CN107860681B - Gas adsorption and desorption characteristic testing device and method for pre-adsorbing moisture coal sample - Google Patents
Gas adsorption and desorption characteristic testing device and method for pre-adsorbing moisture coal sample Download PDFInfo
- Publication number
- CN107860681B CN107860681B CN201711091105.2A CN201711091105A CN107860681B CN 107860681 B CN107860681 B CN 107860681B CN 201711091105 A CN201711091105 A CN 201711091105A CN 107860681 B CN107860681 B CN 107860681B
- Authority
- CN
- China
- Prior art keywords
- valve
- pressure
- coal sample
- gas
- adsorption
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Solid Fuels And Fuel-Associated Substances (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a gas adsorption and desorption characteristic testing device and a gas adsorption and desorption characteristic testing method for a pre-adsorbed moisture coal sample. The device can change the inherent water content of the coal sample through the water adsorption system, thereby being capable of researching the gas adsorption and desorption characteristics of the coal sample under different inherent water content conditions and the influence rule of the inherent water content, being capable of better reflecting the evolution rule of the gas adsorption and desorption performance of the in-situ coal reservoir, particularly the low-rank coal with higher inherent water content characteristics, not only being beneficial to effectively preventing and controlling coal bed gas disasters, but also being beneficial to reliably evaluating coal bed gas (gas) resources, and having simple structure, simple and convenient test steps and good use effect.
Description
Technical Field
The invention belongs to the technical field of gas experiments, and particularly relates to a gas adsorption and desorption characteristic testing device for pre-adsorbing a moisture coal sample, which is mainly suitable for simulating the gas adsorption and desorption characteristics of an in-situ coal reservoir under different internal moisture content conditions in a laboratory.
Background
The "strategic action plan for energy development (2014-plus 2020)" made by State administration indicates that "the national coal consumption proportion is controlled within 62% by 2020". Therefore, the primary energy structure mainly based on coal in China is still difficult to change in a long period in the future. Coal bed gas (gas) is formed in the coal-forming process and is present in coal reservoirs as methane (CH)4) The coal bed gas is a main mixed gas, is the first killer of the coal mine safety production in China, for example, 10 major gas accidents in China in 2014 occur, the number of dead people reaches 162, and accounts for 70.7% of the total number of dead people in the coal mine accidents in China, however, the coal bed gas is a clean and efficient energy source, and the resource amount of shallow coal bed gas (gas) reaches 32.86 × 10 when the depth of the coal bed buried in China is 2000m and the resource amount of shallow coal bed gas (gas) reaches 32.86 ×12m3And has great development and utilization prospect. In view of the two aspects, the gas adsorption and desorption characteristics of the in-situ coal reservoir are mastered so as to reliably evaluate the coal bed gas content, the coal bed gas recoverable resource amount and the like, and the method is the basis for treating and utilizing the coal bed gas.
In fact, an in situ coal reservoir is a geologic body in which three phases of coal, gas and water coexist. Water in coal exists mainly as free water in fissures and intrinsic water in the coal matrix, both forms. Intrinsic water is mainly present in the pore system of coal in the form of multi-molecular-layer physical adsorption and agglomeration. Especially low rank coals tend to have higher intrinsic moisture content due to their higher oxygen-containing functional groups and more developed micropore porosity. For example, the moisture content of lignite in China is as high as 25-40%, and the moisture content of long flame coal is 8.57% on average.
At present, the research on the influence of water on the gas adsorption and desorption characteristics in coal is mainly carried out in a laboratory, and more attention is paid to the influence of added water on the gas adsorption and desorption performance in coal under different water injection conditions, namely a test method for liquid water to invade a coal sample. Obviously, this ignores the effect of the inherent moisture in the coal. In fact, under the influence of pore interface tension, liquid water cannot overcome the interface tension and enter a small hole and micropore system, so that the method for injecting liquid water cannot reflect the influence rule of internal moisture on the coal adsorption and desorption characteristics, and cannot reduce the essence of the influence of moisture in an in-situ coal reservoir on the coal adsorption and desorption characteristics. Scholars at home and abroad also carry out adsorption and desorption tests of coal samples under different internal moisture content conditions, however, after the coal samples adsorb moisture in advance, the coal samples are subjected to a long-time vacuumizing process, and part of internal water in the coal is pumped out under the action of negative pressure. Therefore, the moisture content of the coal sample in the test process is less than the highest intrinsic moisture content, which is not favorable for analyzing the evolution law of gas adsorption and desorption of the coal sample under the condition of higher intrinsic moisture content.
Disclosure of Invention
The invention aims to solve the technical problem of providing a gas adsorption and desorption characteristic testing device and a gas adsorption and desorption characteristic testing method which are simple in structure, simple and convenient in testing method and capable of effectively pre-adsorbing a moisture coal sample.
