Volume 97, Issue 7 pp. 703-709

Short Communication

Open Access

CO₂-Responsive Polymers for Membrane Applications: Synthesis and Adsorption Performance

Emil Pashayev,

Emil Pashayev

Helmholtz-Zentrum Geesthacht, Institute of Membrane Research, Max-Planck-Str. 1, 21502 Geesthacht, Germany

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Dr. Prokopios Georgopanos,

Corresponding Author

Dr. Prokopios Georgopanos

[email protected]

orcid.org/0000-0002-6394-0628

Helmholtz-Zentrum Geesthacht, Institute of Membrane Research, Max-Planck-Str. 1, 21502 Geesthacht, Germany

E-mail: [email protected]

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Emil Pashayev,

Emil Pashayev

Helmholtz-Zentrum Geesthacht, Institute of Membrane Research, Max-Planck-Str. 1, 21502 Geesthacht, Germany

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Dr. Prokopios Georgopanos,

Corresponding Author

Dr. Prokopios Georgopanos

[email protected]

orcid.org/0000-0002-6394-0628

Helmholtz-Zentrum Geesthacht, Institute of Membrane Research, Max-Planck-Str. 1, 21502 Geesthacht, Germany

E-mail: [email protected]

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First published: 15 May 2025

https://doi.org/10.1002/cite.202500056

[Correction added on 15 May 2025 after first online publication: The Article title was corrected.]

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Abstract

The pressing need to address climate change has driven research into novel CO₂ capture materials. Here, the synthesis of CO₂-responsive diblock copolymers, i.e., poly(N-[3-(dimethylamino)propyl]-acrylamide)-b-poly(methyl methacrylate) (PDMAPAm-b-PMMA) through a two-step RAFT polymerization process, as well as the use of the synthesized diblock copolymer as a membrane for CO₂ capture were investigated. The resulting diblock copolymer features distinct segments with different properties. The PDMAPAm segment offers CO₂-responsive characteristics, while the PMMA segment provides mechanical stability. The gas transport properties of the fabricated thin-film composite membrane composed of PDMAPAm-b-PMMA or PDMAPAm and polydimethylsiloxane with a gutter layer were measured and the CO₂ adsorption behavior of both PDMAPAm and PDMAPAm-b-PMMA was evaluated. The copolymer exhibits responsiveness to CO₂ and can be customized for use in the fabrication of membranes and membrane adsorbers for direct air capture technologies.

1 Introduction

Carbon capture is a specific area of research that is currently sought after for implementation as a technology [¹] in various sectors, including power generation [²], chemical manufacturing [³], and metal production facilities [⁴], to mitigate CO₂ emissions. Apart from that, the small amount of CO₂ present in the atmosphere can be captured using the newly developed method known as direct air capture (DAC) [⁵]. In DAC technologies, a stronger bond between CO₂ molecules and the solid adsorbent is necessary, indicating that the process is more associated with chemisorption rather than physisorption [⁵].

A block copolymer is a type of polymer that derives from combining different polymers as blocks to merge properties like soft and rigid (i.e., in polystyrene-b-polyisoprene), creating a new material with mixed characteristics. Diblock copolymers can have a significant potential as adsorbents for DAC because of their capacity to develop films with a high active area for gas sorption [^6-10] and scalability [^11-13]. Specifically, diblock copolymers with amine functional groups can exhibit outstanding performance in capturing CO₂, given the strong affinity of amine groups for CO₂ [^{14, 15}]. Some acrylate polymers such as poly(2-(dimethylamino)ethyl methacrylate) (PDMAEMA) [^16-19], poly(N,N-dimethylallylamine) (PDMAAm) [^20-22], poly(2-aminoethyl methacrylate) (PAEM) [^{23, 24}] with amine groups that behave CO₂-responsive, can be utilized as the first block for further chain extension to diblock or triblock copolymers.

