AU2022202272B2 - Gas detection device and method - Google Patents
Gas detection device and method Download PDFInfo
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- AU2022202272B2 AU2022202272B2 AU2022202272A AU2022202272A AU2022202272B2 AU 2022202272 B2 AU2022202272 B2 AU 2022202272B2 AU 2022202272 A AU2022202272 A AU 2022202272A AU 2022202272 A AU2022202272 A AU 2022202272A AU 2022202272 B2 AU2022202272 B2 AU 2022202272B2
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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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
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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
- G01N7/14—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
- G01N7/16—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 by heating the material
Abstract
A gas detection device includes: a methane input section for feeding methane; an air
input section for feeding air; a temperature controlled box provided with a sample tank; a
temperature sensor and a pressure sensor disposed in the sample tank; a vacuum pumping
5 section connected to a main gas inlet path of the sample tank and configured to evacuate the
sample tank; a desorption measuring cylinder and a gas sample collection bag each connected
to a gas outlet path of the sample tank; and a controller electrically connected to the methane
input section, the air input section, the vacuum pumping section and the temperature
controlled box, respectively, and the methane input section, the vacuum pumping section and
10 the air input section are each connected to a main gas inlet path of the sample tank.
Description
The present disclosure relates to the field of gas detection, and more particularly to a gas
detection device and method.
Coal spontaneous combustion (CSC), which is the main cause of underground fires and
gas explosions, seriously threatens mining safety. With the gradual increase in the depth of
coal mining, the coal and rock occurrence environment features more prominent
characteristics of high-ground-stress, high-temperature and high-seepage-pressure, and the
compound disaster of gas and CSC will be a common disaster threatening coal mining safety.
Gas in coal mainly exists in a form of adsorbed gas (more than 90%). The spontaneous
combustion of residual coal in goaf is accompanied by desorption and migration of adsorbed
gas and the competitive adsorption of gas and oxygen in airflow. Therefore, CSC is inevitably
affected by the residual gas in coal. However, at present, few studies were conducted on the
variations for the generation of oxidative gas and characteristics of oxygen consumption in
the spontaneous combustion of gas-bearing coal. Moreover, there is a lack of related
equipment and method that can be directly applied in research.
Embodiments of the present disclosure seek to solve at least one of the problems existing
in the related art to at least some extent.
In a first aspect of the present disclosure, a gas detection device is provided. The gas
detection device includes:
a methane input section for feeding methane;
an air input section for feeding air;
a temperature controlled box provided with a sample tank for placing a coal sample;
a vacuum pumping section connected to a main gas inlet path of the sample tank and
configured to evacuate the sample tank;
a desorption measuring cylinder connected to a gas outlet path of the sample tank, and configured to measure a quantity of methane removed from the coal sample; a gas sample collection bag connected to the gas outlet path of the sample tank, and configured to collect a gas sample from the gas outlet path; and a controller electrically connected to the methane input section, the air input section, the vacuum pumping section and the temperature controlled box, respectively, and configured to control the methane input section and the air input section to control and detect an input flow of methane and air. The sample tank includes a temperature sensor and a pressure sensor, and the main gas inlet path of the sample tank is connected to the methane input section and the air input section, respectively. In some embodiments of the present disclosure, the gas detection device further includes: a helium input section connected to the main gas inlet path. The helium input section includes: a helium cylinder, connected to the main gas inlet path; and a first pressure reducing valve, a first throttle valve and a first pressure sensor, located between the helium cylinder and the main gas inlet path and electrically connected to the controller, respectively. In some embodiments of the present disclosure, the methane input section includes: a methane cylinder, connected to the main gas inlet path; and a second pressure reducing valve, a second throttle valve and a second pressure sensor, located between the methane cylinder and the main gas inlet path and electrically connected to the controller, respectively. In some embodiments of the present disclosure, the air input section includes: a compressed air cylinder, connected to the main gas inlet path; and a third pressure reducing valve, a third throttle valve and a third pressure sensor, located between the compressed air cylinder and the main gas inlet path and electrically connected to the controller, respectively. In some embodiments of the present disclosure, the gas detection device further includes: a main stop valve, located on the main gas inlet path, electrically connected to the controller, and configured to open or close the main gas inlet path; a main flow control valve, located on the main gas inlet path, electrically connected to the controller, and configured to control an input flow; a main flowmeter, located on the main gas inlet path, electrically connected to the controller, and configured to detect the input flow; an explosion-proof valve, located on the main gas inlet path, and configured to prevent gas backflow from the sample tank; and a three-way valve, located on the gas outlet path, and connecting the desorption measuring cylinder and the gas sample collection bag to the gas outlet path. In some embodiments of the present disclosure, the vacuum pumping section includes: a vacuum pump, connected to the main gas inlet path; and a vacuum pumping stop valve, located between the vacuum pump and the main gas inlet path and electrically connected to the controller. In some embodiments of the present disclosure, the gas detection device further includes a gas discharging section, connected to the main gas inlet path, and configured to discharge gas inside the sample tank. The gas discharging section includes: a gas discharging path, connected to the main gas inlet path; and a gas discharging valve, located on the gas discharging path and electrically connected to the controller. In some embodiments of the present disclosure, the sample tank has a sealed cabin. The sealed cabin includes: a sealing cover; a screen mesh, configured to place the coal sample; a gas outlet, located on the sealing cover and connected to the gas outlet path; and a gas inlet, located below the screen mesh, and connected to the main gas inlet path via a gas preheating pipe. In some embodiments of the present disclosure, the