氨基功能化多孔氧化硅材料合成及其CO_2吸附性能研究
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摘要
众所周知,由于人类排放至大气中的CO2数量不断增加且CO2与气候变化密切相关,因此CO2的排放引起了世人的高度关注。本文以氨基功能化SBA-15和以阴离子表面活性剂为模板剂合成氨基功能化多孔氧化硅(AFPS)为研究体系,主要采用优化实验条件(如pH值、陈化温度、阴离子类型等)方式,提高室温和常压下氨基功能化多孔氧化硅的CO2吸附量。同时,还利用(原位)红外、N2吸-脱附、元素分析、SEM、TG-DTA、TPD、XRD和TEM等技术对合成的多孔氧化硅进行了表征。本文的主要研究内容和结果如下：(1)氨基功能化SBA-15的直接合成及其CO2吸附性能。
通过直接法合成了氨基功能化的介孔氧化硅材料。实验结果表明,当合成体系中APTES(氨丙基三乙氧基硅烷)与(APTES+TEOS)的摩尔比小于0.20或APTMS(氨丙基三甲氧基硅烷)与(APTMS+TEOS)的摩尔比小于0.10时,所合成的材料均具有SBA-15介孔结构。由于氨基对SBA-15结构的形成产生副作用,当上述两比值分别大于0.20和0.10时,介孔结构将会坍塌。但是,引入F-后,即使上述两比值达到0.25和0.30时,所合成的材料仍具有有序的介孔结构,且材料的孔容和比表面积较高。CO2吸附实验表明,随着反应体系中氨基功能化物质(APTES或APTMS)含量增加,所合成的材料吸附CO2的能力提高；在F-辅助下合成的材料吸附CO2的能力远远高于无F-辅助下合成材料的。(2)表面羟基高密度化SBA-15的合成、氨基功能化及其CO2吸附性能。
在HCl溶液中引入HAc后,由于Ac-可降低硅羟基的水解与聚合反应,因此可合成表面羟基高密度化的SBA-15材料。通过填充TEPA(tetraethylenepentamine)可获得氨基功能化SBA-15(AF-SBA-15)材料。实验表明,当TEPA与SBA-15的质量比(x)小于0.6时,所获得的AF-SBA-15均具有与纯SBA-15一样的结构。CO2吸附实验说明,当x为0.1时,随着吸附温度升高,AF-SBA-15对CO2的吸附能力降低；当x为0.6时,随着吸附温度升高,AF-SBA-15对CO2的吸附能力增加。
(3)萃取方式、陈化温度、pH值和反应物组成等对以阴离子表面活性剂为模板剂合成氨基功能化多孔氧化硅吸附CO2的影响。
分别以十二烷基肌氨酸钠(Sar-Na)、APTMS和TEOS为结构导向剂(SDA)、共结构导向剂(CSDA)和硅源合成了氨基功能化介孔氧化硅预产物。分别用乙醇-乙醇胺和盐酸-乙睛混合液萃取预产物中的模板剂。研究表明,乙醇-乙醇胺的萃取效果好于盐酸-乙晴的,且萃取后获得的材料对CO2的吸附能力优于由盐酸-乙睛萃取后获得材料的。
从元素分析和TEM表征结果可知,陈化温度和pH值对介孔材料内氨基含量影响较大。当在较低的陈化温度和相对较低的pH值下,所合成材料对CO2的吸附量较高。
CO2吸附实验表明,在以阴离子表面活性剂为模板剂合成介孔氧化硅中,APTMS与TEOS的比值对合成材料的C02吸附性能起重要作用。当加入0.6 ml APTMS和3.0 mlTEOS至含39 ml HCl (0.1 mol/1),70 ml H2O和1.76 g Sar-Na的混合溶液中时,所合成材料的CO2吸附能力优于其它条件下(如加入0.3 ml的APTMS和3.0 ml的TEOS至含13 mlHCl (0.1 mol/1),70ml H2O和0.59 g的Sar-Na昆合溶液中)合成材料的。
(4)以月桂酸为模板剂合成氨基功能化多孔氧化硅及其CO2吸附性能。
分别使用月桂酸为SDA、APTMS为CSDA、TEOS为硅源,采用溶胶-凝胶法,通过乙醇胺-乙醇体系萃取模板剂后,合成了氨基功能化多孔氧化硅。CO2吸附实验表明,随着反应体系中APTMS含量提高,所合成材料对CO2的吸附能力不断提高；但当APTMS与月桂酸体积比大于2.2：3.0时,随着APTMS含量提高,所合成材料对CO2的吸附量降低。此外,通过调查甲醇、乙醇、丙醇和正丁醇等对吸附剂的CO2吸附性能影响时表明,使用乙醇为共溶剂合成的材料对CO2的吸附效果最好。
It is well known that carbon dioxide (CO2) has become an important global issue due to the significant and continuous rise in anthropic CO2 emissions to the atmosphere and their connection with global climate change. Two kinds of amino-functionalized porous silicas (AFPS), i.e. amino-functionalized SBA-15 and porous silicas templated by anionic surfactants, have been studied in this dissertation. To improve adsorption capacity of CO2 on the AFPS at ambient temperature and atmospheric pressure, this study has been focused on investigating the effects of experimental conditions such as pH value, aging temperature, types of anionic surfactant etc., on AFPS adsorption properties for CO2. Inherently, the synthesized porous silicas have been characterized by the FT-IR, in-situ FT-IR, N2 adsorption-desorption, elemental analysis, SEM, TG-DTA, TPD, XRD, and TEM techniques. The obtained results are summarized as follows:
