CO_2优先渗透的“双高”杂化功能炭膜的制备及性能研究
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摘要
CO2作为一种主要的温室气体,其产生的“温室效应”日益严重地威胁着人类的生产和生活。实现对CO2的减排、分离及回收利用,已成为人类共同关心的问题。炭膜是近二十多年来迅速发展起来的一种新型多孔炭基膜材料,它可通过“分子筛分”机理对分子直径相近的小分子气体进行分离,并具有较高的气体渗透能力和分离选择性,可实现C02／CH4,C02/N2等体系中C02的有效分离,然而,目前制备的炭膜其C02气体的渗透通量还无法满足工业实际应用要求。因此,如何在保持较高选择性的条件下,进一步提高C02气体的渗透能力,是制备高性能分离C02的功能炭膜的关键。
本文采用共混的方法,在前驱体聚酰胺酸中分别掺杂钛硅分子筛(TS-1)、纳米炭粉及纳米碳管,经高温热解炭化制备出杂化功能炭膜。分别考察了掺杂物种类及其掺杂浓度、热解温度、测试温度、测试压力等因素对功能炭膜气体渗透性和分离选择性的影响,并通过XRD、TEM、FTIR及TG等分析手段对所制备功能炭膜进行表征,采用恒压变体积法与色谱联用的技术测定膜的气体渗透性能。
结果表明,掺杂钛硅分子筛(TS-1)可大幅提高炭膜对各种气体尤其是吸附性气体C02的渗透性能；当掺杂浓度为20wt.%,炭化温度为600℃时,C02、H2、02、N2、CH4的渗透系数分别可达9087 Barre、8111 Barre、2017 Barre、426 Barrer和357 Barrer; CO2(0.33nm)对纯气体的渗透通量首次超过了分子直径比其小的H2(0.289nm)的渗透通量。各功能炭膜的气体渗透系数均随掺杂量的增加而增加,而分离选择系数下降。炭化温度对功能炭膜气体渗透性有显著影响,当炭化温度超过700℃时,功能炭膜对各气体的渗透性显著下降,而对气体的分离选择性则急剧增大。钛硅分子筛掺杂制备的功能炭膜的气体渗透性能随测试温度的改变有明显变化,而测试压力对其没有显著影响。纳米炭粉掺杂制备的功能炭膜对提高C02的渗透通量具有一定作用,但对其它气体的渗透性影响不大,纳米炭原粉掺杂制备的功能炭膜与纳米炭粉掺杂制备的功能炭膜相比,气体渗透性有比较明显的提高,分离选择性变化不大。掺杂多壁碳纳米管制备出了CO2渗透性能和分离性能较高的功能炭膜。
因此,通过有效控制功能基团的种类、加入量及炭化工艺条件,可以成功地制备CO2优先渗透的高渗透、高分离选择性的杂化功能炭膜。
As a major greenhouse gas, CO2 has increasingly serious threaten to human production and life with producing a "greenhouse effect". How to reduce carbon dioxide emissions and their separation, recovery, purification, has become a common concern of mankind. Carbon membrane is developed rapidly in recent decades as a new type of porous carbon-based membrane material, which can separate gases with similar diameters with "molecular sieving" mechanism and shows high gas permeability and selectivity. Although the seperation of CO2 can be achieved from CO2/CH4, CO2/N2 systems, the permeability of carbon membranes prepared for CO2 still relatively small and difficult to meet industrial application requirements. Therefore, how to increase the permeability of CO2 and maintain a ralative high selectivity is a critical factor to prepare a high-performance carbon membrane for separation of CO2.
In this paper, functional carbon membranes for CO2 separation were designed and prepared by incorporating titanium silicalite nanoparticles, nano-toner and carbon nanotube into polyimide, which is used as the precursor of carbon membrane in this work, respectively. The characterizations of the as-synthesized membranes were studied by XRD, TEM, and FTIRand TG. The effects of doping agents and amount, permeating temperature and pyrolytic temperature on the gas permeation of functional carbon membranes were mainly investigated by gas permeation GC coupling technique.
Gas permeation test results show the permeability of functional carbon membranes incorperating with TS-1 is improved a lot compared to pure carbon membrane, especially to absorbing gas such as CO2 whose permeability is enhanced by nearly 30 times at most. The permeabilities of membranes dopped with 20.wt% TS-1 and carbonized at 600℃for pure gas CO2、H2、O2、N2、CH4 are 9087、8111、2017、426 and 357 Barrer(1 Barrer=10-10 cm3(STP)·cm·cm-2·s-1·cmHg-1), respectively. The permeability of CO2(0.33 nm) exceeds that of H2 whose molecular diameter is about 0.289nm.With the increase of the dopant amount, gas permeability of the prepared membranes increases. Results also indicate the permeability of prepaerd membranes is affected significantly by the pyrolysis temperature. When the temperature is above 700℃, the gas permeability exhibites a drastic drop, while the selectivity decreases seriously.The performance is also influenced by permeating temperature, not related to feed pressure. The functional membrane prepared with nano-charcoal powders improves the CO2 permeability more or less, but has little effect on other gases. Compared with nano-charcoal powders, incorporating nano-charcoal raw powders enhances the gas permeability a little,while the slectivy has no change. The prepared composite functional memebranes dopped with MWNT exhibit high CO2 peameability and selectivity.