temperature sensor and the pressure sensor are located in the sealed cabin, and connected to a data collector through a temperature monitoring circuit and a pressure monitoring circuit, respectively. The data collector is connected to the controller. In a second aspect of the present disclosure, a gas detection method is provided. The method includes: starting a vacuum pumping section to evacuate a sample tank when a coal sample is placed in the sample tank; starting a methane input section to inject into the sample tank methane with a predetermined pressure, and starting a temperature controlled box where the sample tank is located to maintain an initial temperature; determining whether a pressure of the sample tank reaches an adsorption balance pressure according to pressure detection data transmitted by a pressure sensor in the sample tank when the coal sample adsorbs methane for an adsorption balance time; opening a gas outlet path of the sample tank to remove free methane when the pressure of the sample tank reaches the adsorption balance pressure, and measuring a quantity of the removed methane through a desorption measuring cylinder connected to the gas outlet path; starting an air input section to inject into the sample tank air with a predetermined flow; heating the sample tank uniformly by the temperature controlled box to a maximum testing temperature, and analyzing by a gas chromatography and mass spectrometry analyzer a gas sample collected by a gas sample collection bag connected to the gas outlet path each time the temperature is raised by a certain temperature; obtaining a real-time desorption quantity of original methane in the coal sample according to a quantity of released gas measured by the desorption measuring cylinder; and obtaining a relationship between a quantity of residual methane and a gas product of the coal sample in low-temperature oxidation according to detection data in above-mentioned processes. In some embodiments of the present disclosure, the gas detection method further includes: starting a helium input section and a main stop valve connected to a gas inlet of the sample tank to inject into the sample tank helium with a predetermined pressure; detecting a gas tightness of the sample tank according to detection data of the pressure sensor in the sample tank; and closing the helium input section and opening a gas discharging section to empty the sample tank after the gas tightness is detected. In some embodiments of the present disclosure, the starting the vacuum pumping section to evacuate the sample tank when the coal sample is placed in the sample tank includes: closing the gas discharging section, and starting a vacuum pump and a vacuum pumping stop valve to evacuate the sample tank for not less than a predetermined time; and closing the vacuum pump and the vacuum pumping stop valve after the sample tank is evacuated. In some embodiments of the present disclosure, the starting the methane input section to inject into the sample tank methane with the predetermined pressure, and the starting the temperature controlled box where the sample tank is located to maintain an initial temperature, include: opening a methane cylinder, a second pressure reducing valve and a second throttle valve; controlling the methane input section to inject methane with the predetermined pressure into the sample tank according to detection data detected by a second pressure sensor; and opening the temperature controlled box to maintain the initial temperature at 303.15 K. In some embodiments of the present disclosure, the determining whether the pressure of the sample tank reaches the adsorption balance pressure according to pressure detection data transmitted by the pressure sensor in the sample tank when the coal sample adsorbs methane for the adsorption balance time includes: determining whether the pressure of the sample tank reaches an adsorption balance pressure of 0.5 to 5.0 MPa according to the pressure detection data transmitted by the pressure sensor in the sample tank when the coal sample adsorbs methane for an adsorption balance time of not less than 12 h. In some embodiments of the present disclosure, the opening the gas outlet path of the sample tank to remove free methane when the pressure of the sample tank reaches the adsorption balance pressure, and the measuring the quantity of the removed methane through the desorption measuring cylinder connected to the gas outlet path includes: opening a three-way valve on the gas outlet path of the sample tank to remove free methane when the pressure of the sample tank reaches the adsorption balance pressure; and measuring the quantity of the removed methane through the desorption measuring cylinder connected to the three-way valve. In some embodiments of the present disclosure, the starting the air input section to inject into the sample tank air with the predetermined flow includes: opening a compressed air cylinder, a third pressure reducing valve and a third throttle valve; controlling the air input section to inject air with the predetermined pressure into the sample tank according to detection data detected by a third pressure sensor; and detecting and controlling a flow rate of air injected into the sample tank through a main flow control valve and a main flowmeter connected to the gas inlet of the sample tank. In some embodiments of the present disclosure, the heating the sample tank uniformly by the temperature controlled box to the maximum testing temperature, and the analyzing by the gas chromatography and mass spectrometry analyzer the gas sample collected by the gas sample collection bag connected to the gas outlet path each time the temperature is raised by the certain temperature include: heating the sample tank by the temperature controlled box from 303.15 K to 533.15 K at a constant heating rate of 1 C/min; and analyzing by the gas chromatography and mass spectrometry analyzer the gas sample collected by the gas sample collection bag connected to the three-way valve every time the temperature is raised by 5 °C. In some embodiments of the present disclosure, the obtaining the relationship between the quantity of residual methane and the gas product of the coal sample in low-temperature oxidation according to detection data in above-mentioned processes includes: performing the previous operations for different coal samples and different adsorption balance pressures; and obtaining the relationship between different quantities of residual methane and the gas product of different coal samples in low-temperature oxidation according to detection data acquired in each detecting process. Additional aspects and advantages of embodiments of present disclosure will be given in part in the following descriptions, become apparent in part from the following descriptions, or be learned from the practice of the embodiments of the present disclosure.
BRIEF DESCRIPTION OF THE DRAWINGS These and other aspects and advantages of embodiments of the present disclosure will become apparent and more readily appreciated from the following descriptions made with reference to the drawings, in which: FIG. 1 is a schematic diagram showing a gas detection device according to an embodiment of the present disclosure.
