adsorption unit, until vacuum meter Pressure shows below 20Pa and it is more than hour to be kept for three, is then shut off vacuum pump and all pneumatic operated valves and interface, opens high pressure Methane gas cylinder, high pressure methane gas after first gas pressure reducing valve reduced pressure treatment again through gases at high pressure booster pump be pressurized to experiment before by The predetermined desorption pressure value that testing crew determines is stored in methane air accumulator, opens first interface and the 4th interface, opens the One pneumatic operated valve and the second pneumatic operated valve, first gas surge tank and its height of connection are filled with by the methane gas of predetermined desorption pressure value In pressure pipe, after the registration of first pressure sensor and second pressure sensor stabilization, the first pneumatic operated valve and second pneumatic is closed Valve, then records the registration of first pressure sensor at this time, opens the 3rd pneumatic operated valve on the first to the 5th coal sample tank successively, The 3rd pressure sensor reading and first pressure sensor on corresponding coal sample tank are treated after one the 3rd pneumatic operated valve of opening every time After registration is stablized relatively, the 3rd pneumatic operated valve on the coal sample tank is closed, and record the 3rd pressure sensing on the coal sample tank at this time The registration of device simultaneously closes the 3rd pneumatic operated valve, is kept for seven hours, coal sample is fully adsorbed and reach balance, records the coal sample at this time The registration of the 3rd pressure sensor on tank, and the second pneumatic operated valve is opened, treat first pressure sensor and second pressure sensing After the registration of device is stablized, the second pneumatic operated valve is closed, so as to calculate the methane gas being filled with the first to the 5th coal sample tank respectively Methane gas volume under volume and free state, finally obtains adsorbed methane gas volume in the first to the 5th coal sample tank；Close First interface is closed, opens the 5th interface, the 4th pneumatic operated valve and the 5th pneumatic operated valve are opened, by the methane gas of predetermined desorption pressure value It is filled with second gas surge tank and its high-voltage tube of connection, treats that the registration of the 4th pressure sensor and the 5th pressure sensor is steady After fixed, the 4th pneumatic operated valve and the 5th pneumatic operated valve are closed, then records the registration of the 4th pressure sensor at this time, opens the successively The 6th pneumatic operated valve on six to the tenth coal sample tanks, treats the 6th pressure on corresponding coal sample tank every time after one the 6th pneumatic operated valve of opening Sensor registration it is opposite with the registration of the 4th pressure sensor stablize after, close the 6th pneumatic operated valve on the coal sample tank, and record The registration of the 6th pressure sensor on the coal sample tank and the 6th pneumatic operated valve is closed at this time, kept for seven hours, fill coal sample Divide absorption to reach balance, record the registration of the 6th pressure sensor on the coal sample tank at this time, and open the 5th pneumatic operated valve, treat After the registration of 4th pressure sensor and the 6th pressure sensor is stablized, the 5th pneumatic operated valve is closed, is filled with so as to calculate respectively The methane gas volume under methane gas volume and free state in 6th to the tenth coal sample tank, finally obtains the 6th to the tenth Adsorbed methane gas volume in coal sample tank, closes all pneumatic operated valves and interface, after coal sample reaches adsorption equilibrium, opens the 6th and connects Mouth, the 7th interface, the 8th interface, the tenth interface and the 9th pneumatic operated valve, open the 3rd gas on the first to the 5th coal sample tank successively Dynamic valve, respectively empties the methane gas under free state in the first to the 5th coal sample tank, opens the 3rd gas every time After dynamic valve when the 3rd pressure sensor reading on corresponding coal sample tank is zero, the 9th pneumatic operated valve is closed, it is automatic using computer Control the first desorption gas flowmeter, the second desorption gas flowmeter, the 7th pneumatic operated valve on the 3rd desorption gas flowmeter with And the 8th pneumatic operated valve, the first desorption gas flowmeter is chosen first, when methane gas flow is more than 450ml/min, computer The 7th pneumatic operated valve on the first desorption gas flowmeter is opened in control, must be desorbed by the first desorption gas flow measurement Methane gas volume, when methane gas flow is between 80ml/min-450ml/min, computer is by the second desorption gas stream The 7th pneumatic operated valve on gauge is opened, and the methane gas volume that must be desorbed by the second desorption gas flow measurement, works as methane When gas flow is between 20ml/min-80ml/min, computer makes the 7th pneumatic operated valve on the 3rd desorption gas flowmeter Open, the methane gas volume that must be desorbed by the 3rd desorption gas flow measurement, when methane gas flow is less than 20ml/min, Computer opens the 8th pneumatic operated valve, and the methane gas volume desorbed is measured by gas drainage metering device, so as to measure The methane gas volume desorbed in one to the 5th coal sample tank；It is then shut off the 8th interface, opens the 9th interface and the 9th pneumatic Valve, opens the 6th pneumatic operated valve on the 6th to the tenth coal sample tank, respectively under free state in the 6th to the tenth coal sample tank successively Methane gas emptied, treat the 6th pressure sensor reading on corresponding coal sample tank after opening the 6th pneumatic operated valve every time When being zero, the 9th pneumatic operated valve is closed, using the first desorption gas of computer controlled automatic flowmeter, the second desorption gas flow Meter, the 7th pneumatic operated valve and the 8th pneumatic operated valve on the 3rd desorption gas flowmeter, pass through the first desorption gas flowmeter, second Desorption gas flowmeter, the gentle drainage metering device of the 3rd desorption gas flowmeter, measure and are desorbed in the 6th to the tenth coal sample tank The methane gas volume gone out, whole desorption process Computer gathers instantaneous delivery and integrated flux in real time, and generates datagram Table and curve；
（7）Step（6）For desorption of methane gas volume measuring method, desorption of methane gas volume is measured using this method Before, first gas surge tank and second gas in this method high temperature absorbing unit and low temperature adsorption unit are determined by testing crew N number of predetermined desorption pressure value of surge tank, N are the positive integer less than 10, are carried out using desorption of methane gas volume measuring method N times step（6）, under the conditions of minimum predetermined desorption pressure value, carried out using the desorption of methane gas volume measuring method Operation, obtains the methane gas volume desorbed in the first to the tenth coal sample tank, then by gases at high pressure booster pump by first The pressure value of gas buffer tank and second gas surge tank is increased to next predetermined desorption pressure value；In next predetermined desorption pressures Restored under conditions of value and carry out step（6）, until n times step（6）Operation after the completion of, obtain under N number of predetermined desorption pressure value The first to the tenth coal sample tank in the methane gas volume adsorbed.
