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Original papers
Materials for energy and environment, next-generation photovoltaics, and green technologies УДК 66.021:66.081.32 DOI: 10.17277/jamt.2023.04.pp.270-278
Promising sorbents based on compacted highly porous carbon materials
© Igor N. Shubina^, Elina S. Mkrtchyana, Oksana A. Ananyevaa
a Tambov State Technical University, Bld. 2, 106/5, Sovetskaya St., Tambov, 392000, Russian Federation
И i.shubin77@yandex.ru
Abstract: The paper considers the stages of preparing a compacted highly porous carbon material (HPCM), which involves alkaline high-temperature activation of the initial carbonizate at a temperature of 400-7500 °C for a duration of 2 hours. As a result of activation, a material was produced with a specific surface area of 2600-2700 m2-g-1 and a pore volume of more than 1.3 cm3-g-1. The activated material was compacted using binders, which were basalt fiber (HPCM/BF), polyvinyl alcohol (HPCM/PVA) and polyvinyl acetate (HPCM/PVAC). Conditions for compacting were as follows: pressure in the range from 25 to 1600 kgf-cm-2, temperature 75-1900 °C and duration between 30 and 150 minutes. As a result, the compacted material had a specific surface area of 1550-2000 m2-g-1 and a specific pore volume of 0.693-0.849 cm3-g-1. For the final samples, the sorption capacity for molecules of the organic dye methylene blue (MB) was determined. The kinetic studies showed that the absorptive capacity of h the initial material HPCM was 1691 m-g-1, while that of compacted samples of HPCM/PVAC, HPCM/BF and HPCM/PVA was 1611, 1000, and 1270 mg-g-1, respectively. In this case, the time for the onset of adsorption equilibrium was 15 min. The presented results show that the compacted carbon material can be a promising sorbent of organic pollutants from aqueous solutions.
Keywords: highly porous carbon material; compaction; specific surface area; adsorption; methylene blue; kinetics.
For citation: Shubin IN, Mkrtchyan ES, Ananyeva OA. Promising sorbents based on compacted highly porous carbon materials. Journal of Advanced Materials and Technologies. 2023;8(4):270-278. DOI: 10.17277/jamt.2023.04.pp.270-278
Перспективные сорбенты на основе компактированного высокопористого углеродного материала
© И. Н. Шубник, Э. С. Мкртчян", О. А. Ананьева"
а Тамбовский государственный технический университет, ул. Советская, 106/5, пом. 2, Тамбов, 392000, Российская Федерация
И i.shubin77@yandex.ru
Аннотация: Рассмотрены этапы получения компактированного высокопористого углеродного материала (ВУМ), предусматривающие проведение щелочной высокотемпературной активации исходного карбонизата при температуре 400...750 °С продолжительностью 2 ч. В результате активации получен материал, обладающий удельной поверхностью 2600.2700 м/г и объемом пор более 1,3 см/г. Активированный материал компактирован с применением связующих, в качестве которых использовались базальтовое волокно (ВУМ/БВ), поливиниловый спирт (ВУМ/ПВС) и поливинилацетат (ВУМ/ПВА). Условия проведения компактирования -давление прессования в диапазоне от 25 до 1600 кгс/см , температура 75.190 °С и продолжительность от 30 до 150 мин. В результате компактированный материал обладал удельной поверхностью 1550.2000 м /г и удельным объемом пор 0,693.0,849 см /г. Для конечных образцов определена сорбционная емкость по молекулам органического красителя метиленового синего (МС). В результате кинетических исследований выявлена поглотительная способность как исходного материала ВУМ - 1691 мг/г, так и компактированных образцов ВУМ/ПВС - 1611 мг/г, ВУМ/БВ - 1000 мг/г, ВУМ/ПВА - 1270 мг/г. При этом время наступления адсорбционного равновесия составило « 15 мин. Представленные результаты показывают, что компактированный углеродный материал может являться перспективным сорбентом органических поллютантов из водных растворов.
Ключевые слова: высокопористый углеродный материал; компактирование; удельная площадь поверхности; адсорбция; метиленовый синий; кинетика.