FIG. 2 is a schematic diagram showing a sample tank according to an embodiment of the present disclosure. Reference numerals: 1: vacuum pump; 101: gas discharging valve; 102: vacuum pumping stop valve; 103: main stop valve; 104: main flow control valve; 105: explosion-proof valve; 106: three-way valve; 2: methane cylinder; 201: second pressure reducing valve; 202: second throttle valve; 203: second pressure sensor; 3: compressed air cylinder; 301: third pressure reducing valve; 302: third throttle valve; 303: third pressure sensor; 4: helium cylinder; 401: first pressure reducing valve; 402: first throttle valve; 403: first pressure sensor; 5: temperature controlled box; 6: gas preheating pipe; 7: sample tank; 8: main flowmeter; 9: desorption measuring cylinder; 10: gas sample collection bag; 11: temperature sensor; 12: pressure sensor; 13: data collector; 14: controller; 15: temperature monitoring circuit; 16: pressure monitoring circuit; 17: gas outlet; 18: sealing cover; 19: sealed cabin; 20: screen mesh; 21: gas inlet.
DETAILED DESCRIPTION Reference will be made in detail to embodiments of the present disclosure. The embodiments described herein with reference to drawings are explanatory and illustrative, which are only a part of embodiments of the present disclosure and used to generally understand the present disclosure. The embodiments shall not be construed to limit the present disclosure. All other embodiments obtainable by those skilled in the art based on the present disclosure without creative works shall fall within the scope of the present disclosure. The same or similar elements and the elements having same or similar functions are denoted by like reference numerals throughout the descriptions. In order to solve problems existing in the related art, the present disclosure provides a gas detection device and method for detecting gas adsorption/desorption coupling during coal oxidation at a rising temperature, which can be used for the experimental study on spontaneous combustion of coal with different methane quantities and the exploration of the influence of the residual gas quantity in coal on the characteristic parameters such as gas product generation and oxygen consumption rate, such that the gas detection device method according to embodiments of the present disclosure can provide scientific data support for the establishment of early warning index system of the spontaneous combustion of gas-bearing coal, which is of great significance to the disaster prevention and control engineering practice of coal seams with high gas quantity and prone to spontaneous combustion. As shown in FIG. 1 and FIG. 2, embodiments of the present disclosure provide a gas detection device for detecting gas adsorption/desorption coupling during coal oxidation at a rising temperature. The gas detection device includes a controller 14 and a temperature controlled box 5, and the controller 14 may be an industrial control computer or a programmable logic controller (PLC). The temperature controlled box 5 is provided with a sample tank 7 for placing a coal sample. A main gas inlet path of the sample tank 7 is connected to a methane input section and an air input section, respectively. A vacuum pumping section is connected to the main gas inlet path, and is configured to evacuate the sample tank 7. The vacuum pumping section may evacuate the main input gas path and the sample tank 7 before feeding methane into the sample tank 7, thereby avoiding interference of gases not required in the detection. A gas outlet path of the sample tank 7 is connected to a desorption measuring cylinder 9 and a gas sample collection bag 10, respectively. When the gas outlet path is opened, the gas in the sample tank 7 may enter into the desorption measuring cylinder 9 and the gas sample collection bag 10. A reading of the desorption measuring cylinder 9 may be read and input into the controller 14 by a user directly, or be obtained by analyzing an image displaying the reading and collected by an image acquisition device such as a camera. A gas sample collected by the gas sample collection bag 10 may be analyzed by a gas chromatography and mass spectrometry analyzer to obtain compositions and concentration of the released gas and a quantity of C13 isotope in methane. The sample tank 7 includes therein a temperature sensor 11 and a pressure sensor 12, which are electrically connected to the controller 14, respectively, such that the controller 14 may keep track of the temperature and pressure variations within the coal sample tank 7 in time, thereby ensuring the smooth running of the detection process. The controller 14 is electrically connected to the methane input section and the air input section to control the methane input section and the air input section to control and detect an input flow of methane and air. The controller 14 is also electrically connected to the vacuum pumping section and the temperature controlled box 5, respectively. The temperature controlled box 5 may be a temperature-programmed box, and may be configured to control a temperature and a heating rate through the controller. In order to ensure the accuracy of the detection, the gas tightness of the gas detection device may be detected by the following configurations. The main gas inlet path is connected to a helium input section. The helium input section includes a helium cylinder 4, a first pressure reducing valve 401, a first throttle valve 402 and a first pressure sensor 403. The helium cylinder 4 is connected to the main gas inlet path. The first pressure reducing valve 401, the first throttle valve 402 and the first pressure sensor 403 are located between the helium cylinder 4 and the main gas inlet path and electrically connected to the controller 14, respectively. When detecting the gas tightness, the controller 14 controls the helium input section to activate, and helium with a certain pressure is fed into the sample tank 7 through the main gas inlet path. The pressure may be detected and controlled by the first pressure reducing valve 401, the first throttle valve 402, and the first pressure sensor 403. The controller 14 may obtain a detection signal of the pressure sensor 12 to determine pressure variation in the sample tank 7 so as to determine the gas tightness of the sample tank 7. The pressure reducing valves, the throttle valves and the pressure sensors in other gas input sections work in an analogous way, which will not be elaborated here. The methane input section includes a methane cylinder 2, a second pressure reducing valve 201, a second throttle valve 202 and a second pressure sensor 203. The methane cylinder 2 is connected to the main gas inlet path. The second pressure reducing valve 201, the second throttle valve 202 and the second pressure sensor 203 are located between the methane cylinder 2 and the main gas inlet path and electrically connected to the controller 14, respectively. The air input section includes a compressed air cylinder 3, a third pressure reducing valve 301, a third throttle valve 302 and a third pressure sensor 303. The compressed air cylinder 3 is connected to the main gas inlet path. The third pressure reducing valve 301, the third throttle valve 302 and the third pressure sensor 303 are located between the