(1) One-pot synthesis of amino-functionalized SBA-15 and their CO2-adsorption properties.
Amino-functionalized SBA-15 mesoporous materials were synthesized by a one-pot strategy. The characterized results show that all the obtained materials have a typical meso-SBA-15 structure when the molar ratios of APTES to (APTES+TEOS) in the synthetic solutions are below 0.20 or the molar ratios of APTMS to (APTMS+TEOS) in the synthetic solutions are below 0.10, while the meso-structure could be collapsed when these ratios are more than the corresponding values (0.20 or 0.10) because of the adverse effect of amino groups on the formation of SBA-15. However, with the aid of fluoride ions, even at a molar ratio of APTES to (APTES+TEOS) of 0.25 or a molar ratio of APTMS to (APTMS+TEOS) of 0.30, the amino-functionalized SBA-15 mesoporous material with a larger pore size and a higher BET surface area could be synthesized. The results from CO2 adsorption on the synthesized amino-functionalized SBA-15 mesoporous materials show that under the same conditions the adsorbed amount of CO2 increases with increasing the APTES (APTMS) amount in the synthetic solution and the amino-functionalized SBA-15 mesoporous material synthesized with the aid of fluoride ions has a higher amount adsorbed for CO2 adsorption at 101 kPa and 25℃, compared to those prepared without introduction of fluoride ions.
(2) Synthesis, amino-functionalization of SBA-15 with a high Si-OH density and their C02-adsorption properties.
SBA-15 materials with a high Si-OH density have been successfully prepared by adding HAc solution into HCl solution, because Ac- can slow down the hydrolysis-condensation reaction of silica alkoxides. The amino-functionalized SBA-15 (AF-SBA-15) materials have been obtained via tetraethylenepentamine (TEPA) loaded onto the SBA-15 with a high Si-OH density. The experimental results show that when the mass ratios of TEPA to SBA-15 are below 0.6, the structure of AF-SBA-15 are identical to that of pure SBA-15. When the mass ratio of TEPA to SBA-15 is 0.1, the adsorption capacity of CO2 on the prepared AF-SBA-15 decreases with increasing temperature, while when the mass ratio of TEPA to SBA-15 is 0.6, the adsorption capacity of CO2 on the synthesized AF-SBA-15 increases with increasing temperature.
(3) Effects of extractive method, aging temperature, pH value and and reactant composition on the adsorption properties of CO2 over the amino-functionalized porous silicas templeted by anion surfactants.
