Detecting Pore Size Distribution of Activated Carbon by Low‐Field Nuclear Magnetic Resonance

Author(s):  
Zhihong Zhao ◽  
Bin Wang ◽  
Rui Tan ◽  
Wenjing Liu ◽  
Minghui Zhang
2018 ◽  
Vol 37 (1) ◽  
pp. 412-428
Author(s):  
Feng Zhu ◽  
Wenxuan Hu ◽  
Jian Cao ◽  
Biao Liu ◽  
Yifeng Liu ◽  
...  

Nuclear magnetic resonance cryoporometry is a newly developed technique that can characterize the pore size distribution of nano-scale porous materials. To date, this technique has scarcely been used for the testing of unconventional oil and gas reservoirs; thus, their micro- and nano-scale pore structures must still be investigated. The selection of the probe material for this technique has a key impact on the quality of the measurement results during the testing of geological samples. In this paper, we present details on the nuclear magnetic resonance cryoporometric procedure. Several types of probe materials were compared during the nuclear testing of standard nano-scale porous materials and unconventional reservoir geological samples from Sichuan Basin, Southwest China. Gas sorption experiments were also carried out on the same samples simultaneously. The KGT values of the probe materials octamethylcyclotetrasiloxane and calcium chloride hexahydrate were calibrated using standard nano-scale porous materials to reveal respective values of 149.3 Knm and 184 Knm. Water did not successfully wet the pore surfaces of the standard controlled pore glass samples; moreover, water damaged the pore structures of the geological samples, which was confirmed during two freeze-melting tests. The complex phase transition during the melting of cyclohexane introduced a nuclear magnetic resonance signal in addition to that from liquid in the pores, which led to an imprecise characterization of the pore size distribution. Octamethylcyclotetrasiloxane and calcium chloride hexahydrate have been rarely employed as nuclear magnetic resonance cryoporometric probe materials for the testing of an unconventional reservoir. Both of these materials were able to characterize pore sizes up to 1 μm, and they were more applicable than either water or cyclohexane.


Cellulose ◽  
2020 ◽  
Vol 27 (8) ◽  
pp. 4235-4247 ◽  
Author(s):  
Chenyang Cai ◽  
Muhammad Asadullah Javed ◽  
Sanna Komulainen ◽  
Ville-Veikko Telkki ◽  
Antti Haapala ◽  
...  

2021 ◽  
Vol 21 (1) ◽  
pp. 515-528
Author(s):  
Baoxin Zhang ◽  
Xuehai Fu ◽  
Ze Deng ◽  
Ming Hao

A number of studies have used the nuclear magnetic resonance (NMR) technique to analyse pore characteristics and to discuss the influencing mechanisms of pore structure on methane adsorption. However, there are few studies on the dynamic characteristics of methane adsorption over time under the same temperature and pressure conditions, especially by using the cylindrical coal samples. In this study, scanning electron microscopy (SEM), mercury injection porosimetry (MIP), isothermal adsorption and NMR techniques were carried out on the four medium-high volatile bituminous coal samples from Shanxi Province, China. The simulation of methane adsorption was carried out with the custom adsorption instruments. Based on the experimental results and the Hodot pore size classification standard, the pore size distribution of the samples was analysed. In addition, the influence of nanopore structure and water content on methane adsorption was discussed. The results show that the T2 relaxation diagram of the four coal samples has a bimodal-triple peak, which reflects the complexity of the pore structure. Due to the clay minerals filling microfractures in the sample HX, the connectivity of the nanopores is reduced, in addition there is an obvious gap between the peaks in the relaxation diagram. After calculation of the T2 relaxation diagrams of the coals, the results can be converted into the pore size distribution map. The pores in the four samples are mainly composed of the macropores, followed by the mesopores, and the ratio of micropores and transition pores is relatively small. At Sw (saturated in 5% brine for 24 h) and Sir (dried at 333 K for 3 h) conditions, the adsorption capacity of the four samples presented a positive correlation with the effective porosity and the ratio of micropores, and presented a negative correlation with the ratio of mesopores, while the macropores contribute less to the adsorption. Compared with samples at Sw conditions, the adsorption capacity of the samples at Sir conditions shows an overall increasing trend, which is approximately 1.6 times that of the samples at Sw conditions on average. When a large amount of liquid water invades the nanopores and fractures, the water occupies the adsorption space of the methane due to the wettability effects and capillary pressure, which reduces the adsorption capacity.


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