compressed air cylinder 3 and the main gas inlet path and electrically connected to the controller 14, respectively. In some embodiments of the present disclosure, the gas detection device further includes a main stop valve 103, a main flow control valve 104 and a main flowmeter 8, which are located on the main gas inlet path and electrically connected to the controller 14. The main stop valve 103 is configured to open or close the main gas inlet path. The main flow control valve 104 is configured to control an input flow in the main gas inlet path. The main flowmeter 8 is configured to detect the input flow in the main gas inlet path. When the main stop valve 103 is closed, no gas is fed into the sample tank 7 through the main input gas path, and the main flow control valve 104 and the main flow meter 8 cooperate with each other to control the input flow of the gas like the air. The gas detection device further includes an explosion-proof valve 105 located on the main gas inlet path. The explosion-proof valve 105 is configured to prevent gas backflow from the high-pressure sample tank 7, and used for explosion-proof and flame-proof for the oxidation reaction of the coal sample in the high-pressure sample tank 7, thereby ensuring the safety of the detection process. The gas detection device further includes a three-way valve 106 located on the gas outlet path. The desorption measuring cylinder 9 and the gas sample collection bag 10 are connected to the gas outlet path through the three-way valve 106. In some embodiments of the present disclosure, the vacuum pumping section includes a vacuum pump 1 connected to the main gas inlet path, and a vacuum pumping stop valve 102 located between the vacuum pump 1 and the main gas inlet path and electrically connected to the controller 14. The gas detection device further includes a gas discharging section, which is connected to the main gas inlet path, and configured to discharge gas inside the sample tank 7. The gas discharging section includes a gas discharging path connected to the main gas inlet path, and a gas discharging valve 101 located on the gas discharging path and electrically connected to the controller 14. In some embodiments of the present disclosure, the sample tank 7 has a sealed cabin 19. The sealed cabin 19 includes a sealing cover 18, a screen mesh 20 for placing the coal sample, a gas outlet 17 located on the sealing cover 18, and a gas inlet 21 located below the screen mesh 20. The gas inlet 21 is connected to the main gas inlet path via a gas preheating pipe 6. The gas outlet 17 is connected to the gas outlet path. The temperature sensor 11 and the pressure sensor 12 are located in the sealed cabin 19, and connected to a data collector 13 through a temperature monitoring circuit 15 and a pressure monitoring circuit 16, respectively. The data collector 13 is connected to the controller 14. The gas detection device as described in any above-mentioned embodiment may be used for detecting gas adsorption/desorption coupling during coal oxidation at a rising temperature, which may be implemented as follows. The coal sample with a certain particle size is placed in the high-pressure sample tank 7, followed by tightening the sample tank 7. The temperature sensor 11 and the high-temperature pressure sensor 12 are connected to the sample tank 7. The gas discharging section 101, the vacuum pumping stop valve 102, the methane cylinder 2, the second pressure reducing valve 201, the second throttle valve 202, the compressed air cylinder 3, the third pressure reducing valve 301, the third throttle valve 302 and the three-way valve 106 are closed. The main stop valve 103 and the main flow control valve 104 are opened, and then the high-pressure helium cylinder 4, the first pressure reducing valve 401 and the first throttle valve 402 are opened. The helium cylinder 4 is controlled to inject helium with a pressure of 5 to 7 MPa into the sample tank 7 according to a reading of a pressure gauge of the helium cylinder 4. Variation of gas pressure in the high-pressure sample tank 7 is observed through a data acquisition and storage unit including the high-temperature pressure sensor 12, the data collector 13 and the industrial control computer 14 to determine the gas tightness of the device. After the gas tightness is detected, the high-pressure helium cylinder 4, the first pressure reducing valve 401 and the first throttle valve 402 are closed, and the gas discharging valve 101 is opened. When the helium in the sample tank is emptied, the gas discharging valve 101 is closed, and the vacuum pumping stop valve 102 and the vacuum pump 1 are opened to evacuate the sample tank for at least 4 h. After the sample tank is evacuated, the vacuum pump 1 and the vacuum pumping stop valve 102 are closed, and the high-pressure methane cylinder 2, the second pressure reducing valve 201 and the second throttle valve 202 are opened. The methane cylinder 2 is controlled to inject methane with a predetermined pressure of 0.5 to 5.0 MPa into the sample tank 7 according to a reading of a pressure gauge of the methane cylinder 2. The temperature-programmed box 5 is opened to maintain an initial temperature at 303.15 K. The coal sample in the high-pressure sample tank 7 adsorbs methane for an adsorption balance time of not less than 12 h. At the same time, based on data monitored by the high-temperature pressure sensor 12, the data collector 13, and the industrial control computer 14, the adsorption balance pressure of the coal sample in the sample tank is ensured to reach a predetermined value of 0.5 to 5.0 MPa. When the adsorption balance pressure of the coal sample in the sample tank 7 is reached, the three-way valve 106 is opened to remove free methane of the high-pressure sample tank 7, and the quantity of the removed methane is measured through the desorption measuring cylinder 9. At the same time, the compressed air cylinder 3, the third pressure reducing valve 301 and the third throttle valve 302 are opened. The compressed air cylinder 3 is controlled to inject a certain amount of air into the sample tank 7 according to a reading of a pressure gauge of the compressed air cylinder 3. The air is controlled to be injected into the high-pressure sample tank 7 at a predetermined flow of 50 mL/min by the main flow control valve 104, and the air flow is monitored by the main flowmeter 8 in real time. The sample tank 7 is heated from 303.15 K to 533.15 K at a constant heating rate of 1 C/min, During the hating process, the quantity of gas released from the sample tank 7 is measured through the desorption measuring cylinder 9 in real time, and each time the temperature is raised by 5 °C, a gas sample is collected by the gas sample collection bag 10 and is analyzed by the gas chromatography and mass spectrometry analyzer to obtain compositions and concentration of the released gas and a quantity of C13 isotope in the methane. With the aid of the data obtained by the desorption measuring cylinder 9, a real-time desorption quantity of original methane (13CH 4 ) in the coal sample is obtained. The coal sample in the high-pressure sample tank 7 is replaced after the raising temperature oxidation process, and the above-mentioned steps are repeated in sequence, except that the methane pressure for the adsorption balance of the coal sample is adjusted. By gradually adjusting the methane pressure for the adsorption balance of the coal sample, the variations of the gas product released in low-temperature oxidation of gas-bearing coal samples with different residual methane quantities is obtained. The specific calculation is as follows. A free volume Vz in the high-pressure sample tank 7 containing the coal sample may be obtained as follows. A true density d of the coal sample is obtained by a true density meter, and an actual volume Vd of the coal sample in the high-pressure sample tank 7 is calculated. The free volume Vz in the high-pressure sample tank 7 containing the coal sample is a difference between an internal volume Vo of the empty sample tank 7 and the actual volume