Using N-lauroylsarcosine sodium (Sar-Na),3-aminopropyltrimethoxysilane (APTMS) and TEOS as structure-directing agent (SDA), co-structure-directing agent (CSDA) and silicon source, respectively, the pre-products of amino-functionalized mesoporous silicas have been prepared by a sol-gel method. The template in the pre-products can be efficiently removed by extraction either using a basic solution of monoethanol amine (MEA) in ethanol or an acetonitrile solution acidified with HCl. The experimental results indicate that, when compared to the adsorbent treated with acidic acetonitrile, the adsorbent treated with the MEA-ethanol solution has a much higher adsorption capacity towards CO2, exhibits a higher degree of reversibility in the adsorption process, and has a much higher CO2/N2 selectivity.
The results from both elemental analysis and TEM characterizations show that the amount of amino groups inside the mesoporous materials is greatly controlled by the aging temperature and pH value of the synthetic solution. The adsorption of CO2 on the synthesized materials implies that the low aging temperature and relatively low pH value of the synthetic solution would be benefit to enhance the adsorbed amount of CO2 on the resulted materials.
The results from CO2 adsorption on the amino-functionalized mesoporous silicas templeted by anion surfactants also show that the ratio of APTMS to TEOS is a key parameter that affects the CO2 adsorption capacity. When a miture of 0.6 ml APTMS and 3.0 ml TEOS is added into a solution containing 39 ml HCl(0.1 mol/l),70 ml H2O and 1.76 g Sar-Na, the synthesized adsorbent exhibites a much higher CO2 adsorption capacity, compared to those synthesized under other conditions, for example, a mixture of 0.3 ml APTMS and 3.0 ml TEOS added into a solution containing 13 ml HCl (0.1 mol/1),70 ml H2O and 0.59 g Sar-Na.
(4) Preparation of amino-functionalized porous silicas templeted by dodecanoic acid and their CO2-adsorption properties.
Using dodecanoic acid (DAA), APTMS and TEOS as SDA, CSDA, and silicon source, respectively, the pre-products of amino-functionalized mesoporous silicas have been prepared by a sol-gel method. The template in the pre-products can be efficiently removed by extraction using a basic solution of MEA in ethanol. The results from CO2 adsorption show that, when the content of APTMS in the synthetic system is increased, the adsorption capacity of CO2 adsorption on the synthesized adsorbent is increased as well. However, when the volume ratio of APTMS to DAA is above 2.2:3.0, the adsorption capacity of CO2 decreases with increasing the content of APTMS. Additionally, a systematic investigation on the effects of the use of alcohols, such as methanol, ethanol, propanol, and butanol, on the adsorption properties of CO2 on the resulted adsorbents indicates that the adsorbent synthesized by the use of ethanol has the highest adsorption capacity towards CO2.
通过直接法合成了氨基功能化的介孔氧化硅材料。实验结果表明,当合成体系中APTES(氨丙基三乙氧基硅烷)与(APTES+TEOS)的摩尔比小于0.20或APTMS(氨丙基三甲氧基硅烷)与(APTMS+TEOS)的摩尔比小于0.10时,所合成的材料均具有SBA-15介孔结构。由于氨基对SBA-15结构的形成产生副作用,当上述两比值分别大于0.20和0.10时,介孔结构将会坍塌。但是,引入F-后,即使上述两比值达到0.25和0.30时,所合成的材料仍具有有序的介孔结构,且材料的孔容和比表面积较高。CO2吸附实验表明,随着反应体系中氨基功能化物质(APTES或APTMS)含量增加,所合成的材料吸附CO2的能力提高；在F-辅助下合成的材料吸附CO2的能力远远高于无F-辅助下合成材料的。(2)表面羟基高密度化SBA-15的合成、氨基功能化及其CO2吸附性能。
