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In This Article

  • Summary
  • Abstract
  • Introduction
  • Protocol
  • Results
  • Discussion
  • Disclosures
  • Acknowledgements
  • Materials
  • References
  • Reprints and Permissions

Summary

This protocol demonstrates how to prepare a briquette sample and conduct a uniaxial compression experiment with a briquette in different CO2 pressures using a visualized and constant-volume gas-solid coupling test system. It also aims to investigate changes in terms of coal’s physical and mechanical properties induced by CO2 adsorption.

Abstract

Injecting carbon dioxide (CO2) into a deep coal seam is of great significance for reducing the concentration of greenhouse gases in the atmosphere and increasing the recovery of coalbed methane. A visualized and constant-volume gas-solid coupling system is introduced here to investigate the influence of CO2 sorption on the physical and mechanical properties of coal. Being able to keep a constant volume and monitor the sample using a camera, this system offers the potential to improve instrument accuracy and analyze fracture evolution with a fractal geometry method. This paper provides all steps to perform a uniaxial compression experiment with a briquette sample in different CO2 pressures with the gas-solid coupling test system. A briquette, cold-pressed by raw coal and sodium humate cement, is loaded in high-pressure CO2, and its surface is monitored in real-time using a camera. However, the similarity between the briquette and the raw coal still needs improvement, and a flammable gas such as methane (CH4) cannot be injected for the test. The results show that CO2 sorption leads to peak strength and elastic modulus reduction of the briquette, and the fracture evolution of the briquette in a failure state indicates fractal characteristics. The strength, elastic modulus, and fractal dimension are all correlated with CO2 pressure but not with a linear correlation. The visualized and constant-volume gas-solid coupling test system can serve as a platform for experimental research about rock mechanics considering the multifield coupling effect.

Introduction

The increasing concentration of CO2 in the atmosphere is a direct factor causing the global warming effect. Due to the strong sorption capacity of coal, CO2 sequestration in a coal seam is regarded as a practical and environment-friendly means to reduce the global emission of greenhouse gas1,2,3. At the same time, the injected CO2 can replace CH4 and result in gas production promotion in coalbed methane recovery (ECBM)4,5,6. The ecological and economic prospects of CO2 sequestration have recently attracted worldwide attention among researchers, as well as among different international environmental protection groups and governmental agencies.

Coal is a heterogeneous, structurally anisotropic rock composed of a pore, fracture, and coal matrix. The pore structure has a large specific surface area, which can adsorb a large amount of gas, playing a vital role in gas sequestration, and the fracture is the main path for free gas flow7,8. This unique physical structure leads to a great gas adsorption capacity for CH4 and CO2. Mine gas is deposited in coalbed in a few forms: (1) adsorbed on the surface of micropores and larger pores; (2) absorbed in the coal molecular structure; (3) as free gas in fractures and larger pores; and (4) dissolved in deposit water. The sorption behavior of coal to CH4 and CO2 causes matrix swelling, and further studies demonstrate that it is a heterogeneous process and is related to the coal lithotypes9,10,11. In addition, gas sorption can result in damage in the constitutive relation of coal12,13,14.

The raw coal sample is generally used in coal and CO2 coupling experiments. Specifically, a large piece of raw coal from the working face in a coal mine is cut to prepare a sample. However, the physical and mechanical properties of raw coal inevitably have a high dispersion degree due to the random spatial distribution of natural pores and fractures in a coal seam. Moreover, the gas-bearing coal is soft and difficult to be reshaped. According to the principles of the orthogonal experimental method, the briquette, which is reconstituted with raw coal powder and cement, is regarded as an ideal material used in the coal sorption test15,16. Being cold-pressed with metal dies, its strength can be preset and remains stable by adjusting the quantity of cement, which benefits the comparative analysis of the single-variable effect. Additionally, although the porosity of the briquette sample is ~4-10 times, that of the raw coal sample, similar adsorption and desorption characteristics and stress-strain curve have been found in the experimental research17,18,19,20. In this paper, a scheme of a similar material for gas-bearing coal has been adopted to prepare the briquette21. The raw coal was taken from the 4671B6 working face in the Xinzhuangzi Coal Mine, Huainan, Anhui Province, China. The coal seam is approximately 450 m below ground level and 360 m below sea level, and it dips at about 15° and is approximately 1.6 m in thickness. The height and diameter of the briquette sample are 100 mm and 50 mm, respectively, which is the recommended size suggested by the International Society for Rock Mechanics (ISRM)22.