In this research, the focus lies on developing a novel diblock copolymer, specifically poly(N-[3-(dimethylamino)propyl]-acrylamide)-b-poly(methyl methacrylate) (PDMAPAm-b-PMMA), using RAFT polymerization, and its initial application is explored as a thin-film composite membrane and polymer powder for CO₂ capture. It should be noted that the type of thin-film composite membranes presented in this work differentiate from the typical gas separation membranes. The thickness of the selective top layer is significantly larger, since the target is to create a type of membrane adsorber.

2 Results and Discussion

The synthesis of PDMAPAm-b-PMMA involves a two-step polymerization of the two monomers. Initially, PDMAPAm was synthesized at 70 °C via RAFT solution polymerization in 1,4-dioxane of the DMAPAm. Subsequently, PDMAPAm serves as a macroRAFT agent to synthesize a PDMAPAm-b-PMMA diblock copolymer by extending the chain through RAFT solution polymerization. Fig. 1 illustrates the pathway for the synthesis of PDMAPAm-b-PMMA.

Details are in the caption following the image — **Figure 1**
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Reaction scheme for the synthesis via RAFT solution polymerization of a) PDMAPAm that serves as the macroRAFT agent and b) of poly(methyl methacrylate) (PMMA) using the macroRAFT agent synthesized in the first step for the synthesis of the PDMAPAm-b-PMMA. Subsequently, the PDMS gutter layer thin-film membrane (on PAN porous support) was coated with the synthesized PDMAPAm-b-PMMA diblock copolymer. The detailed information regarding the coating process has been described in our previous publication [³⁰].

The detailed synthesis procedure of the polymers PDMAPAm and PDMAPAm-b-PMMA is described in previous work [³⁰]. In this study, gas transport properties of the membrane made of the homopolymer PDMAPAm₂₂₂ and mainly its corresponding diblock copolymer PDMAPAm₂₂₂-b-PMMA₈₀ were investigated. The diblock copolymer consists of PDMAPAm:PMMA block ratio = 80:20. The apparent number average molecular weights of the polymers were 24.900 g/mol for the PDMAPAm₂₂₂ and 28600 g/mol for the PDMAPAm₂₂₂-b-PMMA₈₀, respectively.

The preparation of the PDMAPAm-b-PMMA or PDMAPAm polymer thin-film composite involved three distinct steps. Initially, the polymer PDMAPAm-b-PMMA was dissolved in tetrahydrofuran (THF) to form a solution with a 40 % polymer concentration. Subsequently, this solution was applied to a thin-film composite membrane. This membrane comprises a cross-linked polydimethylsiloxane (PDMS) gutter layer, which is cast onto a porous polyacrylonitrile (PAN) film that is supported by a non-woven substrate. The casting process utilized a doctor blade with a gap set to 50 µm. In the final stage, the cast film was dried under nitrogen (N₂) for 24 h. Upon completion of drying, a thin-film composite membrane coated with the PDMAPAm-b-PMMA or PDMAPAm polymer was obtained. The gas transport properties and thickness layers of the PDMAPAm-b-PMMA polymer thin-film composite membrane were then measured using a time-lag device and scanning electron microscopy (SEM), respectively.

2.1 Membrane Morphological Characteristics

The thickness of each layer of the prepared thin-film membrane, coated with PDMAPAm₂₂₂-b-PMMA₈₀ polymer, was measured using SEM cross-sectional imaging. Fig. 2 represents a cross-sectional SEM image of the PDMAPAm₂₂₂-b-PMMA₈₀ polymer thin-film composite membrane. The cross-sectional image proves that the membrane has, as expected, three layers: at the bottom, non-woven with a porous PAN layer, which has a thickness of 0.1 µm, then the PMDS gutter layer with a thickness of 40 µm, and on top of it the PDMAPAm-b-PMMA diblock copolymer. From this image, the thickness of the PDMAPAm-b-PMMA was determined to be approximately 2 µm. Since the membrane of the homopolymer PDMAPAm₂₂₂ was also made with the same method, the thickness of each layer of the PDMAPAm-made thin film composite membrane was assumed to be the same as the diblock copolymer-made membranes.