在HCl溶液中引入HAc后,由于Ac-可降低硅羟基的水解与聚合反应,因此可合成表面羟基高密度化的SBA-15材料。通过填充TEPA(tetraethylenepentamine)可获得氨基功能化SBA-15(AF-SBA-15)材料。实验表明,当TEPA与SBA-15的质量比(x)小于0.6时,所获得的AF-SBA-15均具有与纯SBA-15一样的结构。CO2吸附实验说明,当x为0.1时,随着吸附温度升高,AF-SBA-15对CO2的吸附能力降低；当x为0.6时,随着吸附温度升高,AF-SBA-15对CO2的吸附能力增加。
(3)萃取方式、陈化温度、pH值和反应物组成等对以阴离子表面活性剂为模板剂合成氨基功能化多孔氧化硅吸附CO2的影响。
分别以十二烷基肌氨酸钠(Sar-Na)、APTMS和TEOS为结构导向剂(SDA)、共结构导向剂(CSDA)和硅源合成了氨基功能化介孔氧化硅预产物。分别用乙醇-乙醇胺和盐酸-乙睛混合液萃取预产物中的模板剂。研究表明,乙醇-乙醇胺的萃取效果好于盐酸-乙晴的,且萃取后获得的材料对CO2的吸附能力优于由盐酸-乙睛萃取后获得材料的。
从元素分析和TEM表征结果可知,陈化温度和pH值对介孔材料内氨基含量影响较大。当在较低的陈化温度和相对较低的pH值下,所合成材料对CO2的吸附量较高。
CO2吸附实验表明,在以阴离子表面活性剂为模板剂合成介孔氧化硅中,APTMS与TEOS的比值对合成材料的C02吸附性能起重要作用。当加入0.6 ml APTMS和3.0 mlTEOS至含39 ml HCl (0.1 mol/1),70 ml H2O和1.76 g Sar-Na的混合溶液中时,所合成材料的CO2吸附能力优于其它条件下(如加入0.3 ml的APTMS和3.0 ml的TEOS至含13 mlHCl (0.1 mol/1),70ml H2O和0.59 g的Sar-Na昆合溶液中)合成材料的。
(4)以月桂酸为模板剂合成氨基功能化多孔氧化硅及其CO2吸附性能。
分别使用月桂酸为SDA、APTMS为CSDA、TEOS为硅源,采用溶胶-凝胶法,通过乙醇胺-乙醇体系萃取模板剂后,合成了氨基功能化多孔氧化硅。CO2吸附实验表明,随着反应体系中APTMS含量提高,所合成材料对CO2的吸附能力不断提高；但当APTMS与月桂酸体积比大于2.2：3.0时,随着APTMS含量提高,所合成材料对CO2的吸附量降低。此外,通过调查甲醇、乙醇、丙醇和正丁醇等对吸附剂的CO2吸附性能影响时表明,使用乙醇为共溶剂合成的材料对CO2的吸附效果最好。
It is well known that carbon dioxide (CO2) has become an important global issue due to the significant and continuous rise in anthropic CO2 emissions to the atmosphere and their connection with global climate change. Two kinds of amino-functionalized porous silicas (AFPS), i.e. amino-functionalized SBA-15 and porous silicas templated by anionic surfactants, have been studied in this dissertation. To improve adsorption capacity of CO2 on the AFPS at ambient temperature and atmospheric pressure, this study has been focused on investigating the effects of experimental conditions such as pH value, aging temperature, types of anionic surfactant etc., on AFPS adsorption properties for CO2. Inherently, the synthesized porous silicas have been characterized by the FT-IR, in-situ FT-IR, N2 adsorption-desorption, elemental analysis, SEM, TG-DTA, TPD, XRD, and TEM techniques. The obtained results are summarized as follows:
(1) One-pot synthesis of amino-functionalized SBA-15 and their CO2-adsorption properties.
Amino-functionalized SBA-15 mesoporous materials were synthesized by a one-pot strategy. The characterized results show that all the obtained materials have a typical meso-SBA-15 structure when the molar ratios of APTES to (APTES+TEOS) in the synthetic solutions are below 0.20 or the molar ratios of APTMS to (APTMS+TEOS) in the synthetic solutions are below 0.10, while the meso-structure could be collapsed when these ratios are more than the corresponding values (0.20 or 0.10) because of the adverse effect of amino groups on the formation of SBA-15. However, with the aid of fluoride ions, even at a molar ratio of APTES to (APTES+TEOS) of 0.25 or a molar ratio of APTMS to (APTMS+TEOS) of 0.30, the amino-functionalized SBA-15 mesoporous material with a larger pore size and a higher BET surface area could be synthesized. The results from CO2 adsorption on the synthesized amino-functionalized SBA-15 mesoporous materials show that under the same conditions the adsorbed amount of CO2 increases with increasing the APTES (APTMS) amount in the synthetic solution and the amino-functionalized SBA-15 mesoporous material synthesized with the aid of fluoride ions has a higher amount adsorbed for CO2 adsorption at 101 kPa and 25℃, compared to those prepared without introduction of fluoride ions.