In order to solve the technical problems, the invention is realized by the following technical scheme: a gas adsorption and desorption characteristic testing device for pre-adsorbing a moisture coal sample comprises a vacuum pumping system, an inflation system, a constant temperature system, a water adsorption system and a gas adsorption and desorption testing system;
the vacuum pumping system comprises a vacuum pump, a vacuum gauge pipe and a vacuum gauge which are connected with the vacuum pump, and a valve F1 and a valve F2 which are connected with a pumping and exhausting pipeline;
the gas charging system comprises a high-pressure helium tank, a high-pressure methane tank, a pressure reducing valve JF1 connected with the high-pressure helium tank and a pressure reducing valve JF2 connected with the high-pressure methane tank;
the water adsorption system comprises a glass vacuum vessel, a digital display humidity sensor arranged on the glass vacuum vessel and a valve F4 connected with the glass vacuum vessel;
the constant temperature system comprises a constant temperature water bath box;
the gas adsorption and desorption testing system comprises two reference tanks, a coal sample tank and a desorption measuring cylinder which have the same volume, a high-precision pressure gauge arranged on a connecting pipeline between the reference tanks and the coal sample tank, a valve F5 and a valve F3 which are connected with the reference tanks, a valve F6 arranged on a connecting pipeline between the coal sample tank and the high-precision pressure gauge, a valve F7 arranged on a connecting pipeline between the coal sample tank and the desorption measuring cylinder and a conical flask connected with the desorption measuring cylinder;
and the pipeline with the pressure reducing valve JF1 and the pressure reducing valve JF2 is communicated with a pipeline with a valve F4 in the water adsorption system after being converged, and the pumping and draining pipeline is communicated with a pipeline with a high-precision pressure gauge.
The invention provides a testing method of a gas adsorption and desorption characteristic testing device for a pre-adsorbed moisture coal sample, which comprises the following steps:
(a) mixing distilled water with the temperature of 60 ℃ and a certain amount of inorganic salt particles to prepare a saturated solution under the condition of 60 ℃, then pouring the saturated solution of the inorganic salt into a glass vacuum vessel and recovering the solution to the room temperature, then sealing the glass vacuum vessel to form a wet environment with the relative humidity reaching the corresponding humidity of the saturated solution of the inorganic salt, simultaneously filling a dry coal sample with the weight of 50g and the particle size of 0.2-0.25mm into a coal sample tank, screwing and sealing;
(b) closing a valve F1, a valve F2, a valve F4 and a valve F7, opening a valve F3, a valve F5 and a valve F6, opening a high-pressure helium bottle and a pressure reducing valve JF1 to fill helium with the pressure of 5-7 MPa, observing a high-precision pressure gauge to check the air tightness of the system, closing the high-pressure helium bottle and the pressure reducing valve JF1 and opening a valve F2 after the air tightness check is finished, completely discharging the helium in the system, then closing the valve F2 and opening a valve F1, and starting a vacuum pump until the pressure value of a vacuum gauge is reduced to be below 4 Pa;
(c) starting and setting the temperature of a constant-temperature water bath tank to be 303.15K, sequentially closing a valve F6, a valve F1 and a vacuum pump, opening a high-pressure helium bottle and a pressure reducing valve JF1 after the water temperature in the water bath tank reaches a set temperature of 303.15K, slowly filling helium with about 3MPa into a reference tank, closing the high-pressure helium bottle, the pressure reducing valve JF1 and the valve F5, recording the reading of a high-precision pressure gauge, then slowly opening the valve F6 to enable gas to enter a coal sample tank, recording the reading of the high-precision pressure gauge again after the reading of the high-precision pressure gauge is stable, and calculating the free volume of the coal sample tank;
(d) opening a valve F2 and a valve F5 to discharge helium in the system, closing the valve F2 and the valve F6, opening a valve F1 and a valve F4, starting a vacuum pump, and vacuumizing the glass vacuum dish for not less than 0.5 h;
(e) closing the valve F4 and opening the valve F6, vacuumizing the coal sample tank, reducing the pressure value of the vacuum gauge to be below 4Pa and ensuring that the vacuumizing time is not less than 6 h;
(f) closing the valve F1 and the vacuum pump in sequence, opening the valve F4, observing the relative humidity of the glass vacuum vessel through a digital display humidity sensor, and ensuring that the time for the coal sample in the coal sample tank to absorb the water is not less than 7 days;
(g) closing a valve F4 and a valve F6, opening a high-pressure methane gas cylinder and a pressure reducing valve JF2, closing the valve F5 after methane gas with certain pressure enters a reference tank, and recording the reading of a high-precision pressure gauge;
(h) slowly opening a valve F6 to enable methane gas to be adsorbed in the pre-adsorbed moisture coal sample, recording the reading of the high-precision pressure gauge when the adsorption is balanced for 12 hours and the reading of the high-precision pressure gauge is basically unchanged, and further calculating the methane gas adsorption capacity under the adsorption balance pressure;
(i) the rotary pressure reducing valve JF2 increases the gas pressure step by step, and the steps (g) and (h) are repeated in sequence, so that gas with higher pressure is injected into the coal sample tank, the saturated adsorption capacity of methane gas under different adsorption equilibrium pressures is obtained, and a gas adsorption isotherm can be drawn for experimental analysis;
(j) after the adsorption test is finished, closing a valve F3, opening a valve F7, closing a valve F7 after a certain amount of methane gas is released, measuring the volume of the released methane gas by using a desorption measuring cylinder and a conical flask, simultaneously ensuring that the time for re-adsorption balance of the coal sample in the coal sample tank is not less than 12 hours, and obtaining the gas pressure of the coal sample tank after adsorption balance through a high-precision pressure gauge;
(k) and (j) repeating the step (j), gradually releasing the methane gas in the coal sample tank to obtain the methane gas desorption amount under different adsorption equilibrium pressures, and drawing a gas desorption isotherm and carrying out test analysis.