Another consideration is that the top layer of the membrane, consisting of the PDMAPAm-b-PMMA diblock copolymer, is a non-porous and dense continuous phase. This means that the gas is transported through the membrane at the molecular level via the solution-diffusion mechanism, in which separation is achieved by differences in the solubility of the gases and the difference in the gas concentrations between the feed and the permeate [³⁰].

2.2 Gas Transport Properties

Time-lag and permeabilities of different gases through thin-film composite membranes with and without the PDMAPAm and PDMAPAm-b-PMMA polymer-coated were measured using the time-lag machine to characterize the gas transport properties of the membranes. As mentioned in our previous publication [³⁰], the membrane without coating exhibits extremely high permeability values for all measured gases (vapor H₂O, CO₂, O₂, N₂), which means it shows no resistance to these gases. However, after coating it with PDMAPAm or PDMAPAm-b-PMMA polymers, the permeability values turned to be reasonable.

In Fig. 3, the permeabilities of H₂O (saturation vapor at a pressure of 10⁻⁶ mBar), CO₂, O₂, and N₂ gases are presented, while Fig. 4 compares selectivities of the PDMAPAm₂₂₂ and PDMAPAm₂₂₂-b-PMMA₈₀ thin-film composite membranes for the corresponding gases.

In detail, for the thin-film composite membranes of PDMAPAm and PDMAPAm-b-PMMA, CO₂ and H₂O gases show larger permeability through the membrane than O₂ and N₂, making the membrane more selective for H₂O and CO₂ than N₂ and O₂. This means that the membranes can separate H₂O and CO₂ from the rest two gases. As for comparison of gas transport properties of the PDMAPAm₂₂₂-coated membrane with the PDMAPAm₂₂₂-b-PMM₈₀-coated membrane, CO₂/N₂ H₂O/N₂ selectivities of the homopolymer-coated membrane appear higher than in the corresponding diblock copolymer-coated copolymer. This means that the PDMAPAm-coated membrane can separate CO₂ and water vapor from other gases, unlike PDMAPAm-b-PMMA.

The membrane performance can be compared to other types of amine-containing polymers, such as poly(amidoamine) (PAMAM)-based membranes that indicated CO₂ permeabilities in the range of 10² to 10³ Barrer with CO₂/N₂ selectivities between 10 and 50 [²⁶]. In addition to that, polyamide-based membranes typically exhibit CO₂ permeabilities around 100 Barrer with CO₂/N₂ selectivities in the range of 10–20 [²⁷], which also meets the selectivities and permeabilities range of PDMAPAm and PDMAPAm-b-PMMA-coated membranes that were obtained from time-lag measurement

Furthermore, by altering the PMMA block amount, different diblock copolymers (such as PDMAPAm₂₂₂-b-PMMA₁₈₆, PDMAPAm₂₂₂-b-PMMA₈₀, and PDMAPAm₂₂₂-b-PMMA₃₉) of the homopolymer PDMAPAm₂₂₂ were synthesized. The same kind of thin-film composite membranes were prepared from the polymers and the gas transport properties of the membrane were determined. As illustrated in Fig. 5, by altering the ratio of the first block to the second block of the copolymer (PDMAPAm-b-PMMA), the selectivity of the PDMAPAm-b-PMMA thin-film composite membrane was customized (see Tab. S1 in the Supporting Information). It is clear from the figure below that the membrane's selectivity rises up to five times as the PDMAPAm proportion of the diblock copolymer is increased. This can be explained by the fact that more amine groups that have affinity to CO₂ and H₂O [^{14, 28}], interact and make the polymer more selective for CO₂ in comparison to other gases.

Moreover, considering the thickness of the PDMAPAm₂₂₂-b-PMMA₈₀ and PDMAPAm₂₂₂ polymer layer was 2 µm(as mentioned before) and knowing the time lag and permeability of each gas through the membrane, diffusion coefficients and solubility of the gases can be calculated using the equation described in the literature [²⁵].

In Table 1, the calculated values of the diffusion coefficients and solubilities of all four gases for the PDMAPAm and PDMAPAm-b-PMMA polymer film composite membranes are presented.