Для цитирования: Shubin IN, Mkrtchyan ES, Ananyeva OA. Promising sorbents based on compacted highly porous carbon materials. Journal of Advanced Materials and Technologies. 2023;8(4):270-278. DOI: 10.17277/jamt.2023.04.pp.270-2780
1. Introduction
The development and study of promising highly porous carbon materials with a large specific surface and porosity with a predominance of micro- and mesopores are of interest for many studies, the results of which are in demand in a number of branches of modern industry. These materials seem to be the most promising as universal sorbents for various liquid and gaseous media, devices for storing and transporting fuel, as catalysts, fertilizer carriers, fuel cells, as well as solving environmental problems in such industries as petrochemistry, power engineering, radio electronics, medicine, and agriculture. This is explained primarily by the presence of a balanced combination of a developed system of micro- and mesopores, with a significant specific surface area, corresponding accessible pores and their large volume, with the presence of sufficiently large transport pores that ensure rapid diffusion of sorbed substances, chemical inertness, and stability under real conditions of the use of such materials [1-4].
To produce highly porous carbon materials, various pre-carbonized initial carbon raw materials, including phenol-formaldehyde resin, hydroquinone, carboxymethylcellulose, natural coals, furfural, dextrin, urotropine, carbon nanotubes, graphene, or their combinations are activated with various gasphase or liquid-phase reagents, such as various acids or alkalis, water vapor, etc. [5-11].
Thus, the authors in [12-16] conducted a study of the impact of activation parameters of the initial carbon raw material and the modes of its subsequent compaction on the sorption characteristics of a highly porous carbon material (HPCM), noting their direct relationship and the possibility of scaling the results of laboratory studies in relation to the possibilities of real production.
The use of graphene in the preparation of a highly porous carbon material with a hierarchical pore structure for potential applications in electronics, catalysis, and sorption is the subject of studies [17], where the authors pointed out the promise of the obtained materials, the presence of a significant surface area, and the possibility of chemical doping and functionalization.
The evaluation of the adsorption properties of highly porous materials with the determination of
their structural characteristics was the subject of research in [18, 19], which considered the mechanisms of adsorption and phase behavior of liquids in ordered nanoporous materials with a well-defined pore structure and prove the importance of studying these mechanisms for improving the characteristics of physical adsorption.
The activation process aimed at increasing and improving the volume of micropores, while maintaining a clear network of mesopores was studied in [20]. It was proven that the applied activator - potassium hydroxide - had the biggest impact on the material characteristics, directly contributing to an increase in the volume of micropores. It was shown that alkaline activation is a suitable method for increasing the adsorption capacity of carbon while maintaining a mesoporous structure.
The study of microporous carbon modified with organic substances as fillers to improve thermal and mechanical properties was conducted in [21]. The prepared sorption material showed a significant increase in characteristics when used in thin-film composite direct osmosis membranes.
The prepared highly porous carbon materials can be used in various forms: in the form of powder, granules, films or fibers, both for absorption, separation, purification of various liquid and gaseous substances, and as carriers for catalysts, medicines, etc. However, high requirements are often imposed on them in terms of the possibility of molding into blocks or granules for the convenience of further use in finished products and improvement of its sorption characteristics [22-26].
They are a type of materials with a high specific surface area, large pore volume, and a hierarchical porous structure [27]; they are environmentally friendly, economical, nontoxic, and selective, which makes them good candidates for adsorption of organic and inorganic pollutants from aqueous media, including heavy metals and dyes [28, 29]. They can also be used for drug delivery, catalysis, storage and transportation of gaseous media, ecology, etc. [30].
In modern industry, various dyes are widely used, one of the most common representatives of which is methylene blue (MB), which has the chemical formula C16H18ON3S, which is a representative of the group of quinoneimine dyes
Table 1. Comparative characteristics of MB dye molecules on various carbon nanomaterials
Adsorbent
Nanocomposite of saponified polymethyl acrylate with grafted dextrin with embedded nanosilica
Activated charcoal from seed husks
Nickel alginate aerogel/activated carbon
Activated charcoal derived from corn stalks
Activated charcoal made from olive pits
Biochar obtained from leaf litter by slow pyrolysis
Activated charcoal from walnut shell
Activatedcarbon/cellulose
Activated charcoal from barley husks
рН Experiment conditions Initial concentration, Sorbent mg-L-1 weight, g Time, min Adsorption capacity, mg-g-1 Ref.