Above-mentioned technical proposal is used, the invention has the advantages that：
1st, high/low temperature High Pressure Absorption test device for desorption of the invention includes inflation system, degassing system, adsorption system, solution Desorption system, temperature control system and data collecting system, inflation system include methane inflation unit and helium inflation unit, methane Inflation unit first passes through the decompression of first gas pressure reducing valve using high pressure methane gas cylinder, then through gases at high pressure booster pump by methane gas Pressure is adjusted to the pressure needed for experiment, and the methane gas for setting pressure value is filled into methane air accumulator, by methane Air accumulator provides the methane gas of scheduled pressure value into adsorption system, and helium inflation unit is using high pressure helium gas cylinder through the second gas It is passed through after body pressure reducing valve reduced pressure treatment in adsorption system, for demarcating the free space volumes of each coal sample tank；Degassing system is adopted Processing is de-gassed to adsorption system with vacuum pump, it is ensured that only have methane gas to participate in experiment during experiment, so as to arrange Except interference of other gases to result of the test；Temperature control system utilizes the high temperature adsorption list in high temperature unit combination adsorption system Methane adsorption desorption experiment under member simulation hot environment, and utilize the low temperature adsorption unit in cryogenic unit combination adsorption system Simulate the methane adsorption desorption experiment under low temperature environment；
2nd, desorption system of the invention uses the desorption gas flowmeter and gas drainage metering device of three different ranges, Measured using the first desorption gas flowmeter at desorption experiment initial stage, with the flow-reduction of desorption gas, used successively Second desorption gas flowmeter, the 3rd desorption gas flowmeter and gas drainage metering device are measured, in whole desorption examination During testing, switched by computer according to the size automatic control interface of desorption gas flow, and real-time automatic collecting number According to, test accuracy is effectively improved, and operation difficulty is reduced, test operation is easy, effectively improves test efficiency；
3rd, high/low temperature High Pressure Absorption test device for desorption of the invention can provide -100 DEG C of low temperature ring using cryogenic unit Border, experimental condition is provided for the adsorption-desorption characteristics of research methane at low ambient temperatures and the supercritical adsorption of simulation methane；
4th, the test method of high/low temperature High Pressure Absorption test device for desorption of the invention, the data acquisition during experiment There is computer control with Interface Controller, instrument workflow is shown on interface, after operating personnel set parameter, computer Can be with all pressure of automatic collection, temperature, flow, and initial data report, analytical table and curve map are generated through processing, effectively The test error that artificial reading and manual record are brought is avoided, the accuracy and test efficiency of experiment is improved, reduces examination Test the operation difficulty of personnel；
5th, the test method of high/low temperature High Pressure Absorption test device for desorption of the invention, can be carried out at the same time five groups of coal samples not The measure of methane gas adsorbance and methane desorbing gas amount under the conditions of under synthermal, different pressures, effectively increases experiment Efficiency, and the methane adsorption desorption experiment under hot conditions and cryogenic conditions different pressures is simulated respectively, to study coal body watt Coal gas adsorption-desorption characteristics provide relatively reliable data basis under this adsorption-desorption rule especially low temperature environment, right The efficient extraction and utilization of gas have important practical significance.
Brief description of the drawings
Fig. 1 is the structure diagram of the present invention.
Embodiment
As shown in Figure 1, the high/low temperature High Pressure Absorption test device for desorption of the present invention, including inflation system, degassing system, suction Attached system, desorption system, temperature control system and data collecting system.
Inflation system includes methane inflation unit and helium inflation unit, methane inflation unit include high pressure methane gas cylinder 1, 2 and first five-way valve of methane air accumulator, is connected, high pressure first between high pressure methane gas cylinder 1 and methane air accumulator 2 by high-voltage tube 3 It is sequentially connected in series along methane gas circulating direction on high-voltage tube 3 between alkane gas cylinder 1 and methane air accumulator 2 and is depressurized equipped with first gas Valve 4 and gases at high pressure booster pump 5, the first five-way valve include the first valve body 6, and the first valve body 6 connects equipped with first interface 7, second Mouthful the 8, the 3rd interface 9, the 4th interface 10 and the 5th interface 11, the first valve body 6 be equipped with the first to the 5th interface 7,8,9,10, 11 corresponding five interface switches（Five-way valve is existing conventional components, its concrete structure is no longer described in detail）, methane air accumulator 2 is logical High-voltage tube 3 is crossed to be connected with the 4th interface 10；Helium inflation unit includes high pressure helium gas cylinder 12 and second gas pressure reducing valve 13, high pressure Helium tank 12 is connected by high-voltage tube 3 with second interface 8, and second gas pressure reducing valve 13 is arranged on high pressure helium gas cylinder 12 and is connect with second On high-voltage tube 3 between mouth 8.