Table 1. Diffusion coefficients and solubilities of gases for PDMAPAm₂₂₂ and PDMAPAm₂₂₂-b-PMMA₈₀ polymer film composite membranes [³⁰].

Polymers	Gases	D [cm²s⁻¹]	S [cm³(STP)/(cm³ cmHg)]	S (CO₂)/S (N₂)
PDMAPAm₂₂₂	H₂O	5.6·10⁻⁹	2.9·10³	5.3
	CO₂	3.9·10⁻⁹	2.6·10¹
	O₂	1.5·10⁻⁹	8.7·10⁰
	N₂	2.1·10⁻⁹	4.8·10⁰
PDMAPAm₂₂₂-b-PMMA₈₀	H₂O	3.1·10⁻⁹	8.5·10²	1.0
	CO₂	6.0·10⁻⁹	1.3·10¹
	O₂	2.0·10⁻⁹	1.9·10¹
	N₂	2.2·10⁻⁹	1.3·10¹

Generally, diffusion coefficients of CO₂ and H₂O of both PDMAPAm and PDMAPAm-b-PMMA-coated polymer membranes are higher than the diffusion coefficient values of O₂ and N₂. As for comparison of homopolymer-contained membrane with the diblock copolymer-contained, the CO₂ and H₂O diffusion coefficients through the PDMAPAm polymer membrane appears almost double times lower than through the PDMAPAm-b-PMMA-coated membrane.

Apart from that, it can be clearly seen from Tab. 1 that CO₂ and H₂O gases are more soluble in both PDMAPAm and PDMAPAm-b-PMMA-coated polymers than the rest two gases are. Going in more detail, the solubility of CO₂ than N₂ especially in the PDMAPAm polymer membrane turns to be almost five times higher than in the PDMAPAm-b-PMMA polymer membrane. This can be related to the fact that there is a higher amount of tertiary amine groups per mol in the homopolymer case leading to more physical interaction of amine groups with CO₂ than in the diblock copolymer that makes the PDMAPAm polymer membrane more CO₂-responsive than PDMAPAm-b-PMMA polymer membrane [^{30, 31}]. This part will be discussed in more detail in our publications.

Furthermore, the PDMAPAm and PDMAPAm-b-PMMA thin-film composite membrane show diffusion coefficients and solubility values for gases that align with the literature for similar polymers. Membranes from hyperbranched polymers such as from poly(amidoamine) (PAMAM) [²⁶] and also polyamide membranes containing PDMS groups [²⁹] exhibit CO₂ diffusion coefficients in the range of 10⁻⁸ cm²s⁻¹ and solubility values around 10⁻¹ cm³(STP)/(cm³ cmHg)), which agree well with the results in this study.

2.3 CO2 Adsorption Behavior of Synthesized Polymers

Furthermore, to investigate the CO₂ capture capacity of the newly developed polymer, CO₂ adsorption was measured using the powdered PDMAPAm and PDMAPAm-b-PMMA polymers in the device Rubotherm at 30 °C and up to 2 bar. Fig. 6 illustrates the CO₂ adsorption isotherms produced from PDMAPAm₂₂₂ and PDMAPAm₂₂₂-b-PMMA₈₀. As it is observed, PDMAPAm and PDMAPAm-b-PMMA polymers illustrate CO₂ sorption behavior, and both PDMAPm and PDMAPAm-b-PMMA show similar trends of CO₂ adsorption uptake with respect to pressure increase. However, the existence of PMMA in the polymer as a block increases, the CO₂ the uptake capacity of the polymer. This may be related to the possible physical interaction that can occur between PMMA and CO₂ under mild pressures and temperatures as described in [³¹].

