Highly efficient CO2 adsorption by imidazole and tetraethylenepentamine functional sorbents: Optimization and analysis using response surface methodology

doi:10.1016/j.jece.2021.105639

Journal of Environmental Chemical Engineering

Volume 9, Issue 4, August 2021, 105639

https://doi.org/10.1016/j.jece.2021.105639 Get rights and content

Highlights

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Imidazole was introduced into the TEPA-functionalized adsorbent.
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The RSM was used to optimize the experiments conditions.
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The sorbents showed excellent amine efficiency after the introduction of Im.
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The sorbents showed higher adsorption capacity and thermal stability under low pressure.
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The adsorption energy of the TEPA-Im functionalized adsorbent was calculated by DFT.

Abstract

SBA-15 was selected as a support and modified with a mixture of tetraethylenepentamine (TEPA) and imidazole (Im) by impregnation method to prepare CO₂ solid adsorbents. The Response Surface Methodology (RSM) based on Central Composite Design (CCD) was used to evaluate and optimize the effect of Im, TEPA loading and adsorption temperature as independent variables on the CO₂ adsorption capacity as the response function. A good agreement between the model prediction and experimental results. The adsorbents were characterized by BET, XRD, FT-IR, TG, TEM and elemental analysis. The introduction of Im improved the adsorption capacity and thermal stability of the adsorbents, but did not change the structure of SBA-15. This is mainly because that the CO₂-C₃H₄N₂ complex formed by Im and CO₂ reaction can effectively improve the adsorption efficiency of the adsorbent. SBA-15-39.5% TEPA-22% Im showed the highest adsorption energy by density functional theory (DFT) calculation, − 39.82 kJ/mol. SBA-15-39.5% TEPA-22% Im obtained the highest CO₂ adsorption capacity of 4.27 mmol/g in 15 vol% CO₂ at 50 °C. After 10 cycles, CO₂ uptake remained relatively stable at 4.07 mmol/g.

Graphical Abstract

Introduction

The problems caused by the greenhouse effect have attracted global attention [1], [2], [3]. Carbon dioxide (CO₂) produced by the burning of fossil fuels is considered to be the main cause of the greenhouse effect [2], [3], [4]. Therefore, capturing CO₂ from the flue gas produced by the combustion of fossil fuels is an effective solution to reduce CO₂ emissions [3], [4], [5], [6]. At present, carbon dioxide capture and storage (CCS) is considered the most reliable method [5], [6], [7], [8]. Among them, the use of liquid amine to capture CO₂ is the most mature method, and which has been successfully industrialized [5], [6], [9], [10], [11]. However, it also has some disadvantages, such as high energy consumption for amine regeneration, corrosion of equipment and huge absorption equipment [12], [13].

Studies have shown that the solid amine adsorbent can better solve the above problems [14], [15]. It can not only solve the problem of equipment corrosion in the liquid amine absorption process [16], but also reduce the energy consumption of regeneration [17]. Typically, the regeneration temperature of traditional amine solutions was higher than 120 °C [18]. Whereas the solid amine adsorbent was regenerated in an inert gas atmosphere (such as N₂, He or Ar) at a temperature of 50–120 °C [19]. The lower the desorption temperature, the lower the regeneration energy consumption [20]. In addition, a lower regeneration working temperature can reduce the loss of amine during the regeneration process, improve amine efficiency, and reduce CO₂ capture costs. Commonly used solid amine adsorbent supports are mainly porous materials, such as zeolite [21], activated carbon [22], metal organic framework [23] and mesoporous silica [24], [25]. Among them, the typical mesoporous silica SBA-15 is the most representative of the adsorbent carrier [26], [27]. SBA-15 has the advantages of high specific surface area, orderly mesopore arrangement and adjustable pore size. TEPA has the advantages of high nitrogen content, low viscosity and low CO₂ diffusion resistance. After SBA-15 is impregnated with tetraethylenepentamine (TEPA), the prepared adsorbent has a higher CO₂ adsorption capacity. Therefore, it has attracted the attention of researchers [28], [29], [30]. Olea et al. modified SBA-15 with a pore expander and functionalized it with amine impregnation. Studies have shown that the adsorption temperature is 45 °C, and the adsorption capacity of the prepared PE-SBA-15(17e)-TEPA adsorbent reaches 105 mg CO₂/ g. After 4 adsorption-desorption, the adsorption capacity loss of the adsorbent is 26% [31]. Liu et al. studied the effect of impregnating mesoporous silica foam (TEPA-MSF-x) with different masses of TEPA loads on the performance of adsorbents. The results show that at an adsorption temperature of 75 °C, the TEPA-MSF-1.0P adsorbent has poor circulation, and the capacity loss is as high as 54% after 5 adsorption-desorption cycles [32]. However, the study also found that the stability of TEPA in the adsorption-desorption cycle is relatively low [15], [31], [32]. Fortunately, researchers found that imidazole (Im) has good thermal and antioxidant stability [33], [34], [35], [36]. Therefore, Im can be introduced during the preparation of the adsorbent to improve the stability of the adsorbent. However, the adsorption capacity of Im is inferior to TEPA, and it has the disadvantages of high viscosity and low vapor pressure. Therefore, when Im is introduced into the adsorbent, its addition has a greater impact on the adsorption capacity of the adsorbent [33], [36].