Degassing system includes vacuum pump 14, vacuum tank 15,16 and second five-way valve of vacuum meter, and the second five-way valve includes the Two valve bodies 17, the second valve body 17 are equipped with the 6th interface 18, the 7th interface 19, the 8th interface 20, the 9th interface 21 and the tenth and connect Mouthfuls 22, the second valve body 17 be equipped with 18,19,20,21,22 corresponding five interface switches of the 6th to the tenth interface,
Vacuum pump 14 is connected by high-voltage tube 3 with vacuum tank 15, and vacuum meter 16 is located on vacuum tank 15, vacuum tank 15 are connected by high-voltage tube 3 with the 3rd interface 9, and the 8th interface 20 of 7 and second five-way valve of first interface of the first five-way valve is logical Cross high-voltage tube 3 to connect, the 5th interface 11 of the first five-way valve is connected with the 9th interface 21 of the second five-way valve by high-voltage tube 3.
Temperature control system includes high temperature unit and cryogenic unit, and high temperature unit includes high-temperature incubator 23 and is located at high temperature The first control panel 24 on insulating box 23, the first control panel 24 are equipped with the first temperature controller 25, the first power switch 26, add Thermal switch 27, indicator light switch 28 and the heater controlled by heater switch 27；Cryogenic unit includes cryostat 29 and sets The second control panel 30 on cryostat 29, the second control panel 30 is equipped with the second temperature controller 31, second source is opened Close 32, refrigeration switch 33 and the refrigeration unit by 33 control of refrigeration switch；Each several part is existing in high temperature unit and cryogenic unit There are routine techniques, not shown heater and refrigeration unit.The temperature setting scope of high-temperature incubator 23 is 20 DEG C to 80 DEG C, high temperature 23 frontal design of insulating box has the rotating single open-door with observation window, and ray lamp, box outer surface plastic-spraying, interior table are housed in operating room Face uses stainless steel material, and endless form circulates for hot air convection, and adjusts temperature using the first temperature controller 25, is provided for experiment Required isoperibol；Cryostat 29 is using three-level automatic cascaded circulation refrigeration unit refrigeration, it is possible to provide -100 DEG C to 20 DEG C experimental enviroment, box outer surface plastic-spraying, inner surface uses stainless steel material, and interior four wall is equipped with refrigerating evaporator, internal step Terraced stent is used to place cryogenic absorption room, ensures that ultra low temperature state temperature is kept constant using horizontal type structure.
Adsorption system includes high temperature adsorption unit and low temperature adsorption unit, and high temperature adsorption unit includes being arranged on high temperature constant temperature First gas surge tank 34 and some coal sample tanks in case 23, first gas surge tank 34 and each coal sample tank pass through connection respectively Pipe 83 is arranged in parallel on the high-voltage tube 3 between 7 and the 8th interface 20 of first interface, between 7 and the 8th interface 20 of first interface High-voltage tube 3 on be sequentially connected in series along gas circulating direction equipped with the first pneumatic operated valve 35 and first pressure sensor 36, first gas Surge tank 34 is equipped with the first temperature sensor 37 and second pressure sensor 38, the connection connected on first gas surge tank 34 Pipe 83 is equipped with the second pneumatic operated valve 39, and 40 and the 3rd pressure sensor of second temperature sensor is respectively equipped with each coal sample tank 41, the 3rd pneumatic operated valve 42 is respectively equipped with the connecting tube 83 connected on each coal sample tank.
Low temperature adsorption unit includes second gas surge tank 43 and some coal sample tanks being arranged in cryostat 29, the Two gas buffer tanks 43 and each coal sample tank respectively by connecting tube 83 be arranged in parallel the 5th interface 11 and the 9th interface 21 it Between high-voltage tube 3 on, be sequentially connected in series and be equipped with along gas circulating direction on the high-voltage tube 3 between the 5th interface 11 and the 9th interface 21 4th pneumatic operated valve 44 and the 4th pressure sensor 45, second gas surge tank 43 are pressed equipped with three-temperature sensor 46 and the 5th Force snesor 47, the connecting tube 83 connected on second gas surge tank 43 are equipped with the 5th pneumatic operated valve 48, on each coal sample tank point Not She You the 4th temperature sensor 49 and the 6th pressure sensor 50, be respectively equipped with the connecting tube 83 connected on each coal sample tank 6th pneumatic operated valve 51.
Desorption system includes gas drainage metering device, electronic balance 52 and some desorption gas flows being connected in parallel Meter, the range of each desorption gas flowmeter is different, and each desorption gas flowmeter passes through 3 and the 7th interface of high-voltage tube respectively 19 connect, and the 7th pneumatic operated valve 53 is respectively equipped with the high-voltage tube 3 between each desorption gas flowmeter and the 7th interface 19.
Gas drainage metering device includes tank 54, drainpipe 55 and collecting container 56, and 54 upper end of tank passes through High-voltage tube 3 is connected with the 6th interface 18, and the high-voltage tube 3 between 54 and the 6th interface 18 of tank is equipped with the 8th pneumatic operated valve 57,55 one end of drainpipe is connected with 54 bottom of tank, and 55 other end of drainpipe is connected with the top of collecting container 56, collects the water capacity Device 56 is placed on electronic balance 52, and evacuated tube 58 is connected with the tenth interface 22, and evacuated tube 58 is equipped with the 9th pneumatic operated valve 59.
