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. 2024 Dec 11;9(51):50466-50475.
doi: 10.1021/acsomega.4c07631. eCollection 2024 Dec 24.

In Situ Polymerization Electrospinning of Amine-Epoxy/Poly(vinyl alcohol) Nanofiber Webs for Direct CO2 Capture from the Air

Chisato Okada  1   2 , Zongzi Hou  3 , Hiroaki Imoto  2 , Kensuke Naka  2 , Takeshi Kikutani  4 , Midori Takasaki  3
Affiliations

In Situ Polymerization Electrospinning of Amine-Epoxy/Poly(vinyl alcohol) Nanofiber Webs for Direct CO2 Capture from the Air

Chisato Okada et al. ACS Omega. .

Abstract

To achieve carbon neutrality by 2050, there is a growing need to actively capture carbon dioxide (CO2) from the atmosphere. As a method to capture CO2 directly from the atmosphere, direct air capture (DAC) is attracting attention and amine-based compounds have been extensively studied as CO2 adsorbents. In this research, we developed thermosetting DAC nanofibers with excellent low-temperature desorption properties and good heat resistance by polymerizing an amine with epoxy. For the fabrication of epoxy-cross-linked amine nanofibers through the electrospinning process, poly(vinyl alcohol) (PVA) was added for the improvement of spinnability, and the direct spin-line heating was conducted for the in situ thermal polymerization. As a result, nanofiber webs with fiber diameters of approximately 300-400 nm were fabricated successfully. The investigation of the CO2 adsorption and desorption performance of the obtained amine/epoxy/PVA (AE/PVA) nanofiber webs verified the high adsorption amount of 1.8 mmol/g at a CO2 concentration of 400 ppm. Additionally, 93% of adsorbed CO2 could be desorbed at a low temperature of 65 °C. These results suggested the possibility of low-energy-consumption CO2 recovery. By improving the adsorption rate and by making desorption possible at low temperatures, the adsorption/desorption cycle can be repeated more quickly, increasing the amount of CO2 that can be recovered in a day. The prepared webs also exhibited an excellent adsorption retention ratio of 75% after 100 h of operation at 85 °C, while general amine-filled mesoporous silica usually shows a retention ratio of only 13%. In addition, FT-IR, DSC, and elemental analysis of amine/epoxy/PVA nanofibers were carried out to analyze the reaction mechanism during fiber production. It was revealed that PVA was not involved in the reaction, and as in the bulk state, almost all primary amines were converted to secondary amines due to the in situ polymerization of amines and epoxy to form nanofibers.

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Conflict of interest statement

The authors declare no competing financial interest.

Figures

Figure 1
Figure 1
Chemical structural formula of (a) PEI, (b) EDE, (c) T-X, and (d) PVA and (e) chemical reaction of amine and epoxy to form secondary amine as indicated.
Figure 2
Figure 2
Schematic of the adsorption/desorption measurement system.
Figure 3
Figure 3
CO2-amine reactions under dry and humid conditions. (a) Reaction of CO2–primary amine under dry condition, (b) reaction of CO2–secondary amine under dry condition, and (c) reaction of CO2–primary and secondary amine under humid condition.
Figure 4
Figure 4
Process schematic for making fibers by electrospinning; (a) without heating and (b) heating with a heat gun.
Figure 5
Figure 5
SEM images of the top surface of electrospun sheet/fiber; (a) amine–epoxy/PVA prepared at room temperature, (b) only PVA prepared at room temperature, and (c) amine–epoxy/PVA prepared at 100 °C (collector temperature).
Figure 6
Figure 6
DSC thermograms measured with a heating and cooling rate of 10 °C/min for the AE/PVA nanofiber web prepared with a heat gun temperature of 120 °C; (a) DSC curves during heating, cooling, and second heating cycles, and (b) enlarged DSC curve of the second heating.
Figure 7
Figure 7
Variation of CO2 adsorption amount with time measured at 20 °C, 50%RH using the N2 mixture gas with a CO2 content of 400 ppm for the AE/PVA nanofiber web, and the corresponding data calculated excluding the mass of PVA (based on mass of AE). Data for amine–epoxy monolith and mesoporous silica filled with liquid amine are also shown for comparison.
Figure 8
Figure 8
Saturated adsorption amount of CO2, before and after 100 h of heat treatment at 85 °C for the AE/PVA nanofiber web. Data for amine–epoxy monolith and mesoporous silica filled with liquid amine are shown for comparison. Retention ratios representing heat resistance properties are also indicated.
Figure 9
Figure 9
DSC curves of the first and second heating for the analysis of the heat of reaction (HR) measured at the heating rate of 10 °C/min for the mixture of amine, epoxy, and PVA (A + E + PVA), the mixture of amine and epoxy (A + E), and pure PVA. Peak temperatures HR for (A + E + PVA) and (A + E) are shown in the figure.
Figure 10
Figure 10
ATR-FTIR spectra of the AE/PVA nanofiber, pure PVA, the reaction product of amine and epoxy (AE), and the mixture of amine and epoxy (A + E).
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