7.5 - 20 mg 45 515.40 [36]
- 316 0.055 19.3 436.68 [37]
- 1000 10 mg 48 h 465.12 [38]
11 10 1.4 50 90 % [39]
10 - 0.05 24 h 714 [40]
12 - - - 101.27 [41]
- 50 10 mg 540 632 [42]
6.9 100 - 24 h 103.66 [43]
8 50 0.2 180 61.60 [44]
containing a phenothiazine ring [31]. MB is a cationic dye that is not considered highly toxic to human health at low doses and short-term contact [32]. However, long-term exposure or high levels of MB in water can cause detrimental effects on human health. The toxic effects of methylene blue include permanent damage to human eyes, nausea, diarrhea, skin irritation, and possibly cancer [33, 34]. In connection with the development of anthropogenic activities, a large number of toxic contaminants, including the MB dye, affect the environment due to improper disposal of wastewater from various enterprises. In this regard, the problem of purification of aqueous media from industrial dyes, including MB, the decomposition process of which is very complicated, becomes especially urgent [35].
Currently, materials that are used as sorbents for these purposes and their characteristics are presented in Table 1.
On the basis of preliminary studies, the authors of the paper developed and investigated a compacted highly porous carbon material to solve this environmental problem.
Thus, the purpose of this paper is to study the sorption characteristics of a compacted highly porous carbon material with respect to the organic dye MB.
2. Materials and Methods
2.1. Reagents and method for preparing a compacted highly porous carbon material
At the first stage of research aimed at obtaining a compacted highly porous carbon material, the issues of chemical activation were worked out, which made it possible to determine rational operating parameters and materials: the initial carbon raw material for carbonizate is a mixture of dextrin (Dekstrinzavod CJSC, Murom, Russia) and graphene oxide (Nanotechcenter Ltd., Tambov, Russia), an activator is potassium hydroxide (RM Engineering, Moscow, Russia), the ratio of components of the reaction mixture of carbonizatewas potassium hydroxide: 1 : 3, activation temperature range 400-750 °C, the duration of the main stage was 2 hours [7, 9].
Basalt fiber (HPCM/BF) (KamennyVek Ltd., Dubna, Russia) in the amount of 1-10%, polyvinyl alcohol (HPCM/PVA) (TK Spektr-Khim, Moscow, Russia) and polyvinyl acetate (HPCM/PVAC) (JSC Pigment, Tambov, Russia) - 10-30 % were used as a binder.
2.2. Characterization
The diagnostics of the characteristics of the activated carbon material before compaction, i.e., its specific surface area and porosity, was carried out on the analytical complex Nova Quantachrome E1200 (Quantachrome, Boynton Beach, USA). As a result, a material was obtained with a specific surface area of 2600-2700 m2-g-1 and a pore volume of more than 1.3 cm3-g-1 [7, 9].
2.3. Adsorption studies
To analyze the efficiency of sorption of the synthetic organic MB dye on compacted carbon sorbents, batch experiments were carried out. The sorbent weighing 0.01 g was placed in 30 mL of MB solution with Q| = 1500 mg-L1 according to the Russian standard 4453-74. Each test tube with the solutions to be purified and the sorbent was continuously shaken on a programmable rotator Multi Bio RS-24 (Biosan, Riga, Latvia) for 5, 15, 30, and 60 min. The equilibrium Ce concentration of MB molecules was determined from the optical density measured on a PE-5400V spectrophotometer (Ekros, St. Petersburg, Russia) at a wavelength of I = 815 nm.
The static sorption capacity of Qe sorbents, mg-g-1, was calculated by the formula:
(C0 - Ce)V
Qe = <_0-(1)
m
where Q and Ce are initial and final concentrations of substances in solution, mg-L-1; V is the volume of the solution, L; m is the sorbent sample weight, g.