Compared with the prior art, the invention has the beneficial effects that: the invention comprises a vacuum-pumping system, an inflation system, a constant temperature system, a water adsorption system and a gas adsorption and desorption test system, and has a simple integral structure. The invention uses the wet environment formed by saturated salt solution to carry out water adsorption treatment on the coal sample under the vacuum condition in advance, and then carries out the test of gas adsorption and desorption characteristics on the coal sample, particularly can realize the test of gas adsorption and desorption characteristics of low-rank coal with the characteristic of high internal moisture content, such as brown coal, long-flame coal and the like, fully simulates the gas adsorption and desorption characteristics of an on-site in-situ coal reservoir, can reflect the evolution rule of the gas adsorption and desorption characteristics of the coal under the influence of the internal moisture of the coal body, enables the gas adsorption and desorption kinetic process of the coal body of the in-situ coal reservoir to be studied more deeply, fills the blank of a domestic research device for the gas adsorption and desorption characteristics of the coal body under the influence of the internal moisture, and has the advantages of simple structure, simple and convenient test method, good use.
Drawings
FIG. 1 is a schematic structural view of the present invention;
in the figure: 1-a vacuum pump; 2-vacuum gauge pipe; 3-a vacuum gauge; 4-a high-pressure helium tank; 5-high pressure methane cylinder; 6-glass vacuum vessel; 7-digital display humidity sensor; 8-constant temperature water bath box; 9-reference tank; 10-a coal sample tank; 11-desorption measuring cylinder; 12-high precision pressure gauge; 13-Erlenmeyer flask.
Detailed Description
The present invention is described in further detail below with reference to the attached drawing figures.
As shown in fig. 1, the apparatus of the present invention mainly comprises a vacuum pumping system, an inflation system, a constant temperature system, a water adsorption system and a gas adsorption/desorption testing system, wherein: the vacuum pumping system comprises a vacuum pump 1, a vacuum gauge pipe 2 and a vacuum gauge 3 which are connected with the vacuum pump, and a valve F1 and a valve F2 which are connected with a pumping and exhausting pipeline; the inflation system comprises a high-pressure helium tank 4, a high-pressure methane tank 5, a pressure reducing valve JF1 connected with the high-pressure helium tank 4 and a pressure reducing valve JF2 connected with the high-pressure methane tank 5; the water adsorption system comprises a glass vacuum vessel 6, a digital display humidity sensor 7 arranged on the glass vacuum vessel 6 and a valve F4 connected with the glass vacuum vessel 6; the constant temperature system comprises a constant temperature water bath box 8, and in the embodiment, the constant temperature system further comprises a constant temperature element for controlling the temperature of the water bath, and the constant temperature system is used for setting the test simulation temperature; the gas adsorption and desorption testing system comprises a reference tank 9, a coal sample tank 10, a desorption measuring cylinder 11, a high-precision pressure gauge 12 arranged on a connecting pipeline of the reference tank 9 and the coal sample tank 10, a valve F5 and a valve F3 connected with the reference tank 9, a valve F6 arranged on a connecting pipeline of the coal sample tank 10 and the high-precision pressure gauge 12, a valve F7 arranged on a connecting pipeline of the coal sample tank 10 and the desorption measuring cylinder 11 and a conical flask 13 connected with the desorption measuring cylinder.