Data collecting system includes computer 60 and control unit, and control unit includes the 3rd control panel 61, the 3rd control Panel 61 processed be equipped with pressure logging 62, temperature polling instrument 63, flow meter display, for controlling second source switch 32 Cryostat switch 64, the high-temperature incubator switch 65 for controlling the first power switch 26, and patrolled for control pressure The 3rd power switch 66 of instrument 62 and temperature polling instrument 63 is examined, computer control connection first gas pressure reducing valve 4, second gas subtract Pressure 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.Calculate Machine 60 is programmed using DelPhi, has gas parameter conversion, data analysis function, and instrument workflow is shown on interface, can After realizing that human-computer dialogue, operating personnel set parameter, computer can with all pressure of automatic collection, temperature, flow, and through place Reason generation initial data report, analytical statement and curve map.
The methane gas being filled with high pressure methane gas cylinder 1 is commercially available methane Standard Gases, and volume is 40L/ bottles, purity >= 99.99%, the helium being filled with high pressure helium gas cylinder 12 is commercial standard helium, and pressure 15MPa, volume is 40L/ bottles, high-voltage tube 3 pressure voltage is in more than 50MPa.
The coal sample tank is five in high temperature adsorption unit, is respectively the first coal sample tank 67, the second coal sample tank 68, the 3rd coal Sample tank 69, the 4th coal sample tank 70 and the 5th coal sample tank 71, the coal sample tank is five in low temperature adsorption unit, is respectively the 6th coal Sample 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.
The desorption gas flow is calculated as three in desorption system, is respectively the first desorption gas flowmeter 77, second solution 78 and the 3rd desorption gas flowmeter 79 of air-breathing flowmeter body, the range of the first desorption gas flowmeter 77 is 0-2000ml/ Min, the range of the second desorption gas flowmeter 78 is 0-500ml/min, and the range of the 3rd desorption gas flowmeter 79 is 0- 100ml/min；The flow meter display be three, respectively with the first desorption gas flowmeter 77, the second desorption gas stream Gauge 78,79 corresponding first flowmeter display 80 of the 3rd desorption gas flowmeter, second flowmeter display the 81, the 3rd Flow meter display 82.
Wherein, vacuum 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 stripping gas flowmeter body etc. are This area existing conventional techniques, its concrete structure are no longer described in detail.
The test method of high/low temperature High Pressure Absorption test device for desorption comprises the following steps successively：
（1）Block fresh coal sample is drilled through on down-hole mining working face, send after tightly encapsulating to ground experiment room, will Fresh coal sample crushes, is sieved into different granularities, and the coal sample for choosing corresponding granularity respectively carries out Industrial Analysis, real density and regarding close The measure of the parameters such as degree；
（2）Checkout facility device ensures that experimental rig connection is reliable, opens second gas pressure reducing valve 13, first interface 7, the Two interfaces 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 gas 48 and the 6th pneumatic operated valve 51 of dynamic valve, first gas surge tank 34, second gas surge tank 43 and first to the tenth are filled with by helium Coal sample tank 67,68,69,70,71,72,73,74,75,76, the air-tightness of checkout facility device ensure that experimental rig air-tightness is good It is good, it is then shut off all gas pressure reducing valve, pneumatic operated valve and interface；First interface 7, the 3rd interface 9 and the 5th interface 11 are opened, is beaten It is pneumatic to drive 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 valve 48 and the 6th Valve 51, starts vacuum pump 14 and is de-gassed processing to high temperature adsorption unit and low temperature adsorption unit, until 16 pressure of vacuum meter is shown Show that below 20Pa three more than hour, is then shut off vacuum pump 14 and all gas pressure reducing valve, pneumatic operated valve and interface, by electronics day Flat 52 are placed at evacuated tube 58, and collecting container 56 is placed on electronic balance 52 and injects water, by the outlet of evacuated tube 58 End is extend into below 56 water surface of collecting container, records the registration g of electronic balance 521, open the 8th interface 20 and the tenth interface 22, the 9th pneumatic operated valve 59 is opened, the water in collecting container 56 is flowed into and filled between the first pneumatic operated valve 35 and the 8th interface 20 High-voltage tube 3, records the registration g of electronic balance 522, g1With g2Difference corresponding to the volume of water be the first pneumatic operated valve 35 The volume of high-voltage tube 3 between the 8th interface 20, open successively the second pneumatic operated valve 39 and the first to the 5th coal sample tank 67,68, 69th, the 3rd pneumatic operated valve 42 on 70,71, opens after corresponding pneumatic operated valve after the registration of electronic balance 52 is stablized, records this every time When electronic balance 52 registration and close the pneumatic operated valve, measure respectively flow into water quality, draw 34 He of first gas surge tank The volume of first to the 5th coal sample tank 67,68,69,70,71, closes total interface and pneumatic operated valve, then opens the 9th interface 21 With the tenth interface 22, the 9th pneumatic operated valve 59 is opened, the water in collecting container 56 flows into and fills the 4th pneumatic operated valve 44 to be connect with the 9th High-voltage tube 3 between mouth 21, records the registration of electronic balance 52, calculates between the 4th pneumatic operated valve 44 and the 9th interface 21 The volume of high-voltage tube 3, then opens the on the 5th pneumatic operated valve 48 and the 6th to the tenth coal sample tank 72,73,74,75,76 successively Six pneumatic operated valves 51, open after corresponding pneumatic operated valve after the registration of electronic balance 52 is stablized every time, record electronic balance 52 at this time Registration simultaneously closes the pneumatic operated valve, measures the quality for flowing into water respectively, draws 43 and the 6th to the tenth coal sample of second gas surge tank The volume of tank 72,73,74,75,76；