2.4. Compaction of activated carbon material
For compaction of the activated carbon material, a laboratory setup was developed based on the "IP 100 M - Auto" testing press (Plant of testing instruments and equipment "ZIPO", Armavir, Russia) (Fig. 1).
During this stage, compaction modes were investigated; they included several series of experiments with different pressing pressures, temperatures, and process durations. The amount of the binder was established as a result of preliminary studies by the authors and analysis of literary sources.
For the next stage of research (determination of sorption activity), the samples prepared under the compaction parameters given in Table 2 were used.
Fig. 1. Laboratory setup for studying the compaction
modes of a highly porous carbon material: 1 - press; 2 - heated mold; 3 - press control cabinet; 4 - monitor for setting and displaying the operating modes
Table 2. Compaction mode parameters and characteristics of the prepared samples (blocks)
Parameter HPCM/PVA Composites HPCM/BF HPCM/PVAC
Step wise heating and 75 °C, 3.5 kN, for 15 min 75 °C, 3.5 kN, for 15 min 75 °C, 1.5 kN, for 1 min
pressing 90 °C, 7.5 kN, for 60 min 90 °C, 7.5 kN, for 60 min 90 °C, 3.5 kN, for 1 min
120 °C, 7.5 kN, for 60 min 120 °C, 7.5 kN, for 60 min 130 °C, 7.5 kN, for 1 min
190 °C, kN, for 120 min 190 °C, kN, for 120 min
Mold cooling and pressing-off Up to 40-50 °C Up to 40-50 °C Up to 40-50 °C, placing the sample in an oven for 120 min at a temperature of 80 °C
Block weight, g 16.3-16.8 24.5-25.5 32-33
Height x diameter, mm (24.5-25,5) x 40 (24-25) x 40 (33-234) x 40
3. Results and Discussion
3.1. Finding specific surface area and porous structure parameters
The resulting compacted carbon materials had the following characteristics: specific surface area 1550-2000 m2-g-1, specific micropore volume 0.693-0.849 cm3-g-1.
An analysis of the causes of the difference in the physical and structural characteristics of the resulting materials requires additional research and the accumulation of experimental data, since the mechanism of the binder impact on the carbon material is not fully understood at the moment. At the same time, the authors are inclined to believe that polymeric binders (PVA and PVAC) form a certain spatial structure that provides relatively good permeability and contact surface of the block. In the case of a fiber (BF), it is assumed that a rigid spatial framework is formed in a compacted sample, practically without transport pores.
At the same time, the parameters of compacted materials confirm the correctness and promise of this line of research and can be considered a starting point for further work within this stage, which involves further testing of the pressing parameters and the study of binders, including combinations of polymers with fibers.
3.2. Kinetic studies
As a result of kinetic studies in a static mode, graphs of the dependences of the adsorption capacity of the synthesized materials on the time of contact with a pollutant, the MB dye, were plotted (Fig. 2).
As a result of kinetic studies, it was found that the initial HPCM has an absorption capacity of 1691 mg-g-1 when removing MB dye molecules. When a binding agent is added, the compacted carbon sorbent
M M
ö o
•■ö &
o
T3
<Î
2000 1800 1600 1400 1200 1000 800 600 400 200
-m HPCM
HPCM/PVAC
—A— HPCM/PVA
HPCM/BF
0 5 10 15 20 25 30 35 40 45 50 55 60 65
Time, min
Fig. 2. Adsorption kinetics of MB dye molecules on compacted carbon sorbents HPCM, HPCM/PVA, HPCM/PVAC, HPCM/BF
HPCM/PVA exhibits the highest absorption capacity -1611 mg-g-1. In turn, when using basalt fiber (HPCM/BF) and polyvinyl acetate (HPCM/PVAC), the adsorption capacity is 1000 and 1270 mg-g-1, respectively.
To describe the process of sorption of MB molecules (Table 3), namely, the mechanisms involved in the transfer of sorbate to the surface and inside the structure of sorbents, the obtained experimental data were processed by equations of known kinetic models (equations of pseudo-first and pseudo-second order, the Elovich equation and the intraparticle diffusion equation) [45].