The testing method of the gas adsorption and desorption characteristic testing device comprises the following steps:
(a) mixing distilled water with the temperature of 60 ℃ and a certain amount of inorganic salt particles to prepare a saturated solution under the condition of 60 ℃, then pouring the saturated solution of the inorganic salt into a glass vacuum vessel (6) and recovering the solution to the room temperature, then sealing the glass vacuum vessel (6) to form a wet environment with the relative humidity reaching the corresponding humidity of the saturated solution of the inorganic salt, simultaneously filling a dry coal sample with the weight of about 50g and the particle size of 0.2-0.25mm into a coal sample tank (10), screwing and sealing;
(b) closing a valve F1, a valve F2, a valve F4 and a valve F7, opening a valve F3, a valve F5 and a valve F6, opening a high-pressure helium bottle (4) and a pressure reducing valve JF1 to fill helium with the pressure of 5-7 MPa, observing a high-precision pressure gauge (12) to check the air tightness of the system, closing the high-pressure helium bottle (4) and the pressure reducing valve JF1 and opening a valve F2 to completely discharge the helium in the system after the air tightness is checked, then closing the valve F2 and opening a valve F1, and starting a vacuum pump (1) until the pressure value of a vacuum gauge (3) is reduced to be below 4 Pa;
(c) starting and setting the temperature of a constant-temperature water bath box (8) to be 303.15K, sequentially closing a valve F6, a valve F1 and a vacuum pump (1), opening a high-pressure helium bottle (4) and a pressure reducing valve JF1 after the water temperature in the water bath box reaches a set temperature of 303.15K, slowly filling helium with about 3MPa into a reference tank (9), closing the high-pressure helium bottle (4), the pressure reducing valve JF1 and the valve F5, recording the reading of a high-precision pressure gauge (12), then slowly opening the valve F6, enabling gas to enter a coal sample tank (10), recording the reading of the high-precision pressure gauge (12) again after the reading of the high-precision pressure gauge (12) is stable, and calculating the free volume of the coal sample tank (10);
(d) after opening a valve F2 and a valve F5 to discharge helium in the system, closing a valve F2 and a valve F6, opening a valve F1 and a valve F4 and starting a vacuum pump (1), and vacuumizing a glass vacuum dish (6) for not less than 0.5 h;
(e) closing the valve F4 and opening the valve F6, vacuumizing the coal sample tank (10) to reduce the pressure value of the vacuum gauge (3) to be below 4Pa and ensure that the vacuumizing time is not less than 6 h;
(f) closing the valve F1 and the vacuum pump (1) in sequence, opening the valve F4, observing the relative humidity of the glass vacuum dish (6) through the digital display humidity sensor (7), and ensuring that the time for the coal sample in the coal sample tank (10) to adsorb the water is not less than 7 days;
(g) closing a valve F4 and a valve F6, opening a high-pressure methane gas cylinder (5) and a pressure reducing valve JF2, closing the valve F5 after methane gas with certain pressure enters a reference tank (9), and recording the reading of a high-precision pressure gauge (12);
(h) slowly opening a valve F6 to enable methane gas to be adsorbed in the pre-adsorbed moisture coal sample, recording the reading of the high-precision pressure gauge (12) at the moment after adsorption balance is carried out for 12 hours and when the reading of the high-precision pressure gauge (12) is basically unchanged, and further calculating the methane gas adsorption capacity under the adsorption balance pressure;
(i) the rotary pressure reducing valve JF2 increases the gas pressure step by step, and the steps (g) and (h) are repeated in sequence, so that gas with higher pressure is injected into the coal sample tank (10), the saturated adsorption capacity of methane gas under different adsorption equilibrium pressures is obtained, and a gas adsorption isotherm can be drawn for experimental analysis;
(j) after the adsorption test is finished, closing a valve F3, opening a valve F7, closing a valve F7 after a certain amount of methane gas is released, measuring the volume of the released methane gas by using a desorption measuring cylinder (11) and a conical flask (13), simultaneously ensuring that the time for re-adsorption balance of the coal sample in the coal sample tank (10) is not less than 12h, and obtaining the gas pressure after adsorption balance of the coal sample tank (10) by using a high-precision pressure gauge (12);
(k) and (j) repeating the step (j), gradually releasing the methane gas in the coal sample tank (10), obtaining the methane gas desorption amount under different adsorption equilibrium pressures, and drawing a gas desorption isotherm and carrying out experimental analysis.
The test method is illustrated below by means of specific examples.