The previous uniaxial or triaxial loading test instruments for gas-bearing coal experiments under laboratory conditions have some shortages and limitations, presented as fellows23,24,25,26,27,28: (1) during the loading process, the vessel volume decreases with the piston moving, causing fluctuations in gas pressure and disturbances in gas sorption; (2) the real-time image monitoring of samples, as well as circumferential deformation measurements in a high gas pressure environment, is difficult to conduct; (3) they are limited to stimulation of dynamic load disturbances on preloaded samples to analyze their mechanical response characteristics. In order to improve the instrument precision and data acquisition in the gas-solid coupling condition, a visualized and constant-volume test system29 has been developed (Figure 1), including (1) a visualized loading vessel with a constant volume chamber, which is the core component; (2) a gas filling module with a vacuum channel, two filling channels, and a releasing channel; (3) an axial loading module consisting of an electro-hydraulic servo universal testing machine and control computer; (4) a data acquisition module comprised of a circumferential displacement measurement apparatus, a gas pressure sensor, and a camera at the window of the visualized loading vessel.

The core visualized vessel (Figure 2) is specifically designed so that two adjusting cylinders are fixed on the upper plate and their pistons move simultaneously with the loading one through a beam, and the sectional area of the loading piston is equal to the sum of that of the adjusting cylinders. Flowing through an inner hole and soft pipes, the high-pressure gas in the vessel and the two cylinders is connected. Therefore, when the vessel-loading piston moves downward and compresses the gas, this structure can offset the change in volume and eliminate pressure interference. In addition, the enormous gas-induced counterforce exerting on the piston is prevented during the test, significantly improving the safety of the instrument. The windows, which are equipped with tempered borosilicate glass and situated on three sides of the vessel, provide a direct way to take a photograph of the sample. This glass has been successfully tested and proved to resist up to 10 MPa gas with a low expansion rate, high strength, light transmittance, and chemical stability29.

This paper describes the procedure to perform a uniaxial compression experiment of CO2-bearing coal with the new visualized and constant-volume gas-solid coupling test system, which includes the description of all pieces that prepare a briquette sample using raw coal powder and sodium humate, as well as the successive steps to inject high-pressure CO2 and conduct uniaxial compression. The whole sample deformation process is monitored using a camera. This experimental approach offers an alternative way to quantitively analyze the adsorption-induced damage and fracture evolution characteristic of gas-bearing coal.