The pseudo-second order model has high correlation coefficients R = 0.9999 for all compacted carbon sorbents HPCM, HPCM/PVA, HPCM/PVAC, HPCM/BF. Accordingly, we can conclude that the reaction between the adsorbate and the functional groups of the sorbent proceeds strictly stoichiometrically (one molecule occupies one
Table 3. Description of the sorption process of MB dye molecules
Sorbents
Pseudo-first order
l0g(Qe - Qt ) = log Qe -
k1
2.303
-t
Pseudo-second order
t 1 1
— =-+—t
Qe
k1
Qe
Qt k2Q2 Qe k2
HPCM 362 -0.0014 0.1387 1666 0.0120 0.9999
HPCM/PVA 400 -0.0062 0.4072 1666 0.0018 0.9999
HPCM/PVAC 232 0.0009 0.3039 1250 -0.0032 0.9999
HPCM/BF 141 -0.0066 0.3716 1000 0.0050 0.9999
Continued Table 3
Elovich equation Intraparticle diffusion equation
Sorbents Qt = 1 1 -ln (aß) + - ln t ß ß Qt = kd t0 5 + C
a ß R2 kid C R2
HPCM 40,28-1036 0.0478 0.3859 6.9197 1616.4 0.2519
HPCM/PVA 22,95-109 0.0136 0.7397 28.866 1516.4 0.564
HPCM/PVAC 96,65-1013 -0.4771 0.0559 -1.6535 1270.0 0.1711
HPCM/BF 11,72-1014 0.0351 0.7113 11.113 925.43 0.5335
Note: Qe is the number of adsorbed dye molecules on the adsorbent surface at the moment of equilibrium, mg-g-1; Qt is the number of adsorbed dye molecules on the surface of the adsorbent at time t, mg-g-1; k1 is the pseudo-first order adsorption rate constant, min-1; k2 is the pseudo-second order adsorption rate constant, g-(mg-min)1; a is the constant adsorption constant, (min-mg-g1)1; p is the degree of surface coverage and chemisorption activation energy, g-mg- ; kid is the internal diffusion coefficient, (mg-(g-min)- )- ; C is the thickness of the boundary layer, mg-g- .
log(Qe - Qt)
2.6 ■
2.4 -2.2 -2.0 -1. 1.6 -1.4 ■ 1.2
0
Qt, mg-g
1700 1500 -1300 -1100 900 -700 -500
0,1387 ■ HPCM R2= 0,4072 ♦ hpcmtvac R2= 0,3039 A hfcm/FVA R2=0,3716 • hpcmbf
20
40 (a)
60 Time, min
■ -i"-t
*
A
R2= 0,3859 ■ HPCM
Ra= 0,7397 ♦ HPCM/PVAC
Ri= 0,0559 A HPCMPVA
R1 = 0,7113 • HPCMBF
1
(c)
ln(t)
t/Qt
0.060.050.040.030.020.01-
0
Qt, mg-g 1
18001600140012001000800600400
R» = 0,9999 ■ hpcm Rs=0,9999 ♦ hpcm p vac RI=0 9999 A hpcm/pva ri=0 9999* hpcmbf
20
40 (b)
60 Time, min
2-- *
♦
A * A
* Ra = 0,2519"HPCM = 0,564 ♦ HPCMTVAC R2 = 0 1711 A HPCWtfVA Rs = 0,5335 • HPCMBF
1
.0.5 t , min
(d)
Fig. 3. Results of mathematical processing of experimental kinetic data: a - the pseudo-first order model; b - the pseudo-second order model; c - the Elovich equation model; d - the intraparticle diffusion equation model
1
3
5
7
2
3
4
position on the sorbent), i.e. a chemical interaction occurs between the dye molecules and the functional groups of the sorbent.