Vd of the coal sample. The residual methane quantity in the coal sample may be obtained as follows. An original methane quantity Q of the coal sample may be determined by the gas-solid adsorption Langmuir theory, and a residual methane quantity Qc of the coal sample in the high-pressure sample tank 7 is a difference between the original methane quantity Q of the coal sample and a quantity Qf of free methane removed at the beginning of the detection method, and a quantity Qt of methane desorbed from the coal sample and measured by the desorption measuring cylinder 9 in real time. The calculation formulas are as follows. 'rn d
Vz= VO-V
abP VZPTO 1+ bP mT POE
QC= Q- - Q
m m where Q --- original methane quantity of the coal sample, mL/g;
Q - quantity of free methane removed at the beginning of the detection method, mL; Qt --- quantity of methane desorbed from the coal sample in a time t, mL; Qc - quantity of residual methane of the coal sample in the time t, mL/g; Vo --- internal volume of the empty sample tank, cm 3;
Vd --- actual volume of the coal sample, not including pore volume, cm 3
Vz --- internal free volume of the sample tank with the coal sample, cm 3 d --- true density of the coal sample, g/cm 3;
m --- quality of the coal sample in the sample tank, g;
a and b --- Langmuir adsorption constants;
P --- gas pressure (13CH4 adsorption balance pressure in the sample tank), Pa; T --- absolute temperature, K;
s--- compression coefficient of methane;
Po --- pressure in a standard state, 101325 Pa; and To --- absolute temperature in the standard state, 273.15 K. Embodiments of the present disclosure also provide a gas detection method for gas adsorption/desorption coupling during coal oxidation at a rising temperature. The gas detection method is applied to the gas detection device as described in any embodiment hereinbefore. The gas detection includes: starting the vacuum pumping section to evacuate the sample tank when a coal sample is placed in the sample tank; starting the methane input section to inject into the sample tank methane with a predetermined pressure, and starting the temperature controlled box where the sample tank is located to maintain an initial temperature; determining whether a pressure of the sample tank reaches an adsorption balance pressure according to pressure detection data transmitted by the pressure sensor in the sample tank when the coal sample adsorbs methane for an adsorption balance time; opening the gas outlet path of the sample tank to remove free methane when the pressure of the sample tank reaches the adsorption balance pressure, and measuring a quantity of the removed methane through the desorption measuring cylinder connected to the gas outlet path; starting the air input section to inject into the sample tank air with a predetermined flow; heating the sample tank uniformly by the temperature controlled box to a maximum testing temperature, and analyzing by a gas chromatography and mass spectrometry analyzer a gas sample collected by the gas sample collection bag connected to the gas outlet path each time the temperature is raised by a certain temperature; obtaining a real-time desorption quantity of original methane in the coal sample according to a quantity of released gas measured by the desorption measuring cylinder; and obtaining a relationship between a quantity of residual methane and a gas product of the coal sample in low-temperature oxidation according to detection data acquired in above-mentioned processes. Further, the gas detection method further includes: starting the helium input section and the main stop valve connected to the gas inlet of the sample tank to inject into the sample tank helium with a predetermined pressure; detecting a gas tightness of the sample tank according to detection data of the pressure sensor in the sample tank; and closing the helium input section and opening the gas discharging section to empty the sample tank after the gas tightness is detected. In some embodiments of the present disclosure, the starting the vacuum pumping section to evacuate the sample tank when the coal sample is placed in the sample tank includes: closing the gas discharging section, and starting the vacuum pump and the vacuum pumping stop valve to evacuate the sample tank for not less than a predetermined time; and closing the vacuum pump and the vacuum pumping stop valve after the sample tank is evacuated. In some embodiments of the present disclosure, the starting the methane input section to inject into the sample tank methane with the predetermined pressure, and the starting the temperature controlled box where the sample tank is located to maintain the initial temperature, include: opening the methane cylinder, the second pressure reducing valve and the second throttle valve; controlling the methane input section to inject methane with the predetermined pressure into the sample tank according to detection data detected by the second pressure sensor; and opening the temperature controlled box to maintain the initial temperature at 303.15 K. In some embodiments of the present disclosure, the determining whether the pressure of the sample tank reaches the adsorption balance pressure according to the pressure detection data transmitted by the pressure sensor in the sample tank when the coal sample adsorbs methane for the adsorption balance time includes: determining whether the pressure of the sample tank reaches an adsorption balance pressure of 0.5 to 5.0 MPa according to the pressure detection data transmitted by the pressure sensor in the sample tank when the coal sample adsorbs methane for an adsorption balance time of not less than 12 h. In some embodiments of the present disclosure, the opening the gas outlet path of the sample tank to remove free methane when the pressure of the sample tank reaches the adsorption balance pressure, and the measuring the quantity of the removed methane through the desorption measuring cylinder connected to the gas outlet path includes: opening the three-way valve on the gas outlet path of the sample tank to remove free methane when the pressure of the sample tank reaches the adsorption balance pressure; and measuring the quantity of the removed methane through the desorption measuring cylinder connected to the three-way valve. In some embodiments of the present disclosure, the starting the air input section to inject into the sample tank air with the predetermined flow includes: opening the compressed air cylinder, the third pressure