Different parameters such as amine species, mixing ratio of amine and adsorption temperature could affect the CO₂ adsorption performance of adsorbent. In most reported literature, the effect of each variable was invested independently, with the other variables kept constant. This method does not consider the mutual influence of all the variables involved, and optimizing these factors will require a lot of experimentation, more time and more cost. In order to overcome the limitations and shortcomings of conventional research methods, it is necessary to optimize the factors affecting the preparation of adsorbents. In the theoretical design and statistical evaluation of experiments, response surface methodology (RSM) is a reliable statistical tool in multivariate systems. It uses a reasonable experimental design method to treat the response of the system as a function of one or more factors, and seeks the optimal process parameters through the analysis of the regression equation. As a result, the mathematical function relationship as well as the mutual effect between various factors will be directly displayed through graphic technology. Therefore, it can select the optimal conditions in the experimental design by intuitive observation and provide guidance for subsequent design or testing [37], [38]. Through reasonable experimental design, the number of experiments can be reduced, thereby reducing the time and cost of the experiment. Response surface methodology RSM has been successfully applied to the development of new advanced adsorption and catalytic materials [39], [40].

In this paper, the preparation of imidazole and tetraethylenepentamine functional adsorbents and their adsorption performance for CO₂ adsorption was investigated. First, we introduced Im into TEPA-based solid adsorbents, the effect of adsorption temperature, TEPA loading, Im loading and their interactions was evaluated using a Central Composite Design (CCD) combined with RSM. Under the optimal conditions, the maximum CO₂ adsorption capacity was obtained, which was verified by experiments. Then the influence of the introduction of Im on the adsorption performance of the amine modified adsorbent was studied by a series of characterization. Finally, the corresponding adsorption mechanism is proposed, and the adsorption energy is calculated by density functional theory (DFT).

Section snippets

Materials

Imidazole (Im, Mw=68.08, Sigma-Aldrich), Tetraethylenepentamine (TEPA, Tianjin Dadong Chemical Reagent Factory) and SBA-15 (Xianfeng Nano Factory) were purchased and used without purification. Ethanol (≥ 99.9%) were purchase from Tianjin Damao Chemical Reagent Factory. CO₂ (99.99%) and N₂ (99.99%) were obtained from Anqiu Hengan Gas Plant.

Synthesis of different adsorbents

Different adsorbents were prepared by impregnation method [41]. A certain ratio of TEPA and Im was dissolved in 20 mL anhydrous ethanol. The mixture was

Data analysis

Data were analyzed by the analysis of variance (ANOVA), as shown in Table 2 and Table S2. 17 groups of experimental data were subjected to regression analysis to obtain quadratic regression equation of CO₂ capture capacity (Eq. (4).) The coefficient of each term in the quadratic regression equation can indicate its effect on CO₂ adsorption to a certain extent. A positive sign represents a favorable or synergistic effect on CO₂ capture capacity, and negative sign represents a unfavorable effect

Conclusion

In this paper, a CCD combined with RSM was used to evaluate and to optimize the effect of the adsorption temperature, TEPA and Im loading on CO₂ adsorption capacity of adsorbent. The optimal conditions found for adsorption capacity of CO₂ were, 39.5 wt%TEPA, 22 wt%Im and adsorption temperature 50 °C; by using optimized values, the adsorption capacity of CO₂ reached 4.27 mmol/g. Results were in good agreement with the ones predicted by the model. TG and XRD analysis showed that the introduction

CRediT authorship contribution statement

Huangyu Yan: Conceptualization, Methodology, Investigation, Writing - original draft. Guojie Zhang: Writing - review & editing, Resources, Supervision, Funding acquisition. Jun Liu: Methodology, Validation, Writing - review & editing. Guoqiang Li: Validation, Writing - review & editing. Ying Wang: Project administration.

Declaration of Competing Interest

The authors declare no conflict of interest.

Acknowledgments

This work was supported by the National Natural Science Foundation of China (Nos. 21878200 and 21676174), Shanxi Scholarship Council of China (2017–036) and Graduate Research and Innovation Projects of Shanxi Province (2020).

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Highly efficient CO2 adsorption by imidazole and tetraethylenepentamine functional sorbents: Optimization and analysis using response surface methodology

Highlights

Abstract

Graphical Abstract

Introduction

Section snippets

Materials

Synthesis of different adsorbents

Data analysis

Conclusion

CRediT authorship contribution statement

Declaration of Competing Interest

Acknowledgments

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Chem. Eng. J.

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J. Environ. Sci. (China)

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Highly efficient CO₂ adsorption by imidazole and tetraethylenepentamine functional sorbents: Optimization and analysis using response surface methodology