（3）Filling coal sample, passes through first in the first to the tenth coal sample tank 67,68,69,70,71,72,73,74,75,76 Temperature controller 25 controls the test temperature in heater setting high-temperature incubator 23, controls refrigeration unit to set by the second temperature controller 31 Determine the test temperature in cryostat 29,23 temperature setting scope of high-temperature incubator is 20 DEG C to 80 DEG C, cryostat 29 Temperature setting scope 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 Pneumatic operated valve 35,39,42,44,48,51, closes remaining interface and pneumatic operated valve, starts vacuum pump 14 to high temperature adsorption unit and low temperature Absorbing unit is de-gassed processing, and until 16 pressure of vacuum meter display below 20Pa and it is more than hour to be kept for three, is then shut off Vacuum pump 14 and all pneumatic operated valves and interface, open first interface 7 and second interface 8, open the first pneumatic operated valve 35, open high pressure Helium tank 12, high-pressure helium, into the high-voltage tube 3 of high temperature adsorption unit, treat the after 13 reduced pressure treatment of second gas pressure reducing valve After one pressure sensor, 36 registration is stablized, close the first pneumatic operated valve 35, open successively the first to the 5th coal sample tank 67,68,69, 70th, the 3rd pneumatic operated valve 42 on 71, opens the 3rd pressure sensor 41 treated after the 3rd pneumatic operated valve 42 on corresponding coal sample tank every time When registration is consistent with the registration of first pressure sensor 36, the 3rd pneumatic operated valve 42 closed on the coal sample tank simultaneously records the coal sample The registration of the 3rd pressure sensor 41 on tank, and the first pneumatic operated valve 35 is again turned on, open high pressure helium gas cylinder 12, high pressure helium Gas enters in the high-voltage tube 3 of high temperature adsorption unit after 13 reduced pressure treatment of second gas pressure reducing valve, treats first pressure sensor 36 After registration is stablized, the first pneumatic operated valve 35 is closed, so as to draw the free space of the first to the 5th coal sample tank 67,68,69,70,71 Volume；First interface 7 is closed, opens the 5th interface 11, opens the 4th pneumatic operated valve 44, opens high pressure helium gas cylinder 12, high-pressure helium Enter after 13 reduced pressure treatment of second gas pressure reducing valve in the high-voltage tube 3 of low temperature adsorption unit, treat that the 4th pressure sensor 45 shows After number is stablized, the 4th pneumatic operated valve 44 is closed, the 6th on the 6th to the tenth coal sample tank 72,73,74,75,76 of opening is pneumatic successively Valve 51, treats 50 registration of the 6th pressure sensor and the 4th pressure sensing on corresponding coal sample tank every time after the 6th pneumatic operated valve 51 of opening When the registration of device 45 is consistent, the 6th pneumatic operated valve 51 closed on the coal sample tank simultaneously records the 6th pressure sensing on the coal sample tank The registration of device 50, and the 4th pneumatic operated valve 44 is again turned on, high pressure helium gas cylinder 12 is opened, high-pressure helium is through second gas pressure reducing valve Enter after 13 reduced pressure treatments in the high-voltage tube 3 of low temperature adsorption unit, after 45 registration of the 4th pressure sensor stabilization, close the 4th Pneumatic operated valve 44, so as to draw the free space volumes of the 6th to the tenth coal sample tank 72,73,74,75,76, closes 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, 4th pneumatic operated valve 44 and the 6th pneumatic operated valve 51, start vacuum pump 14 and are de-gassed place to high temperature adsorption unit and low temperature adsorption unit Reason, until 16 pressure of vacuum meter shows below 20Pa and is kept for three more than hour, is then shut off vacuum pump 14 and all pneumatic Valve and interface, open high pressure methane gas cylinder 1, high pressure methane gas is after 4 reduced pressure treatment of first gas pressure reducing valve again through gases at high pressure Booster pump 5 is pressurized to the predetermined adsorption pressure force value determined before experiment by testing crew and is stored in methane air accumulator 2, opens first 7 and the 4th interface 10 of interface, opens the first pneumatic operated valve 35 and the second pneumatic operated valve 39, the methane gas of predetermined adsorption pressure force value is filled Enter in first gas surge tank 34 and its high-voltage tube 3 of connection, treat first pressure sensor 36 and second pressure sensor 38 After registration is stablized, the first pneumatic operated valve 35 and the second pneumatic operated valve 39 are closed, then records showing for first pressure sensor 36 at this time Number, opens the 3rd pneumatic operated valve 42 on the first to the 5th coal sample tank 67,68,69,70,71, opens the 3rd gas every time successively Treat that 41 registration of the 3rd pressure sensor on corresponding coal sample tank is opposite with the registration of first pressure sensor 36 after dynamic valve 42 to stablize Afterwards, the 3rd pneumatic operated valve 42 on the coal sample tank is closed, and records the registration of the 3rd pressure sensor 41 on the coal sample tank at this time And the 3rd pneumatic operated valve 42 is closed, kept for seven hours, coal sample is fully adsorbed and reach balance, record is at this time on the coal sample tank The registration of 3rd pressure sensor 41, and the second pneumatic operated valve 39 is opened, treat first pressure sensor 36 and second pressure sensing After