Analyzing the differences in the adsorption characteristics of the studied samples, it can be assumed at this stage of research that when PVA is used as a binder, a certain stable spatial structure is formed that ensures good transport permeability of the adsorbed substances, when PVAC is used, such a structure is formed somewhat worse, with the possible closure of part of the pores directly by the binder. In the case of application as a binder fiber, a significant drop in the sorption capacity can be explained by the formation of a rigid spatial framework in a compacted sample without the formation of transport pores, i.e. only the outer surface of the sample remains active.
4. Conclusion
The conducted studies have shown the relevance of the development of compacted carbon materials for their use as sorption materials. The main stages of obtaining these materials were determined, which included the selection of the initial carbon raw material, the activator and process parameters for high-temperature chemical activation, the establishment of process modes for compacting the prepared activated carbon material (pressure, duration and temperature) - for which a laboratory setup was developed and various binders were selected (for which polyvinyl alcohol, polyvinyl acetate and basalt fiber were used).
The characteristics of the compacted carbon
material were found: the specific surface area and
2 —1
pore volume amounted to 1550-2000 m -g and 0.693-0.849 cm3-g-1, respectively. The maximum adsorption capacity for methylene blue for the initial HPCM was 1691 mg-g-1, while for materials with binding agents HPCM/PVA, HPCM/BF, and HPCM/PVAC it was 1611 mg-g-1, 1000 mg-g-1, and 1270 mg-g-1, respectively. The time of adsorption equilibrium of the process when using carbon sorbents HPCM, HPCM/PVA, HPCM/PVAC, HPCM/BF was « 15 minutes. Also, experimental kinetic data were described using the known equations of kinetic models (the pseudo-first and pseudo-second order equations, the Elovich equation and the intraparticle diffusion equation). As a result, it was found that the experimental dependences have high correlation coefficients R with the calculated values obtained using the pseudo-second order model. This brings us to the conclusion that chemical sorption of the MB dye has a predominant effect on
compacted carbon sorbents. A direct dependence of the sorption capacity of compacted samples and their strength characteristics on the type and content of the binder used and compaction modes was established, which can be explained by the obtained structure of the material, however, these areas are separate stages of research that are not included in this study.
Thus, it can be concluded that the compacted carbon material prepared with various binders can be an effective adsorbent of pollutants from aqueous solutions, which makes it a promising material for solving environmental problems.
5. Funding
The study was supported by the Russian Science Foundation grant No. 22-13-20074, https://rscf.ru/ project/22-13-20074/.
6. Acknowledgments
This work was done using facilities of the shared access center "Production and application of multifunctional nanomaterials" (Tambov State Technical University).
7. Conflict of interests
The authors declare no conflict of interest.
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Information about the authors / Информация об авторах
Elina S. Mkrtchyan, Postgraduate, Tambov State Technical University (TSTU), Tambov, Russian Federation; ORCID 0000-0002-3867-7063; e-mail: elina.mkrtchyan@yandex.ru
Oksana A. Ananyeva, Master's Degree Student, TSTU, Tambov, Russian Federation; ORCID 0000-0002-11889402; e-mail: oksana.a9993471@gmail.com Igor N. Shubin, Cand. Sc. (Eng.), Associate Professor, Associate Professor, TSTU, Tambov, Russian Federation; ORCID 0009-0007-3235-5702; e-mail: i.shubin77@yandex.ru
Мкртчян Элина Сааковна, аспирант, Тамбовский государственный технический университет (ТГТУ), Тамбов, Российская Федерация; ORCID 0000-00023867-7063; e-mail: elina.mkrtchyan@yandex.ru Ананьева Оксана Альбертовна, магистрант, ТГТУ, Тамбов, Российская Федерация; ORCID 0000-00021188-9402; e-mail: oksana.a9993471@gmail.com Шубин Игорь Николаевич, кандидат технических наук, доцент, ТГТУ, Тамбов, Российская Федерация; ORCID 0009-0007-3235-5702; e-mail:
i.shubin77@yandex.ru
Received 25 August 2023; Accepted 9 October 2023; Published 15 December 2023
Copyright: © Shubin IN, Mkrtchyan ES, Ananyeva OA, 2023. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY) license (https://creativecommons.Org/licenses/by/4.0/).