reducing valve and the third throttle valve; controlling the air input section to inject air with the predetermined pressure into the sample tank according to detection data detected by the third pressure sensor; and detecting and controlling a flow rate of air injected into the sample tank through the main flow control valve and the main flowmeter connected to the gas inlet of the sample tank. In some embodiments of the present disclosure, the heating the sample tank uniformly by the temperature controlled box to the maximum testing temperature, and the analyzing by the gas chromatography and mass spectrometry analyzer the gas sample collected by the gas sample collection bag connected to the gas outlet path each time the temperature is raised by the certain temperature include: heating the sample tank by the temperature controlled box from 303.15 K to 533.15 K at a constant heating rate of 1 C/min; and analyzing by the gas chromatography and mass spectrometry analyzer the gas sample collected by the gas sample collection bag connected to the three-way valve every time the temperature is raised by 5 °C. In some embodiments of the present disclosure, the obtaining the relationship between the quantity of residual methane and the gas product of the coal sample in low-temperature oxidation according to detection data acquired in above-mentioned processes includes: performing the previous operations for different coal samples and different adsorption balance pressures; and obtaining the relationship between different quantities of residual methane and the gas product of different coal samples in low-temperature oxidation according to detection data acquired in each detecting process. In embodiments of the present disclosure, under different methane adsorption balance pressures, the coal sample may have different methane content.
In the following, the gas detection method will be illustrated with reference to an example where the methane adsorption balance pressure is 1.0 MPa. A true density d of a coal sample is tested by a true density meter, an actual volume Vd of the coal sample in the high-pressure sample tank is obtained by calculation. An internal volume Vo of the empty sample tank is obtained by an irrigation method. An inter free volume Vz of the sample tank containing the coal sample is a difference between the internal volume Vo of the empty sample tank and the actual volume Vd of the coal sample. 50 g of a coal sample with a particle size of 0.074 to 0.2 mm is placed in the high-pressure sample tank, followed by tightening the sample tank 7. The temperature sensor 11 and the high-temperature pressure sensor 12 are connected to the sample tank 7. The gas discharging valve, the vacuum pumping stop valve, the high-pressure methane cylinder, the second pressure reducing valve, the second throttle valve, the compressed air cylinder, the third pressure reducing valve, the third throttle valve and the three-way valve are closed. The main stop valve and the main flow control valve are opened, and then the high-pressure helium cylinder, the first pressure reducing valve, and the first throttle valve are opened. The helium cylinder is controlled to inject helium with a pressure of 5 to 7 MPa into the sample tank according to a reading of a pressure gauge of the helium cylinder. Variation of gas pressure in the high-pressure sample tank is observed through the data acquisition and storage unit including the high-temperature pressure sensor, the data collector and the industrial control computer to determine the gas tightness of the device. After the gas tightness is detected, the high-pressure helium cylinder, the first pressure reducing valve and the first throttle valve are closed, and the gas discharging valve is opened. When the helium in the sample tank is emptied, the gas discharging valve is closed, and the vacuum pumping stop valve and the vacuum pump are opened to evacuate the sample tank for at least 4 h. After the sample tank is evacuated, the vacuum pumping stop valve and the vacuum pump are closed, and the high-pressure methane cylinder, the second pressure reducing valve and the second throttle valve are opened. The methane cylinder is controlled to inject methane with a pressure of 1.0 MPa into the sample tank according to a reading of a pressure gauge of the methane cylinder. The temperature-programmed box is opened to maintain an initial temperature at 303.15 K. The coal sample in the high-pressure sample tank adsorbs methane for an adsorption balance time of not less than 12 h. At the same time, based on data monitored by the high-temperature pressure sensor, the data collector, and the industrial control computer, the adsorption balance pressure of the coal sample in the sample tank is ensured to reach 1.0 MPa. When the adsorption balance pressure of the coal sample in the sample tank is reached, the three-way valve is controlled to open a path between the gas outlet path and the desorption measuring cylinder to remove free methane of the high-pressure sample tank, and the quantity Qf of the removed methane is measured through the desorption measuring cylinder. At the same time, the compressed air cylinder, the third pressure reducing valve and the third throttle valve are opened. The compressed air cylinder is controlled to inject compressed air of 0.1 MPa into the sample tank according to a reading of a pressure gauge of the compressed air cylinder. The air is controlled to be injected into the high-pressure sample tank at a predetermined flow of 50 mL/min by the main flow control valve, and the air flow is monitored by the main flowmeter in real time. The sample tank is heated from 303.15 K to 533.15 K at a constant heating rate of 1 C/min. During the hating process, The quantity of the gas released from the sample tank is measured through the desorption measuring cylinder in real time, and each time the temperature is raised by 5°C, the heating is stopped for 10 min, so as to ensure the coal sample in the high-pressure sample tank to fully react with the air at the corresponding temperature. The temperatures of the coal sample and the sample tank are monitored by the temperature sensor in the high-pressure sample tank. After ensuring that the coal sample reacts smoothly, the path between the gas output path of the three-way valve and the desorption measuring cylinder is closed, and a path between the desorption measuring cylinder and the gas sample collection bag is opened to release all the gas in the desorption measuring cylinder into the gas sample collection bag. Then, the gas sample collection bag is replaced, and the path between the desorption measuring cylinder and the gas sample collection bag is closed, and the path between the gas output path of the three-way valve and the desorption measuring cylinder is opened to continue the heating process. The gas sample collected by the gas sample collection bag is analyzed by the gas chromatography and mass spectrometry analyzer to obtain the compositions and concentration of the released gas and the quantity of Cl3 isotope in the methane gas. Further, with the aid of the data obtained by the desorption measuring cylinder, a real-time desorption quantity Qt of original methane (1 3 CH4) in the coal sample is obtained and recorded.