The CO₂ uptake capacity of PDMAPAm and PDMAPAm-b-PMMA of 6 mg g⁻¹ at 2 bar and 30 °C is quite comparable with the performance of the other polymers existing in the literature. For comparison, some hyper-cross-linked polymers (HCPs) have shown CO₂ uptake capacities ranging from 1.7 mmol g⁻¹ (approximately 75 mg g⁻¹) at atmospheric pressure to 13.4 mmol g⁻¹ (approximately 590 mg g⁻¹) at 30 bar [^{32, 33}]. Another study reported a CO₂ uptake of 0.82 g g⁻¹ (820 mg g⁻¹) for certain carbon-sulfur or carbon-nitrogen solid sorbents [³⁴]. While the newly developed polymer uptake is lower than these high-pressure values, it is important to consider the specific conditions and applications.

To sum it all up, both time-lag and sorption measurement demonstrated that the newly developed polymers, PDMAPAm and PDMAPAm-b-PMMA, show CO₂-responsiveness because CO₂ and H₂O diffusion coefficients and solubilities appear to be higher than the rest two gases and the polymers in powdered form exhibit CO₂ sorption behavior, which can be comparable with literature. The CO₂ sorption and solubility performance of PDMAPAm and PDMAPAm-b-PMMA is promising and could be optimized further for application in DAC technologies.

3 Conclusion

A new CO₂-reactive material, namely, PDMAPAm-b-PMMA diblock copolymers, was developed by a two-step RAFT solution polymerization. After that, the gas transport properties of the thin composite film membrane made of the PDMAPAm-b-PMMA polymer and PDMS with a gutter layer were examined. According to the time-lag measurement of the gases, the membrane is more selective for CO₂ and H₂O than for O₂ and N₂, which means the membrane can separate CO₂ and H₂O from the rest of the gases. Additionally, diffusion coefficients of CO₂ were calculated to be 2–3 times higher than those for the other three gases, approximately 6.4·10⁻⁸ cm²s⁻¹. Ultimately, the CO₂ capture performance of PDMAPAm-b-PMMA was evaluated up to 2 bar, revealing that the polymer exhibits significant potential for effective CO₂ capture. For the future, this indicates that PDMAPAm-b-PMMA copolymer could be a promising material for application in DAC technologies, which, however, needs to be further advanced via the improvement of polymer synthesis and membrane fabrication.

Supporting Information

Supporting information for this article can be found under DOI: https://doi.org/10.1002/cite.202500056.

Acknowledgment

The authors thank Silvio Neumann and Maren Brinkmann for performing the NMR, TGA, DSC, and GPC measurements, Dr. Evgeni Sperling for SEM measurement, and Dr. Sergey Shishatskiy for his assistance on the Time-Lag measurements. Scientific discussions with Prof. Dr. Volker Abetz are greatly acknowledged. This work was supported by the Initiative and Networking Fund of the Helmholtz Association, project DACStorE (KA2-HSC-12).

Open access funding enabled and organized by Projekt DEAL.

Abbreviations

DAC: direct air capture
PAN: polyacrylonitrile
PDMAPAm-b-PMMA: poly(N-[3-(dimethylamino)propyl]-acrylamide)-b-poly(methyl methacrylate)
PDMS: polydimethylsiloxane
SEM: scanning electron microscopy

Supporting Information

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Volume97, Issue7

Special Issue: Membrantechnik

July 2025

Pages 703-709

CO₂-Responsive Polymers for Membrane Applications: Synthesis and Adsorption Performance

Abstract

1 Introduction

2 Results and Discussion

2.1 Membrane Morphological Characteristics

2.2 Gas Transport Properties

2.3 CO2 Adsorption Behavior of Synthesized Polymers

3 Conclusion

Supporting Information

Acknowledgment

Abbreviations

Supporting Information

References

Figures

References

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CO2-Responsive Polymers for Membrane Applications: Synthesis and Adsorption Performance

Abstract

1 Introduction

2 Results and Discussion

2.1 Membrane Morphological Characteristics

2.2 Gas Transport Properties

2.3 CO2 Adsorption Behavior of Synthesized Polymers

3 Conclusion

Supporting Information

Acknowledgment

Abbreviations

Supporting Information

References

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CO₂-Responsive Polymers for Membrane Applications: Synthesis and Adsorption Performance