As a result, membranes with high CO2 permeaselecticity can be prepared through controlling the doping agents, amount and conditions of carbonization.
本文采用共混的方法,在前驱体聚酰胺酸中分别掺杂钛硅分子筛(TS-1)、纳米炭粉及纳米碳管,经高温热解炭化制备出杂化功能炭膜。分别考察了掺杂物种类及其掺杂浓度、热解温度、测试温度、测试压力等因素对功能炭膜气体渗透性和分离选择性的影响,并通过XRD、TEM、FTIR及TG等分析手段对所制备功能炭膜进行表征,采用恒压变体积法与色谱联用的技术测定膜的气体渗透性能。
结果表明,掺杂钛硅分子筛(TS-1)可大幅提高炭膜对各种气体尤其是吸附性气体C02的渗透性能；当掺杂浓度为20wt.%,炭化温度为600℃时,C02、H2、02、N2、CH4的渗透系数分别可达9087 Barre、8111 Barre、2017 Barre、426 Barrer和357 Barrer; CO2(0.33nm)对纯气体的渗透通量首次超过了分子直径比其小的H2(0.289nm)的渗透通量。各功能炭膜的气体渗透系数均随掺杂量的增加而增加,而分离选择系数下降。炭化温度对功能炭膜气体渗透性有显著影响,当炭化温度超过700℃时,功能炭膜对各气体的渗透性显著下降,而对气体的分离选择性则急剧增大。钛硅分子筛掺杂制备的功能炭膜的气体渗透性能随测试温度的改变有明显变化,而测试压力对其没有显著影响。纳米炭粉掺杂制备的功能炭膜对提高C02的渗透通量具有一定作用,但对其它气体的渗透性影响不大,纳米炭原粉掺杂制备的功能炭膜与纳米炭粉掺杂制备的功能炭膜相比,气体渗透性有比较明显的提高,分离选择性变化不大。掺杂多壁碳纳米管制备出了CO2渗透性能和分离性能较高的功能炭膜。
因此,通过有效控制功能基团的种类、加入量及炭化工艺条件,可以成功地制备CO2优先渗透的高渗透、高分离选择性的杂化功能炭膜。
As a major greenhouse gas, CO2 has increasingly serious threaten to human production and life with producing a "greenhouse effect". How to reduce carbon dioxide emissions and their separation, recovery, purification, has become a common concern of mankind. Carbon membrane is developed rapidly in recent decades as a new type of porous carbon-based membrane material, which can separate gases with similar diameters with "molecular sieving" mechanism and shows high gas permeability and selectivity. Although the seperation of CO2 can be achieved from CO2/CH4, CO2/N2 systems, the permeability of carbon membranes prepared for CO2 still relatively small and difficult to meet industrial application requirements. Therefore, how to increase the permeability of CO2 and maintain a ralative high selectivity is a critical factor to prepare a high-performance carbon membrane for separation of CO2.
In this paper, functional carbon membranes for CO2 separation were designed and prepared by incorporating titanium silicalite nanoparticles, nano-toner and carbon nanotube into polyimide, which is used as the precursor of carbon membrane in this work, respectively. The characterizations of the as-synthesized membranes were studied by XRD, TEM, and FTIRand TG. The effects of doping agents and amount, permeating temperature and pyrolytic temperature on the gas permeation of functional carbon membranes were mainly investigated by gas permeation GC coupling technique.
Gas permeation test results show the permeability of functional carbon membranes incorperating with TS-1 is improved a lot compared to pure carbon membrane, especially to absorbing gas such as CO2 whose permeability is enhanced by nearly 30 times at most. The permeabilities of membranes dopped with 20.wt% TS-1 and carbonized at 600℃for pure gas CO2、H2、O2、N2、CH4 are 9087、8111、2017、426 and 357 Barrer(1 Barrer=10-10 cm3(STP)·cm·cm-2·s-1·cmHg-1), respectively. The permeability of CO2(0.33 nm) exceeds that of H2 whose molecular diameter is about 0.289nm.With the increase of the dopant amount, gas permeability of the prepared membranes increases. Results also indicate the permeability of prepaerd membranes is affected significantly by the pyrolysis temperature. When the temperature is above 700℃, the gas permeability exhibites a drastic drop, while the selectivity decreases seriously.The performance is also influenced by permeating temperature, not related to feed pressure. The functional membrane prepared with nano-charcoal powders improves the CO2 permeability more or less, but has little effect on other gases. Compared with nano-charcoal powders, incorporating nano-charcoal raw powders enhances the gas permeability a little,while the slectivy has no change. The prepared composite functional memebranes dopped with MWNT exhibit high CO2 peameability and selectivity.
As a result, membranes with high CO2 permeaselecticity can be prepared through controlling the doping agents, amount and conditions of carbonization.
引文
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