Protocol

1. Sample preparation

  1. Collect raw coal blocks from the 4671B6 working face from the Xinzhuangzi coal mine. Note that, due to the low strength and looseness of the structure, the raw coal is broken and probably mixed with impurities. To avoid the influence of these internal and external factors, as well as reduce the inhomogeneity of coal as much as possible, select large coal blocks (about 15 cm long, 10 cm wide, and 10 cm high).
  2. Use a tweezer to remove impurities mixed in the coal and scrub the crusher chamber with absorbent cotton and acetaldehyde.
  3. Smash the coal blocks into small pieces with a jaw crusher, and shelter them in a sieve shaker equipped with standard screens of 6 and 16 mesh. Place the sorted coal powder separately according to diameter.
  4. Weigh 1,000 g and 300 g of pulverized coal with a particle size distribution of 0–1 mm and 1– 3 mm, respectively. Put them together in a beaker in a mass proportion of 0.76:0.24 and mix them well with a glass rod (with a diameter of 6 mm).
    NOTE: According to the Gaudian-Schuman function of continuous packing theory, when the particle size distribution value (m) equals approximately 0.25 (mass of particle size is 1–3 mm: total mass = 0.24), the strength of the briquette is maximal30.
  5. To prepare the cement, put 4 g of sodium humate powder (99.99% purity) into a beaker and add approximately 96 mL of distilled water. Use a glass rod to stir them and make sure that all sodium humate is well dissolved.
    NOTE: The concentration of cement directly affects the compressive strength of briquette. Table 1 reveals specific ratios of briquette preparation, of which the No. 2 sample has been used for the representative results.
  6. Put 230 g of mixed coal powder and 20 g of sodium humate solution into a beaker and mix them together.
    NOTE: Based on previous experiences of making samples, a briquette produced with 250 g of material, using the cold press method, meets the size requirement of a standard rock sample22, where coal powder accounts for 92% and cement accounts for 8%.
  7. Cold-press the briquette using the shaping tools adapted to the size of the briquette (Figure 3).
    1. To produce a standard-sized briquette, coat the inner surface of the shaping tools with lubricating oil. Assemble tool components #2, #3, and #4 of Figure 3, and fill the hole with 250 g of mixed material.
    2. Put component #1 of Figure 3 on top of the material, and place everything under the piston of an electro-hydraulic servo universal testing machine.
    3. Launch the software WinWdw (or equivalent) to control the electro-hydraulic servo universal testing machine. In the software, click on Force Range to set the maximum force to 50 kN, and click on Reset to clear the displacement value.
    4. Left-click on the option force loading control. Set the moving ratio at 0.1 kN/s. Set the target force value at 29.4 kN and holding time at 900 s. Then, click on Start.
    5. Take out the shaping tools and invert them onto a rubber plate. Use a rubber hammer to disassemble tool components #4, #2, #3, and #1 in that order.
  8. Put the briquette in a 40 °C incubator for 48 h. Then, weigh its mass with electronic scales (with a precision of 0.01 g) and measure its height and diameter with a Vernier caliper (with a precision of 0.02 mm) after drying.
  9. Measure the moisture content, ash content, and volatile content of the briquette, using a proximate analyzer (see the Table of Materials) at a temperature of 20 °C and a relative humidity of 65% (per standard GB/T 212-2008). Perform a vitrinite reflectance measurement on the polished briquette, using a photometer microscope (per standard GB/T 6948-2008).
  10. Measure the uniaxial compressive strength, tensile strength, cohesion, and internal friction angle, using a universal testing machine and a strain controlled direct shear apparatus (per standard GB/T 23561-2010). Perform a Poisson ratio measurement using a resistance strain gauge (per standard GB/T 22315-2008).
  11. Conduct an adsorption test of the raw coal and the briquette, using an isotherm adsorption instrument (per standard GB/T19560-2008).