the registration of device 38 is stablized, close the second pneumatic operated valve 39, thus calculate respectively be filled with the first to the 5th coal sample tank 67,68,69, 70th, the methane gas volume under the methane gas volume and free state in 71, finally obtain the first to the 5th coal sample tank 67, 68th, adsorbed methane gas volume in 69,70,71；First interface 7 is closed, opens the 5th interface 11, opens 44 He of the 4th pneumatic operated valve 5th pneumatic operated valve 48, second gas surge tank 43 and its high-voltage tube 3 of connection are filled with by the methane gas of predetermined adsorption pressure force value It is interior, after the registration of the 4th pressure sensor 45 and the 5th pressure sensor 47 stabilization, close the 4th pneumatic operated valve 44 and the 5th gas Dynamic valve 48, then records the registration of the 4th pressure sensor 45 at this time, open successively the 6th to the tenth coal sample tank 72,73,74, 75th, the 6th pneumatic operated valve 51 on 76, opens the 6th pressure sensing treated after the 6th pneumatic operated valve 51 on corresponding coal sample tank every time 50 registration of device it is opposite with the registration of the 4th pressure sensor 45 stablize after, close the 6th pneumatic operated valve 51 on the coal sample tank, and remember Record the registration of the 6th pressure sensor 50 on the coal sample tank at this time and close the 6th pneumatic operated valve 51, kept for seven hours, made Coal sample, which is fully adsorbed, reaches balance, records the registration of the 6th pressure sensor 50 on the coal sample tank at this time, and open the 5th Pneumatic operated valve 48, after the registration of the 4th pressure sensor 45 and the 6th pressure sensor 50 stabilization, closes the 5th pneumatic operated valve 48, from And calculate respectively under the methane gas volume and free state being filled with the 6th to the tenth coal sample tank 72,73,74,75,76 Methane gas volume, finally obtains adsorbed methane gas volume in the 6th to the tenth coal sample tank 72,73,74,75,76, closes institute There are pneumatic operated valve and interface；
（5）Step（3）And step（4）For adsorbed methane gas volume measuring method, adsorbed methane is measured using this method Before gas volume, first gas surge tank 34 in this method high temperature absorbing unit and low temperature adsorption unit is determined by testing crew With N number of predetermined adsorption pressure force value of second gas surge tank 43, N is the positive integer less than 10, uses adsorbed methane gas volume Measuring method carries out n times step（3）And step（4）, under the conditions of minimum predetermined adsorption pressure force value, using the adsorbed methane Gas volume measuring method is operated, and is obtained in the first to the tenth coal sample tank 67,68,69,70,71,72,73,74,75,76 The methane gas volume of absorption, then by gases at high pressure booster pump 5 by first gas surge tank 34 and second gas surge tank 43 pressure value is increased to next predetermined adsorption pressure force value；Restored under conditions of next predetermined adsorption pressure force value and carry out step （3）And step（4）, until n times step（3）And step（4）Operation after the completion of, obtain under N number of predetermined adsorption pressure force value The methane gas volume of absorption in one to the tenth coal sample tank 67,68,69,70,71,72,73,74,75,76；
（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, 4th pneumatic operated valve 44 and the 6th pneumatic operated valve 51, start vacuum pump 14 and are de-gassed place to high temperature adsorption unit and low temperature adsorption unit Reason, until 16 pressure of vacuum meter shows below 20Pa and is kept for three more than hour, is then shut off vacuum pump 14 and all pneumatic Valve and interface, open high pressure methane gas cylinder 1, high pressure methane gas is after 4 reduced pressure treatment of first gas pressure reducing valve again through gases at high pressure Booster pump 5 is pressurized to the predetermined desorption pressure value determined before experiment by testing crew and is stored in methane air accumulator 2, opens first 7 and the 4th interface 10 of interface, opens the first pneumatic operated valve 35 and the second pneumatic operated valve 39, the methane gas of predetermined desorption pressure value is filled Enter in first gas surge tank 34 and its high-voltage tube 3 of connection, treat first pressure sensor 36 and second pressure sensor 38 After registration is stablized, the first pneumatic operated valve 35 and the second pneumatic operated valve 39 are closed, then records showing for first pressure sensor 36 at this time Number, opens the 3rd pneumatic operated valve 42 on the first to the 5th coal sample tank 67,68,69,70,71, opens the 3rd gas every time successively Treat that 41 registration of the 3rd pressure sensor on corresponding coal sample tank is opposite with the registration of first pressure sensor 36 after dynamic valve 42 to stablize Afterwards, the 3rd pneumatic operated valve 42 on the coal sample tank is closed, and records the registration of the 3rd pressure sensor 41 on the coal sample tank at this time And the 3rd pneumatic operated valve 42 is closed, kept for seven hours, coal sample is fully adsorbed and reach balance, record is at this time on the coal sample tank The registration of 3rd pressure sensor 41, and the second pneumatic operated valve 39 is opened, treat first pressure sensor 36 and second pressure sensing After the registration of device 38 is stablized, close the second pneumatic operated valve 39, thus calculate respectively be filled with the first to the 5th coal sample tank 67,68,69, 70th, the methane gas volume under the methane gas volume and free state in 71, finally obtain the first to the 5th coal sample tank 67, 68th, adsorbed methane gas volume in 69,70,71；First interface 7 is closed, opens the 5th interface 11, opens 44 He of the 4th pneumatic operated valve 5th pneumatic operated valve 48, second gas surge tank 43 and its high-voltage tube 3 of connection are filled with by the methane gas of predetermined desorption pressure value It is interior, after