After of the programed heating of the coal sample in the high-pressure sample tank is completed, a quantity of residual methane (13 CH4 ) in the coal sample is obtained as follows. An original methane quantity Q of the coal sample may be determined by the gas-solid adsorption Langmuir theory, and the residual methane quantity Qc of the coal sample in the high-pressure sample tank is a difference between the original methane quantity Q of the coal sample and the quantity Qf of free methane removed at the beginning of the detection method, and the quantity Qt of methane desorbed from the coal sample and measured by the desorption measuring cylinder in real time. The calculation formulas are as follows. m d
Vz=V 0 -V
abP VzPTO 1+ bP mT POE
QV=Q-Qf _Q t m m where Q --- original methane quantity of the coal sample, mL/g;
Qf -quantity of free methane removed at the beginning of the detection method, mL; Q, -quantity of methane desorbed from the coal sample in a time t, mL; Qc - quantity of residual methane of the coal sample in the time t, mL/g; Vo --- internal volume of the empty sample tank, cm3 3 Vd -- actual volume of the coal sample, not including pore volume, cm ;
Vz - internal free volume of the sample tank with the coal sample, cm 3; d --- true density of the coal sample, g/cm 3;
m --- quality of the coal sample in the sample tank, g;
a and b --- Langmuir adsorption constants;
P --- gas pressure (13CH4 adsorption balance pressure in the sample tank), Pa; T --- absolute temperature, K; s--- compression coefficient of methane;
Po --- pressure in a standard state, 101325 Pa; and
To --- absolute temperature in the standard state, 273.15 K.
In the gas detecting method and device according to embodiments of the present
disclosure, the controller may control the methane input section, the air input section, the
temperature controlled box and other units, and detection data may be obtained from various
detecting units, such that oxidation of a coal sample with absorbed gas at a rising temperature
was researched. Moreover, the gas detecting device has a simple construction, and the gas
detecting method has simple operations, and thus they have good application value. Further,
the gas detection device and method according to embodiments of the present disclosure can
be used to explore the spontaneous combustion characteristics of gas-bearing coal, the release
of oxidized gas products and oxygen consumption in the spontaneous combustion of the
gas-bearing coal, and analyze effects of residual gas in the coal on the spontaneous
combustion characteristics (such as a gas product generation, an oxygen consumption rate and
a characteristic temperature) of gas-bearing coal, which provide scientific data support for the
establishment of the prediction index system for the spontaneous combustion of gas-bearing
coal, which is conducive to the scientific implementation of the prevention and control
engineering practice of coal spontaneous combustion disaster in mine.
Although specific embodiments have been shown and described above, it would be
appreciated by those skilled in the art that the above embodiments are illustrative and cannot
be construed to limit the present disclosure, and changes, alternatives, and modifications can
be made in the embodiments without departing from spirit, principles and scope of the present
disclosure.
Claims (10)
1. A gas detection device, comprising:
a methane input section for feeding methane;
an air input section for feeding air;
a temperature controlled box provided with a sample tank for placing a coal sample,
wherein the sample tank comprises a temperature sensor and a pressure sensor, and a main
gas inlet path of the sample tank is connected to the methane input section and the air input
section, respectively;
a vacuum pumping section connected to the main gas inlet path of the sample tank and
configured to evacuate the sample tank;
a desorption measuring cylinder connected to a gas outlet path of the sample tank, and
configured to measure a quantity of methane removed from the coal sample;
a gas sample collection bag connected to the gas outlet path of the sample tank, and
configured to collect a gas sample from the gas outlet path; and
a controller electrically connected to the methane input section, the air input section, the
vacuum pumping section and the temperature controlled box, respectively, and configured to
control the methane input section and the air input section to control and detect an input flow
of methane and air.
2. The device according to claim 1, further comprising:
a helium input section connected to the main gas inlet path and comprising:
a helium cylinder, connected to the main gas inlet path; and
a first pressure reducing valve, a first throttle valve and a first pressure sensor,
located between the helium cylinder and the main gas inlet path and electrically
connected to the controller, respectively;
wherein the methane input section comprises:
a methane cylinder, connected to the main gas inlet path; and
a second pressure reducing valve, a second throttle valve and a second pressure sensor,
located between the methane cylinder and the main gas inlet path and electrically connected
to the controller, respectively;
wherein the air input section comprises: a compressed air cylinder, connected to the main gas inlet path; and a third pressure reducing valve, a third throttle valve and a third pressure sensor, located between the compressed air cylinder and the main gas inlet path and electrically connected to the controller, respectively.
3. The device according to claim 1, further comprising: a main stop valve, located on the main gas inlet path, electrically connected to the controller, and configured to open or close the main gas inlet path; a main flow control valve, located on the main gas inlet path, electrically connected to the controller, and configured to control an input flow; a main flowmeter, located on the main gas inlet path, electrically connected to the controller, and configured to detect the input flow; an explosion-proof valve, located on the main gas inlet path, and configured to prevent gas backflow from the sample tank; and a three-way valve, located on the gas outlet path, and connecting the desorption measuring cylinder and the gas sample collection bag to the gas outlet path.