2. Experimental methods

  1. Laboratory setup
    1. Place the test system in a quiet, vibration-free area of a clean laboratory without electromagnetic interference. The room temperature should remain stable during the test.
    2. Put the visualized vessel on the platform of the electro-hydraulic servo universal testing machine. Connect the piston of the testing machine with that of the visualized vessel with the use of a specific tool (see Figure 4).
    3. Install a manual pressure-reducing valve in the gas tank nozzle. Connect the valve with the gas filling channel at the bottom plate of the visualized vessel by soft pipe (with an inner diameter of 5 mm and a maximal pressure of 30 MPa). Link the vacuum channel and the vacuum pump with the same pipe.
    4. Fix the back door of the visualized vessel with high-strength bolts. Connect the computer, data acquisition box (DAQ box), and the embedded gas pressure sensor to the back door.
  2. Air tightness test and blank measurement
    1. To acquire the gas pressure data in the visualized vessel, launch the software DAQ Sensor-16 (or equivalent). On the software, click on Start.
    2. Start the vacuum pump. Open the valve V1 (Figure 2) and close V2, V3, and V4 (Figure 2). Vacuum the visualized vessel chamber. Turn off V1 and vacuum-pump it until it is under vacuum.
    3. Open V2 and the gas tank (with helium). Use the manual pressure-reducing valve to adjust the outlet pressure of the gas tank to approximate 2 MPa (relative pressure).
    4. Carefully observe the gas pressure curve displayed on DAQ Sensor-16. When it is about 2 MPa, turn off V2 and the gas tank.
      NOTE: After 24 h, if the reduction of the gas pressure is less than 5%, the sealability of the visualized vessel is good.
    5. To measure the friction force of the loading piston moving downward, launch the software WinWdw to control the electro-hydraulic servo universal testing machine.
    6. In the software, click on Force Range to set the maximum force to 5 kN and click on Reset to clear the displacement value. Left-click on the option Displacement Loading Rate. Set the moving ratio at 1 mm/min; then, click on Start.
    7. When the displacement displayed on WinWdw is approximately 5 mm, click on Stop. Left-click on Data Save to save the force-displacement curve.
    8. Open V4 and discharge helium into air. Disassemble the back door of the visualized vessel and close V4.
      CAUTION: The door and windows should be open for ventilation during the gas release due to the possible suffocation hazard.
  3. Uniaxial compression experiment
    1. Measure the height (h) and diameter (d) of the briquette with a Vernier caliper (with a precision of 0.02 mm). Weigh the mass (m) of the briquette with electronic scales (with a precision of 0.01 g). Calculate its apparent density (figure-protocol-7964) with the following equation.
      ​figure-protocol-8077
    2. Install the chain roller of the circumferential deformation test apparatus around the middle position of the briquette (Figure 5, #1) and fix the clamp holder (Figure 5, #2). Connect the sensor (Figure 5, #3) with the DAQ box through the aviation connector in the visualized vessel (Figure 2) and place them under the loading piston.
      NOTE: To ensure the accuracy of the data acquisition, adjust the chain roller and the top surface of the sample so that they are parallel to the loading piston.
    3. Launch WinWdw to control the universal testing machine. In the software, left-click on the option Displacement Loading Rate. Set the moving ratio at 10 mm/min. Press the Down button on the remote controller of the universal testing machine until the distance left between the piston and the sample is 1–2 mm. Then, assemble the back door of the visualized vessel.
    4. Repeat steps 2.2.1–2.2.2. Open V3 and the gas tank (CO2, purity = 99.99%). Use the manual pressure-reducing valve to adjust the outlet pressure of the gas tank to a certain value.
    5. Carefully observe the gas pressure curve displayed in DAQ Sensor-16. When it gets close enough to the target value, close V3 and the gas tank (CO2).
      NOTE: When the gas pressure curve remains stable, the briquette has reached its adsorption and desorption dynamic equilibrium state. Generally, it takes 6–8 h for the briquette to fully adsorb. In this test, the adsorption time is set at 24 h.
    6. After 24 h, place the camera with a tripod beside the window of the visualized vessel. Adjust the height and angle to ensure that the image of the sample is shown in the center of the camera screen.
    7. Start the software SDU deformation acquisition V2.0 (or equivalent) to monitor the circumferential deformation of the briquette. Click on Start.
    8. On WinWdw, click on New Sample and type in the height and diameter of the briquette, click on Sectional Area, and then click on Confirm. Click on Force Range to set the maximum force to 5 kN, and click on Reset to clear the displacement value.
    9. Left-click on the option Displacement Loading Rate and set the moving ratio at 1 mm/min. Click on Start to compress the sample. At the same time, press the Start button on the camera to begin video recording.
    10. When the sample totally fails, click on Stop and Data Save, in that order, in both WinWdw and SDU deformation acquisition V2.0. Press the Start button again on the camera to stop video recording.
    11. Repeat step 2.2.8 to release CO2 in the vessel chamber. Disconnect the aviation connectors for the gas pressure sensor and circumferential deformation test apparatus.
    12. Left-click on the option Displacement Loading Rate on WinWdw. Set the moving ratio at 10 mm/min. Press the Up button on the remote controller of the universal testing machine. When the loading piston of the vessel is around 2–3 mm above the briquette, take the briquette out and remove it from the chain roller.
    13. Dismantle the connecting tool between the pistons. Clean the visualized vessel with a vacuum cleaner.
  4. Completion
    1. Based on the stress-axial strain curve and circumferential strain curve obtained from WinWdw and SDU deformation acquisition V2.0, calculate the volume strain of the sample with the following equation.
      figure-protocol-12366
      ​Here, figure-protocol-12455 = volume strain; figure-protocol-12540 = axial strain; figure-protocol-12624 = circumferential strain.
    2. Obtain the peak strength from the stress-axial strain curve. The strength reduction rate is calculated as follows.
      figure-protocol-12852
      ​Here, figure-protocol-12941 = strength reduction rate; figure-protocol-13036 = peak strength of the sample under a different pressure of CO2; figure-protocol-13180 = peak strength of the sample in atmospheric air.
    3. Calculate the elastic modulus using the linear stage in the stress-axial strain curve according to the following equation.
      figure-protocol-13442
      Here, figure-protocol-13526 = elastic modulus of the sample; figure-protocol-13629 = stress increment of linear the stage (in megapascal); figure-protocol-13755 = strain increment of the linear stage. Calculate the elastic modulus reduction rate as follows.
      figure-protocol-13930
      ​Here, figure-protocol-14021 = elastic modulus reduction rate, figure-protocol-14125 = elastic modulus of the sample under a different pressure of CO2; figure-protocol-14273 = elastic modulus of the sample in atmospheric air.
    4. Select sample photos during the test and statistics fracture covering area using a program (e.g., written in MATLAB) according to the box-counting dimension method.
      figure-protocol-14579
      ​Here, figure-protocol-14670 = grid number to cover the fracture area at the square grid side length of figure-protocol-14815; figure-protocol-14886 = a constant; figure-protocol-14970 = fractal dimension; figure-protocol-15061 = side length of the square grid. The minimum grid size equals the pixel size in this test.
      1. Calculate the correlation coefficient according to the following equation.
        figure-protocol-15321
        Here,figure-protocol-15405 = correlation coefficient; figure-protocol-15502 = covariance of figure-protocol-15588 and figure-protocol-15662; figure-protocol-15733 = variance of figure-protocol-15817; figure-protocol-15888 = variance of figure-protocol-15972.