Examples
Different inorganic salt saturated solutions can form wet environments with different relative humidity, so that coal samples with different internal moisture contents can be prepared to saturate K2SO4The test method of the present invention is illustrated by the following solutions:
(a) mixing distilled water at 60 deg.C with a certain amount of K2SO4Mixing the granules, preparing saturated solution at 60 deg.C, and mixing with K2SO4Pouring the saturated solution into a glass vacuum vessel 6, returning the solution to room temperature, sealing the glass vacuum vessel 6 to form a wet environment with relative humidity of 96%, simultaneously filling a dry coal sample with weight of about 50g and particle size of 0.2-0.25mm into a coal sample tank 10, screwing and sealing;
(b) closing a valve F1, a valve F2, a valve F4 and a valve F7, opening a valve F3, a valve F5 and a valve F6, opening a high-pressure helium bottle 4 and a pressure reducing valve JF1 to fill helium with the pressure of 5-7 MPa, observing a high-precision pressure gauge 12 to check the air tightness of the system, closing the high-pressure helium bottle 4 and the pressure reducing valve JF1 and opening a valve F2 after the air tightness check is finished, completely discharging the helium in the system, then closing the valve F2 and opening a valve F1, and starting the vacuum pump 1 until the pressure value of the vacuum gauge 3 is reduced to be lower than 4 Pa;
(c) starting and setting the temperature of a constant-temperature water bath box 8 to be 303.15K, sequentially closing a valve F6, a valve F1 and a vacuum pump 1, opening a high-pressure helium bottle 4 and a pressure reducing valve JF1 after the water temperature in the water bath box reaches a set temperature of 303.15K, slowly filling helium with about 3MPa into a reference tank 9, closing the high-pressure helium bottle 4, the pressure reducing valve JF1 and the valve F5, recording the reading of a high-precision pressure gauge 12, then slowly opening the valve F6 to enable gas to enter a coal sample tank 10, recording the reading of the high-precision pressure gauge 12 again after the reading is stable, and calculating the free volume of the coal sample tank 10;
(d) after opening a valve F2 and a valve F5 to discharge helium in the system, closing a valve F2 and a valve F6, opening a valve F1 and a valve F4 and starting a vacuum pump 1, and vacuumizing the glass vacuum dish 6 for not less than 0.5 h;
(e) closing the valve F4 and opening the valve F6, vacuumizing the coal sample tank 10 to reduce the pressure value of the vacuum gauge 3 to below 4Pa and ensure that the vacuumizing time is not less than 6 h;
(f) closing the valve F1 and the vacuum pump 1 in sequence, opening the valve F4, observing the relative humidity of the glass vacuum vessel 6 through the digital display humidity sensor 7, and ensuring that the time for the coal sample in the coal sample tank 10 to absorb the water is not less than 7 days;
(g) closing the valve F4 and the valve F6, opening the high-pressure methane gas cylinder 5 and the pressure reducing valve JF2, enabling methane gas with certain pressure to enter the reference tank 9, closing the valve F5, and recording the reading of the high-precision pressure gauge 12;
(h) slowly opening a valve F6 to enable methane gas to be adsorbed in the pre-adsorbed moisture coal sample, recording the reading of the high-precision pressure gauge 12 at the moment after adsorption balance is carried out for 12 hours and when the reading of the high-precision pressure gauge 12 is basically unchanged, and further calculating the methane gas adsorption capacity under the adsorption balance pressure;
(i) the rotary pressure reducing valve JF2 increases the gas pressure step by step, and the steps g and h are repeated in sequence, so that gas with higher pressure is injected into the coal sample tank 10, the saturated adsorption capacity of methane gas under different adsorption equilibrium pressures is obtained, and a gas adsorption isotherm can be drawn and experimental analysis can be carried out;
(j) after the adsorption test is finished, closing a valve F3, opening a valve F7, closing a valve F7 after a certain amount of methane gas is released, measuring the volume of the released methane gas by using a desorption measuring cylinder 11 and a conical flask 13, simultaneously ensuring that the time for re-adsorption balance of the coal sample in the coal sample tank 10 is not less than 12h, and obtaining the gas pressure of the coal sample tank 10 after adsorption balance through a high-precision pressure gauge 12;
(k) and repeating the step j, gradually releasing the methane gas in the coal sample tank 10 to obtain the methane gas desorption amount under different adsorption equilibrium pressures, and drawing a gas desorption isotherm and carrying out test analysis.
The water adsorption system can change the inherent water content of the coal sample, so that the gas adsorption and desorption characteristics of the coal sample under different inherent water content conditions and the influence rule of the inherent water content can be researched, the evolution rule of the gas adsorption and desorption performance of an in-situ coal reservoir, particularly low-rank coal with high inherent water content characteristics, can be better reflected, the effective prevention and the control of coal bed gas disasters are facilitated, the reliable evaluation of coal bed gas (gas) resources is facilitated, and the device has a simple structure, simple and convenient test steps and good use effect.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (1)