the registration of the 4th pressure sensor 45 and the 5th pressure sensor 47 stabilization, close the 4th pneumatic operated valve 44 and the 5th gas Dynamic valve 48, then records the registration of the 4th pressure sensor 45 at this time, open successively the 6th to the tenth coal sample tank 72,73,74, 75th, the 6th pneumatic operated valve 51 on 76, opens the 6th pressure sensing treated after the 6th pneumatic operated valve 51 on corresponding coal sample tank every time 50 registration of device it is opposite with the registration of the 4th pressure sensor 45 stablize after, close the 6th pneumatic operated valve 51 on the coal sample tank, and remember Record the registration of the 6th pressure sensor 50 on the coal sample tank at this time and close the 6th pneumatic operated valve 51, kept for seven hours, made Coal sample, which is fully adsorbed, reaches balance, records the registration of the 6th pressure sensor 50 on the coal sample tank at this time, and open the 5th Pneumatic operated valve 48, after the registration of the 4th pressure sensor 45 and the 6th pressure sensor 50 stabilization, closes the 5th pneumatic operated valve 48, from And calculate respectively under the methane gas volume and free state being filled with the 6th to the tenth coal sample tank 72,73,74,75,76 Methane gas volume, finally obtains adsorbed methane gas volume in the 6th to the tenth coal sample tank 72,73,74,75,76, closes institute After thering is pneumatic operated valve and interface, coal sample to reach adsorption equilibrium, open the 6th interface 18, the 7th interface 19, the 8th interface the 20, the tenth and connect 22 and the 9th pneumatic operated valve 59 of mouth, opens the 3rd pneumatic operated valve 42 on the first to the 5th coal sample tank 67,68,69,70,71 successively, point The other methane gas under free state in the first to the 5th coal sample tank 67,68,69,70,71 empties, and opens one every time After 3rd pneumatic operated valve 42 when 41 registration of the 3rd pressure sensor on corresponding coal sample tank is zero, the 9th pneumatic operated valve 59 is closed, is adopted The first desorption gas flowmeter 77, the second desorption gas flowmeter 78, the 3rd desorption gas flow are automatically controlled with computer 60 The 7th pneumatic operated valve 53 and the 8th pneumatic operated valve 57 on meter 79, choose the first desorption gas flowmeter 77, work as methane gas first When flow is more than 450ml/min, computer 60, which controls, opens the 7th pneumatic operated valve 53 on the first desorption gas flowmeter 77, leads to Cross the first desorption gas flowmeter 77 and measure the methane gas volume desorbed, when methane gas flow is in 80ml/min- When between 450ml/min, computer 60 opens the 7th pneumatic operated valve 53 on the second desorption gas flowmeter 78, passes through the second solution Air-breathing flowmeter body 78 measures the methane gas volume desorbed, when methane gas flow is between 20ml/min-80ml/min When, computer 60 opens the 7th pneumatic operated valve 53 on the 3rd desorption gas flowmeter 79, passes through the 3rd desorption gas flowmeter 79 measure the methane gas volume desorbed, and when methane gas flow is less than 20ml/min, computer 60 is by the 8th pneumatic operated valve 57 Open, the methane gas volume desorbed is measured by gas drainage metering device so that measure the first to the 5th coal sample tank 67, 68th, the methane gas volume desorbed in 69,70,71；The 8th interface 20 is then shut off, it is pneumatic to open the 9th interface 21 and the 9th Valve 59, opens the 6th pneumatic operated valve 51 on the 6th to the tenth coal sample tank 72,73,74,75,76, respectively to the 6th to the tenth successively Methane gas in coal sample tank 72,73,74,75,76 under free state is emptied, after opening the 6th pneumatic operated valve 51 every time When 50 registration of the 6th pressure sensor on corresponding coal sample tank is zero, the 9th pneumatic operated valve 59 is closed, it is automatic using computer 60 Control the first desorption gas flowmeter 77, the second desorption gas flowmeter 78, the 7th gas on the 3rd desorption gas flowmeter 79 53 and the 8th pneumatic operated valve 57 of dynamic valve, is desorbed by the first desorption gas flowmeter 77, the second desorption gas flowmeter the 78, the 3rd The gentle drainage metering device of gas flowmeter 79, measures the methane desorbed in the 6th to the tenth coal sample tank 72,73,74,75,76 Gas volume, whole desorption process Computer 60 gathers instantaneous delivery and integrated flux in real time, and generates data sheet and song Line；
（7）Step（6）For desorption of methane gas volume measuring method, desorption of methane gas volume is measured using this method Before, 34 and second gas of first gas surge tank in this method high temperature absorbing unit and low temperature adsorption unit is determined by testing crew N number of predetermined desorption pressure value of body surge tank 43, N are the positive integer less than 10, use desorption of methane gas volume measuring method Carry out n times step（6）, under the conditions of minimum predetermined desorption pressure value, using the desorption of methane gas volume measuring method Operated, obtain the methane gas desorbed in the first to the tenth coal sample tank 67,68,69,70,71,72,73,74,75,76 Volume, is then increased the pressure value of first gas surge tank 34 and second gas surge tank 43 by gases at high pressure booster pump 5 To next predetermined desorption pressure value；Restored under conditions of next predetermined desorption pressure value and carry out step（6）, until n times step （6）Operation after the completion of, obtain the first to the tenth coal sample tank 67 under N number of predetermined desorption pressure value, 68,69,70,71,72, 73rd, the methane gas volume of 74,75,76 interior absorption.
The present embodiment is not the limitations of work in any form such as the shape to the present invention, material, structure, every according to this hair Any simple modification, equivalent change and modification that bright technical spirit makees above example, belongs to the technology of the present invention side The protection domain of case.