(2) Synthesis, amino-functionalization of SBA-15 with a high Si-OH density and their C02-adsorption properties.
SBA-15 materials with a high Si-OH density have been successfully prepared by adding HAc solution into HCl solution, because Ac- can slow down the hydrolysis-condensation reaction of silica alkoxides. The amino-functionalized SBA-15 (AF-SBA-15) materials have been obtained via tetraethylenepentamine (TEPA) loaded onto the SBA-15 with a high Si-OH density. The experimental results show that when the mass ratios of TEPA to SBA-15 are below 0.6, the structure of AF-SBA-15 are identical to that of pure SBA-15. When the mass ratio of TEPA to SBA-15 is 0.1, the adsorption capacity of CO2 on the prepared AF-SBA-15 decreases with increasing temperature, while when the mass ratio of TEPA to SBA-15 is 0.6, the adsorption capacity of CO2 on the synthesized AF-SBA-15 increases with increasing temperature.
(3) Effects of extractive method, aging temperature, pH value and and reactant composition on the adsorption properties of CO2 over the amino-functionalized porous silicas templeted by anion surfactants.
Using N-lauroylsarcosine sodium (Sar-Na),3-aminopropyltrimethoxysilane (APTMS) and TEOS as structure-directing agent (SDA), co-structure-directing agent (CSDA) and silicon source, respectively, the pre-products of amino-functionalized mesoporous silicas have been prepared by a sol-gel method. The template in the pre-products can be efficiently removed by extraction either using a basic solution of monoethanol amine (MEA) in ethanol or an acetonitrile solution acidified with HCl. The experimental results indicate that, when compared to the adsorbent treated with acidic acetonitrile, the adsorbent treated with the MEA-ethanol solution has a much higher adsorption capacity towards CO2, exhibits a higher degree of reversibility in the adsorption process, and has a much higher CO2/N2 selectivity.
The results from both elemental analysis and TEM characterizations show that the amount of amino groups inside the mesoporous materials is greatly controlled by the aging temperature and pH value of the synthetic solution. The adsorption of CO2 on the synthesized materials implies that the low aging temperature and relatively low pH value of the synthetic solution would be benefit to enhance the adsorbed amount of CO2 on the resulted materials.
The results from CO2 adsorption on the amino-functionalized mesoporous silicas templeted by anion surfactants also show that the ratio of APTMS to TEOS is a key parameter that affects the CO2 adsorption capacity. When a miture of 0.6 ml APTMS and 3.0 ml TEOS is added into a solution containing 39 ml HCl(0.1 mol/l),70 ml H2O and 1.76 g Sar-Na, the synthesized adsorbent exhibites a much higher CO2 adsorption capacity, compared to those synthesized under other conditions, for example, a mixture of 0.3 ml APTMS and 3.0 ml TEOS added into a solution containing 13 ml HCl (0.1 mol/1),70 ml H2O and 0.59 g Sar-Na.
(4) Preparation of amino-functionalized porous silicas templeted by dodecanoic acid and their CO2-adsorption properties.
Using dodecanoic acid (DAA), APTMS and TEOS as SDA, CSDA, and silicon source, respectively, the pre-products of amino-functionalized mesoporous silicas have been prepared by a sol-gel method. The template in the pre-products can be efficiently removed by extraction using a basic solution of MEA in ethanol. The results from CO2 adsorption show that, when the content of APTMS in the synthetic system is increased, the adsorption capacity of CO2 adsorption on the synthesized adsorbent is increased as well. However, when the volume ratio of APTMS to DAA is above 2.2:3.0, the adsorption capacity of CO2 decreases with increasing the content of APTMS. Additionally, a systematic investigation on the effects of the use of alcohols, such as methanol, ethanol, propanol, and butanol, on the adsorption properties of CO2 on the resulted adsorbents indicates that the adsorbent synthesized by the use of ethanol has the highest adsorption capacity towards CO2.
引文
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