Results

The average mass of the briquette sample was 230 g. Depending on the industrial analysis, the briquette exhibited a moisture content of 4.52% and an ash content of 15.52%. Furthermore, the volatile content was approximately 31.24%. As the sodium humate was extracted from the coal, the components of the briquette were similar to raw coal. The physical characteristics are displayed in Table 2.

The comparison of th...

Discussion

Considering the danger of high-pressure gas, some critical steps are important during the test. The valves and O rings should be inspected and replaced regularly, and any source of ignition should not be allowed in the laboratory. When using the manual pressure-regulating valve, the experimenter should twist the valve slowly to make the pressure in the visualized vessel increase gradually. Do not disassemble the vessel during the test. When the experiment is finished, the back door of the vessel should be opened after th...

Disclosures

The authors have nothing to disclose.

Acknowledgements

This work was supported by the China National Major Scientific Instruments Development Project (Grant No. 51427804) and the Shandong Province National Natural Science Foundation (Grant No. ZR2017MEE023).

Materials

NameCompanyCatalog NumberComments
3Y-Leica MPV-SP photometer microphotometric systemLeica,GermanyM090063016Used for vitrinite
reflectance measurement
Automatic isotherm adsorption instrumentBeiShiDe Instrument Technology (Beijing)CO.,Ltd.3H-2000PHIsothermal adsorption test
Electro hydraulic servo universal testing machineJinan Shidaishijin testing machine CO.,LtdWDW-100EIIIUsed to provide
axial pressure
Gas pressure sensorBeijing Star Sensor Technology CO.,LTDCYYZ11Gas pressure monitoring
Gas tank(carbon dioxide/helium)Heifei Henglong Gas.,LtdGas resource
high-speed cameraSony corporationFDR-AX30Image monitoring
IncubatorYuyao YuanDong Digital Instrument FactoryXGQ-2000Briquette drying
jaw crusherHebi Tianke Instrument CO.,LtdEP-2Coal grinding
Manual pressure reducing valveShanghai Saergen Instrument CO.,LtdR41Outlet gas pressure adjustment
Proximate AnalyzerChangsha Kaiyuan Instrument CO.,Ltd5E-MAG6700Coal industrial analysis
Resistance strain gaugeJinan Sigmar Technology CO.,LTDASMB3-16/8Poisson ratio measurement
Sieve shaker (6,16mesh)Hebi Tianguan Instrument CO.,LtdGZS-300Coal powder shelter
Soft pipeJinan Quanxing High pressure pipe CO.,LtdInner diameter=5 mm
maximal pressure=30 MPa
Standard rock sample circumferential deformation test apparatusHuainan Qingda Machinery CO.,LtdCircumferential deformation
acquisition
Strain controlled
direct shear apparatus		Beijing Aerospace Huayu Test Instrument CO.,LTDZJ-4ATensile strength, cohesion, internal friction
angle measurement
Vaccum pumpFujiwara,Japan750DUsed to vaccumize the vessel
ValveJiangsu Subei Valve Co.,LtdS4 NS-MG16-MF1Gas seal
Visual loading vesselHuainan Qingda Machinery CO.,LtdInstrument for sample
loading and real-time monitoring

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