1. A testing method of a gas adsorption and desorption characteristic testing device for pre-adsorbing a moisture coal sample is characterized by comprising the following steps: the method is completed by means of a gas adsorption and desorption characteristic testing device, wherein the gas adsorption and desorption characteristic testing device comprises a vacuum pumping system, an inflation system, a constant temperature system, a water adsorption system and a gas adsorption and desorption testing system;
the vacuum pumping system comprises a vacuum pump (1), a vacuum gauge pipe (2) and a vacuum gauge (3) which are connected with the vacuum pump, and a valve F1 and a valve F2 which are connected with a pumping and exhausting pipeline;
the inflation system comprises a high-pressure helium tank (4), a high-pressure methane tank (5), a pressure reducing valve JF1 connected with the high-pressure helium tank (4) and a pressure reducing valve JF2 connected with the high-pressure methane tank (5);
the water adsorption system comprises a glass vacuum vessel (6), a digital display humidity sensor (7) arranged on the glass vacuum vessel (6) and a valve F4 connected with the glass vacuum vessel (6);
the constant temperature system comprises a constant temperature water bath box (8);
the gas adsorption and desorption testing system comprises two reference tanks (9) and a coal sample tank (10) which have the same volume;
the gas adsorption and desorption testing system also comprises a desorption measuring cylinder (11), a high-precision pressure gauge (12) arranged on a connecting pipeline of the reference tank (9) and the coal sample tank (10), a valve F5 and a valve F3 which are connected with the reference tank (9), a valve F6 arranged on a connecting pipeline of the coal sample tank (10) and the high-precision pressure gauge (12), a valve F7 arranged on a connecting pipeline of the coal sample tank (10) and the desorption measuring cylinder (11) and a conical flask (13) connected with the desorption measuring cylinder;
the pipeline with the pressure reducing valve JF1 and the pressure reducing valve JF2 is communicated with a pipeline with a valve F4 in the water adsorption system after being converged, and the pumping and draining pipeline is communicated with a pipeline with a high-precision pressure gauge (12);
the method for testing by adopting the gas adsorption and desorption characteristic testing device for the pre-adsorbed moisture coal sample comprises the following steps:
(a) mixing distilled water with the temperature of 60 ℃ and a certain amount of inorganic salt particles to prepare a saturated solution under the condition of 60 ℃, then pouring the saturated solution of the inorganic salt into a glass vacuum vessel (6) and recovering the solution to the room temperature, then sealing the glass vacuum vessel (6) to form a wet environment with the relative humidity reaching the corresponding humidity of the saturated solution of the inorganic salt, simultaneously filling a dry coal sample with the weight of 50g and the particle size of 0.2-0.25mm into a coal sample tank (10), screwing and sealing;
(b) closing a valve F1, a valve F2, a valve F4 and a valve F7, opening a valve F3, a valve F5 and a valve F6, opening a high-pressure helium bottle (4) and a pressure reducing valve JF1 to fill helium with the pressure of 5-7 MPa, observing a high-precision pressure gauge (12) to check the air tightness of the system, closing the high-pressure helium bottle (4) and the pressure reducing valve JF1 and opening a valve F2 to completely discharge the helium in the system after the air tightness is checked, then closing the valve F2 and opening a valve F1, and starting a vacuum pump (1) until the pressure value of a vacuum gauge (3) is reduced to be below 4 Pa;
(c) starting and setting the temperature of a constant-temperature water bath box (8) to be 303.15K, sequentially closing a valve F6, a valve F1 and a vacuum pump (1), opening a high-pressure helium bottle (4) and a pressure reducing valve JF1 after the water temperature in the water bath box reaches a set temperature of 303.15K, slowly filling helium with about 3MPa into a reference tank (9), closing the high-pressure helium bottle (4), the pressure reducing valve JF1 and the valve F5, recording the reading of a high-precision pressure gauge (12), then slowly opening the valve F6, enabling gas to enter a coal sample tank (10), recording the reading of the high-precision pressure gauge (12) again after the reading of the high-precision pressure gauge (12) is stable, and calculating the free volume of the coal sample tank (10);
(d) after opening a valve F2 and a valve F5 to discharge helium in the system, closing a valve F2 and a valve F6, opening a valve F1 and a valve F4 and starting a vacuum pump (1), and vacuumizing a glass vacuum dish (6) for not less than 0.5 h;
(e) closing the valve F4 and opening the valve F6, vacuumizing the coal sample tank (10) to reduce the pressure value of the vacuum gauge (3) to be below 4Pa and ensure that the vacuumizing time is not less than 6 h;
(f) closing the valve F1 and the vacuum pump (1) in sequence, opening the valve F4, observing the relative humidity of the glass vacuum dish (6) through the digital display humidity sensor (7), and ensuring that the time for the coal sample in the coal sample tank (10) to adsorb the water is not less than 7 days;