Claims (3)

1. high/low temperature High Pressure Absorption test device for desorption, it is characterised in that：Including inflation system, degassing system, adsorption system, solution Desorption system, temperature control system and data collecting system；
Inflation system includes methane inflation unit and helium inflation unit, and methane inflation unit includes high pressure methane gas cylinder, methane Air accumulator and the first five-way valve, are connected between high pressure methane gas cylinder and methane air accumulator by high-voltage tube, high pressure methane gas cylinder and It is sequentially connected in series on high-voltage tube between methane air accumulator along methane gas circulating direction equipped with first gas pressure reducing valve and high pressure gas Body booster pump, the first five-way valve include the first valve body, and the first valve body is equipped with first interface, second interface, the 3rd interface, the 4th Interface and the 5th interface, valve body is equipped with to be passed through with corresponding five interface switches of the first to the 5th interface, methane air accumulator High-voltage tube is connected with the 4th interface；Helium inflation unit includes high pressure helium gas cylinder and second gas pressure reducing valve, and high pressure helium gas cylinder leads to Cross high-voltage tube to be connected with second interface, second gas pressure reducing valve is arranged on the high-voltage tube between high pressure helium gas cylinder and second interface On；
Degassing system includes vacuum pump, vacuum tank, vacuum meter and the second five-way valve, and the second five-way valve includes the second valve body, the Two valve bodies are equipped with the 6th interface, the 7th interface, the 8th interface, the 9th interface and the tenth interface, and the second valve body is equipped with and the Corresponding five interface switches of six to the tenth interfaces, vacuum pump are connected by high-voltage tube with vacuum tank, and vacuum meter is located at very On empty container, vacuum tank is connected by high-voltage tube with the 3rd interface, the first interface of the first five-way valve and the second five-way valve 8th interface is connected by high-voltage tube, and the 9th interface of the 5th interface and the second five-way valve of the first five-way valve is connected by high-voltage tube Connect；
Temperature control system includes high temperature unit and cryogenic unit, and high temperature unit includes high-temperature incubator and is located at high-temperature incubator On the first control panel, the first control panel opens equipped with the first temperature controller, the first power switch, heater switch and indicator light Close, high temperature unit further includes the heater controlled by heater switch；
Cryogenic unit includes cryostat and the second control panel being located on cryostat, and the second control panel is equipped with Second temperature controller, second source switch and refrigeration switch, cryogenic unit are further included by the refrigeration unit of refrigeration switch control；
Adsorption system includes high temperature adsorption unit and low temperature adsorption unit, and high temperature adsorption unit includes being arranged in high-temperature incubator First gas surge tank and some coal sample tanks, first gas surge tank and each coal sample tank be arranged in parallel respectively by connecting tube On high-voltage tube between first interface and the 8th interface, circulate on the high-voltage tube between first interface and the 8th interface along gas Direction is sequentially connected in series is equipped with the first temperature sensor equipped with the first pneumatic operated valve and first pressure sensor, first gas surge tank With second pressure sensor, the connecting tube connected on first gas surge tank is equipped with the second pneumatic operated valve, on each coal sample tank point Not She You second temperature sensor and the 3rd pressure sensor, be respectively equipped with the 3rd gas in the connecting tube connected on each coal sample tank Dynamic valve；
Low temperature adsorption unit includes the second gas surge tank being arranged in cryostat and some coal sample tanks, second gas are delayed Rush tank and each coal sample tank is arranged in parallel on the high-voltage tube between the 5th interface and the 9th interface by connecting tube respectively, the 5th It is sequentially connected in series on high-voltage tube between interface and the 9th interface along gas circulating direction equipped with the 4th pneumatic operated valve and the 4th pressure biography Sensor, second gas surge tank are equipped with three-temperature sensor and the 5th pressure sensor, are connected on second gas surge tank Connecting tube be equipped with the 5th pneumatic operated valve, be respectively equipped with the 4th temperature sensor and the 6th pressure sensor on each coal sample tank, The 6th pneumatic operated valve is respectively equipped with the connecting tube connected on each coal sample tank；
Desorption system includes gas drainage metering device, electronic balance and some desorption gas flowmeters being connected in parallel, each solution The range of air-breathing flowmeter body is different, and each desorption gas flowmeter is connected by high-voltage tube with the 7th interface respectively, often The 7th pneumatic operated valve is respectively equipped with high-voltage tube between a desorption gas flowmeter and the 7th interface；
Gas drainage metering device includes tank, drainpipe and collecting container, and tank upper end passes through high-voltage tube and the 6th Interface connects, and the high-voltage tube between tank and the 6th interface is equipped with the 8th pneumatic operated valve, drainpipe one end and tank Bottom connects, and with being connected at the top of collecting container, collecting container is placed on electronic balance the drainpipe other end, is connected on the tenth interface Evacuated tube is connected to, evacuated tube is equipped with the 9th pneumatic operated valve；
Data collecting system includes computer and control unit, and control unit includes the 3rd control panel, on the 3rd control panel Equipped with pressure logging, temperature polling instrument, flow meter display, for control second source switch cryostat switch, For controlling the high-temperature incubator switch of the first power switch, and for control pressure logging and temperature polling instrument the 3rd Power switch, computer control connection first gas pressure reducing valve, second gas pressure reducing valve, the first five-way valve, the second five-way valve and First to the 9th pneumatic operated valve.
2. high/low temperature High Pressure Absorption test device for desorption according to claim 1, it is characterised in that：In high temperature adsorption unit The 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 sample Tank, the coal sample tank is five in low temperature adsorption unit, is respectively the 6th coal sample tank, the 7th coal sample tank, the 8th coal sample tank, the 9th Coal sample tank and the tenth coal sample tank.
3. high/low temperature High Pressure Absorption test device for desorption according to claim 1 or 2, it is characterised in that：In desorption system The desorption gas flow is calculated as three, is respectively the first desorption gas flowmeter, the second desorption gas flowmeter and the 3rd solution Air-breathing flowmeter body, the range of the first desorption gas flowmeter are 0-2000ml/min, the range of the second desorption gas flowmeter For 0-500ml/min, the range of the 3rd desorption gas flowmeter is 0-100ml/min；The flow meter display is three, point Wei not be corresponding first-class with the first desorption gas flowmeter, the second desorption gas flowmeter and the 3rd desorption gas flowmeter Gauge display, second flowmeter display and the 3rd flow meter display.
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