4. The device according to claim 1, further comprising a gas discharging section, connected to the main gas inlet path, configured to discharge gas inside the sample tank and comprising: a gas discharging path, connected to the main gas inlet path; and a gas discharging valve, located on the gas discharging path and electrically connected to the controller; wherein the vacuum pumping section comprises: a vacuum pump, connected to the main gas inlet path; and a vacuum pumping stop valve, located between the vacuum pump and the main gas inlet path and electrically connected to the controller.
5. The device according to claim 1, wherein the sample tank has a sealed cabin; wherein the sealed cabin comprises: a sealing cover; a screen mesh, configured to place the coal sample; a gas outlet, located on the sealing cover and connected to the gas outlet path; and a gas inlet, located below the screen mesh, and connected to the main gas inlet path via a gas preheating pipe; wherein the temperature sensor and the pressure sensor are located in the sealed cabin, and connected to a data collector through a temperature monitoring circuit and a pressure monitoring circuit, respectively; wherein the data collector is connected to the controller.
6. A gas detection method, comprising: starting a vacuum pumping section to evacuate a sample tank when a coal sample is placed in the sample tank; starting a methane input section to inject into the sample tank methane with a predetermined pressure, and starting a temperature controlled box where the sample tank is located to maintain an initial temperature; determining whether a pressure of the sample tank reaches an adsorption balance pressure according to pressure detection data transmitted by a pressure sensor in the sample tank when the coal sample adsorbs methane for an adsorption balance time; opening a gas outlet path of the sample tank to remove free methane when the pressure of the sample tank reaches the adsorption balance pressure, and measuring a quantity of the removed methane through a desorption measuring cylinder connected to the gas outlet path; starting an air input section to inject into the sample tank air with a predetermined flow; heating the sample tank uniformly by the temperature controlled box to a maximum testing temperature, and analyzing by a gas chromatography and mass spectrometry analyzer a gas sample collected by a gas sample collection bag connected to the gas outlet path each time the temperature is raised by a certain temperature; obtaining a real-time desorption quantity of original methane in the coal sample according to a quantity of released gas measured by the desorption measuring cylinder; and obtaining a relationship between a quantity of residual methane and a gas product of the coal sample in low-temperature oxidation according to detection data in above-mentioned processes.
7. The method according to claim 6, further comprising: starting a helium input section and a main stop valve connected to a gas inlet of the sample tank to inject into the sample tank helium with a predetermined pressure; detecting a gas tightness of the sample tank according to detection data of the pressure sensor in the sample tank; and closing the helium input section and opening a gas discharging section to empty the sample tank after the gas tightness is detected; wherein the starting the vacuum pumping section to evacuate the sample tank when the coal sample is placed in the sample tank comprises: closing the gas discharging section, and starting a vacuum pump and a vacuum pumping stop valve to evacuate the sample tank for not less than a predetermined time; and closing the vacuum pump and the vacuum pumping stop valve after the sample tank is evacuated.
8. The method according to claim 7, wherein the starting the methane input section to inject into the sample tank methane with the predetermined pressure, and the starting the temperature controlled box where the sample tank is located to maintain the initial temperature, comprise: opening a methane cylinder, a second pressure reducing valve and a second throttle valve; controlling the methane input section to inject methane with the predetermined pressure into the sample tank according to detection data detected by a second pressure sensor; and opening the temperature controlled box to maintain the initial temperature at 303.15 K; wherein the determining whether the pressure of the sample tank reaches the adsorption balance pressure according to pressure detection data transmitted by the pressure sensor in the sample tank when the coal sample adsorbs methane for the adsorption balance time comprises: determining whether the pressure of the sample tank reaches an adsorption balance pressure of 0.5 to 5.0 MPa according to the pressure detection data transmitted by the pressure sensor in the sample tank when the coal sample adsorbs methane for an adsorption balance time of not less than 12 h.
9. The method according to claim 8, wherein the opening the gas outlet path of the sample tank to remove free methane when the pressure of the sample tank reaches the adsorption balance pressure, and the measuring the quantity of the removed methane through the desorption measuring cylinder connected to the gas outlet path comprise: opening a three-way valve on the gas outlet path of the sample tank to remove free methane when the pressure of the sample tank reaches the adsorption balance pressure; and measuring the quantity of the removed methane through the desorption measuring cylinder connected to the three-way valve; wherein the starting the air input section to inject into the sample tank air with the predetermined flow comprises: opening a compressed air cylinder, a third pressure reducing valve and a third throttle valve; controlling the air input section to inject air with the predetermined pressure into the sample tank according to detection data detected by a third pressure sensor; and detecting and controlling a flow rate of air injected into the sample tank through a main flow control valve and a main flowmeter connected to the gas inlet of the sample tank; wherein the heating the sample tank uniformly by the temperature controlled box to the maximum testing temperature, and the analyzing by the gas chromatography and mass spectrometry analyzer the gas sample collected by the gas sample collection bag connected to the gas outlet path each time the temperature is raised by the certain temperature comprise: heating the sample tank by the temperature controlled box from 303.15 K to 533.15 K at a constant heating rate of 1 C/min; and analyzing by the gas chromatography and mass spectrometry analyzer the gas sample collected by the gas sample collection bag connected to the three-way valve every time the temperature is raised by 5 °C.
10. The method according to claim 9, wherein the obtaining the relationship between the quantity of residual methane and the gas product of the coal sample in low-temperature oxidation according to detection data in above-mentioned processes comprises: performing the previous operations for different coal samples and different adsorption balance pressures; and obtaining the relationship between different quantities of residual methane and the gas product of different coal samples in low-temperature oxidation according to detection data acquired in each detecting process.
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