(g) closing a valve F4 and a valve F6, opening a high-pressure methane gas cylinder (5) and a pressure reducing valve JF2, closing the valve F5 after methane gas with certain pressure enters a reference tank (9), and recording the reading of a high-precision pressure gauge (12);
(h) slowly opening a valve F6 to enable methane gas to be adsorbed in the pre-adsorbed moisture coal sample, recording the reading of the high-precision pressure gauge (12) at the moment after adsorption balance is carried out for 12 hours and when the reading of the high-precision pressure gauge (12) is basically unchanged, and further calculating the methane gas adsorption capacity under the adsorption balance pressure;
(i) the rotary pressure reducing valve JF2 increases the gas pressure step by step, and the steps (g) and (h) are repeated in sequence, so that gas with higher pressure is injected into the coal sample tank (10), the saturated adsorption capacity of methane gas under different adsorption equilibrium pressures is obtained, and a gas adsorption isotherm can be drawn for experimental analysis;
(j) after the adsorption test is finished, closing a valve F3, opening a valve F7, closing a valve F7 after a certain amount of methane gas is released, measuring the volume of the released methane gas by using a desorption measuring cylinder (11) and a conical flask (13), simultaneously ensuring that the time for re-adsorption balance of the coal sample in the coal sample tank (10) is not less than 12h, and obtaining the gas pressure after adsorption balance of the coal sample tank (10) by using a high-precision pressure gauge (12);
(k) and (j) repeating the step (j), gradually releasing the methane gas in the coal sample tank (10), obtaining the methane gas desorption amount under different adsorption equilibrium pressures, and drawing a gas desorption isotherm and carrying out experimental analysis.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711091105.2A CN107860681B (en) | 2017-11-08 | 2017-11-08 | Gas adsorption and desorption characteristic testing device and method for pre-adsorbing moisture coal sample |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711091105.2A CN107860681B (en) | 2017-11-08 | 2017-11-08 | Gas adsorption and desorption characteristic testing device and method for pre-adsorbing moisture coal sample |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107860681A CN107860681A (en) | 2018-03-30 |
| CN107860681B true CN107860681B (en) | 2020-08-21 |
Family
ID=61701224
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711091105.2A Expired - Fee Related CN107860681B (en) | 2017-11-08 | 2017-11-08 | Gas adsorption and desorption characteristic testing device and method for pre-adsorbing moisture coal sample |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107860681B (en) |
Families Citing this family (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109470834A (en) * | 2018-11-05 | 2019-03-15 | 石家庄铁道大学 | Coal petrography adsorption-desorption deformation Visualizing Test System and test method under water and gas collective effect |
| CN109540734B (en) * | 2019-01-09 | 2023-11-24 | 重庆工业职业技术学院 | Gas-containing coal high-pressure adsorption/desorption test device and method capable of controlling moisture |
| CN109632569A (en) * | 2019-01-24 | 2019-04-16 | 中煤科工集团重庆研究院有限公司 | The measuring method and device of a kind of adscititious gases and moisture to coal containing methane gas grain desorption effects |
| CN109696380B (en) * | 2019-03-04 | 2021-04-16 | 大连理工大学 | Method and device for evaluating gas separation performance of microporous material |
| CN109946215B (en) * | 2019-04-22 | 2024-05-24 | 洛阳理工学院 | In-situ coal gas adsorption capacity test simulation device |
| CN111829917A (en) * | 2019-04-22 | 2020-10-27 | 河南理工大学 | Coal body adsorption desorption deformation anisotropy synchronous testing device and method |
| CN110711548B (en) * | 2019-09-25 | 2021-05-28 | 太原理工大学 | Device and method for converting methane in supercritical water |
| CN110849767B (en) * | 2019-11-11 | 2022-02-22 | 太原理工大学 | Device and method for measuring gas desorption capacity of solution in coal body |
| CN110865005B (en) * | 2019-11-11 | 2022-02-01 | 太原理工大学 | Device and method for measuring liquid absorption rate of coal and rock mass under different stirring rates |
| CN111521516A (en) * | 2019-12-11 | 2020-08-11 | 南通市飞宇石油科技开发有限公司 | Coal body gas adsorption and strain test system |
| CN111624132A (en) * | 2020-06-09 | 2020-09-04 | 中煤科工集团重庆研究院有限公司 | Coal gas desorption constant pressure measuring device |
| CN111855536B (en) * | 2020-08-18 | 2022-02-08 | 西南石油大学 | Method for measuring adsorption of liquid hydrocarbon in reservoir porous medium under high temperature and high pressure |
| CN112432879B (en) * | 2020-09-18 | 2023-08-18 | 郑州大学 | Gas adsorption-desorption-recovery test device and test method for coal body |
| CN113640174A (en) * | 2021-06-30 | 2021-11-12 | 中煤科工集团沈阳研究院有限公司 | Coal gas adsorption desorption heating oxidation coupling experiment platform and experiment method thereof |
| CN113702261B (en) * | 2021-08-25 | 2023-11-03 | 山东科技大学 | Test analysis method for correcting porosity and deformation of gas-containing coal |
| CN113834753A (en) * | 2021-09-18 | 2021-12-24 | 华北科技学院(中国煤矿安全技术培训中心) | Isothermal adsorption-desorption system under coal sample vibration condition |
| CN114324057A (en) * | 2021-12-13 | 2022-04-12 | 西安科技大学 | Experiment system and method for monitoring liquid nitrogen temperature control coal gas adsorption and desorption in real time |
| CN114383978B (en) * | 2021-12-30 | 2024-01-26 | 安徽理工大学 | CO 2 Device and method for testing contact angle of coal-rock component of water-coal system |
| CN114964951A (en) * | 2022-04-25 | 2022-08-30 | 中国矿业大学(北京) | Method capable of uniformly wetting coal sample |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0627016A (en) * | 1992-07-07 | 1994-02-04 | Ishikawajima Harima Heavy Ind Co Ltd | Water permeation and absorption tester for radiation shield |
| CN102901803A (en) * | 2012-10-24 | 2013-01-30 | 河南理工大学 | Water-gas two-phase adsorption-desorption-seepage experimental system and method for loaded coal containing methane |
| CN105424544A (en) * | 2015-11-04 | 2016-03-23 | 安徽理工大学 | Device and method for measuring coal mass deformation through simultaneous adsorption and induction of gas and water |
| CN105738248A (en) * | 2016-03-02 | 2016-07-06 | 重庆大学 | Gas absorption and desorption experimental device with controllable coal sample moisture content and experimental method thereof |
| CN205593876U (en) * | 2016-05-09 | 2016-09-21 | 华北科技学院 | Coal column gas adsorbs many parameter testing of desorption system |
| CN106018734A (en) * | 2016-07-29 | 2016-10-12 | 河南理工大学 | Determination method for reasonable immersion time of coal seam water infusion |
-
2017
- 2017-11-08 CN CN201711091105.2A patent/CN107860681B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0627016A (en) * | 1992-07-07 | 1994-02-04 | Ishikawajima Harima Heavy Ind Co Ltd | Water permeation and absorption tester for radiation shield |
| CN102901803A (en) * | 2012-10-24 | 2013-01-30 | 河南理工大学 | Water-gas two-phase adsorption-desorption-seepage experimental system and method for loaded coal containing methane |
| CN105424544A (en) * | 2015-11-04 | 2016-03-23 | 安徽理工大学 | Device and method for measuring coal mass deformation through simultaneous adsorption and induction of gas and water |
| CN105738248A (en) * | 2016-03-02 | 2016-07-06 | 重庆大学 | Gas absorption and desorption experimental device with controllable coal sample moisture content and experimental method thereof |
| CN205593876U (en) * | 2016-05-09 | 2016-09-21 | 华北科技学院 | Coal column gas adsorbs many parameter testing of desorption system |
| CN106018734A (en) * | 2016-07-29 | 2016-10-12 | 河南理工大学 | Determination method for reasonable immersion time of coal seam water infusion |
Non-Patent Citations (1)
| Title |
|---|
| 水分对煤瓦斯解吸性能及力学特性的影响研究;何涛;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20160215;全文 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107860681A (en) | 2018-03-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107860681B (en) | Gas adsorption and desorption characteristic testing device and method for pre-adsorbing moisture coal sample | |
| CN102053141B (en) | Method for testing desorption characteristic of externally added water on gas-containing coal body | |
| CN103776979B (en) | A kind of coal seam water infusion suppresses analog detection method and the device of desorption of mash gas effect | |
| CN103132971B (en) | Carbon dioxide injection improves the test simulator of coal bed methane recovery rate | |
| CN109540734B (en) | Gas-containing coal high-pressure adsorption/desorption test device and method capable of controlling moisture | |
| CN106970000A (en) | Coal/shale extra-high absorption and Seepage Experiment evaluate shale gas adsorption method | |
| CN105738248A (en) | Gas absorption and desorption experimental device with controllable coal sample moisture content and experimental method thereof | |
| CN105547908A (en) | Experimental testing equipment for mixed gas adsorption capacity of coal rock/shale | |
| CN107192630A (en) | A kind of water filling is to desorption of mash gas characteristic experimental apparatus | |
| CN108303509B (en) | Device and method for correcting free amount calculation of coal bed gas and measuring residual adsorption amount | |
| CN204101416U (en) | Geotechnique's original position dicyclo infiltration experiment device | |
| CN102706779B (en) | Method for measuring diffusion coefficient of carbon dioxide in rock | |
| CN204666464U (en) | The experimental provision of coal-seam gas level pressure desorb | |
| CN207351844U (en) | The controllable gas adsorption desorption experimental apparatus of coal sample moisture | |
| CN109870397A (en) | Isothermal adsorption deformation testing device and test method under the conditions of a kind of mixed gas | |
| CN104655806B (en) | A kind of nitrogen fracturing coal seam energy variation and permeability method of testing and device | |
| CN109946215A (en) | A kind of original position coal body gas absorption amount test simulator | |
| CN108732329B (en) | Coal seam gas pressure measurement simulation experiment device and method | |
| CN108195740A (en) | Carbon dioxide displacement methane device under the conditions of coal-bed flooding | |
| CN107014714B (en) | Be applicable to coal body adsorption desorption deformation test device under high temperature and high pressure | |
| CN109470834A (en) | Coal petrography adsorption-desorption deformation Visualizing Test System and test method under water and gas collective effect | |
| CN106769507B (en) | Seal simulation experiment method up for safekeeping in multi- scenarios method condition carbon dioxide coal seam | |
| CN115656440A (en) | Deep brine layer carbon dioxide sequestration simulation device | |
| CN111323359B (en) | Core spontaneous imbibition measuring device and method for high-pressure natural gas-water system | |
| CN112630121B (en) | Device and method for testing permeability of fractured surrounding rock of deep chamber under stress action |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20200821 Termination date: 20211108 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |