天然高分子基有机及碳气凝胶的制备、结构和性质研究
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摘要
本论文主要探讨利用溶胶-凝胶方法制备具有纳米多孔结构的天然高分子基有机气凝胶及碳气凝胶,并对其微观结构和性质进行了研究。内容包括气凝胶的制备过程、微观结构的表征和制备条件的选择,研究了天然高分子基有机气凝胶及碳气凝胶的对一些常见的水污染物,例如表面活性剂、阴离子染料和阳离子染料的吸附性质。探讨了天然高分子基有机气凝胶及碳气凝胶的形成机理,丰富和发展了的有机气凝胶和碳气凝胶制备的理论和方法。
1.壳聚糖基气凝胶的制备和吸附性质研究
以天然高分子甲壳素的脱乙酰基产物壳聚糖为原料,分别以甲醛、乙二醛、戊二醛为交联剂制备了水凝胶,进一步通过溶剂交换和超临界CO_2干燥,首次成功合成了交联的高比表面积的壳聚糖基气凝胶。本研究选用自然界储量丰富,具有良好生物相容性,价格低廉的壳聚糖为前驱体,首先将不同质量的壳聚糖溶解在1%(v/v)的醋酸溶液中,磁力搅拌10 h以上,使其最大限度完全溶解,过滤除去少量不溶物。然后配制不同浓度的甲醛,乙二醛,戊二醛水溶液,在剧烈搅拌下将交联剂溶液倒入壳聚糖溶液中,一直剧烈搅拌至胶体粘度变大,磁子搅拌不动,取出磁子。密封条件下凝胶老化24 h,然后用无水乙醇交换溶剂得到醇凝胶。将醇凝胶用超临界CO_2进行干燥,得到块状的气凝胶。壳聚糖/甲醛气凝胶的最大比表面积为845 m~2/g,相应的最可几孔径为9.28 nm;壳聚糖/乙二醛气凝胶的最大比表面积为707 m~2/g,相应的最可几孔径为5.38 nm;壳聚糖/戊二醛气凝胶的最大比表面积为569 m~2/g,相应的最可几孔径为4.59 nm。壳聚糖的浓度和交联剂的浓度和种类都对气凝胶的质构产生明显的影响。三种气凝胶的表面在pH＜10条件下都带有正电荷。通过研究三种气凝胶对阴离子表面活性剂十二烷基苯磺酸钠(SDBS)的吸附表明,在pH=3条件下,壳聚糖基气凝胶对十二烷基苯磺酸钠有较大的吸附量,得益于此酸度条件下三种气凝胶均带有高的正电荷。同时,在0.1 M的NaOH溶液中,约97%的吸附的SDBS发生脱附。经过十次重复使用后,吸附量仍能达到最大吸附量的90%。对于去除废水中SDBS的污染提供了新的思路和解决方案。
2.高比表面积淀粉基有机及碳气凝胶的制备和吸附性质研究
以天然高分子淀粉制备的可溶性淀粉为原料,通过常压干燥,制备了淀粉气凝胶,然后在N_2保护下,高温裂解制备了淀粉基碳气凝胶。将一定量的可溶性淀粉加入到去离子水中,在磁力搅拌条件下将悬浮液加热至90℃以上,直至形成半透明溶胶。冷却至室温,得到白色水凝胶。用无水丙酮交换溶剂,得到白色酮凝胶。在50℃条件下常压干燥得到白色淀粉气凝胶。将淀粉气凝胶放入管式炉中,在N_2流中,温度以5℃/min分别升至800℃、810℃、830℃、850℃、870℃和900℃,使淀粉气凝胶发生分解碳化得到碳气凝胶。在通N_2情况下冷却至室温,然后通入CO_2,温度升至800℃,保温不同时间,降至室温,得到活化碳气凝胶。实验结果发现,碳化温度和活化时间对碳气凝胶的质构性质有重要影响。当碳化温度为850℃,CO_2活化时间为7 h时,得到的活化后的碳气凝胶的具有最大的比表面积,达到了1571 m~2/g。当活化时间低于7 h时,随着活化时间的延长,比表面积逐渐增大。而活化时间高于7 h,比表面积开始减小。Zeta电势测定表明,活化碳气凝胶在水溶液中的等电点时pH=5.2,当pH＞5.2时,随着pH的升高,活化碳气凝胶的表面负电荷逐渐增加。而当pH＜5.2时,随着pH值的降低,活化碳气凝胶的表面正电荷逐渐增加。实验测定了活化碳气凝胶对三种阳离子染料结晶紫,甲基紫和亚甲基蓝的的吸附性质,pH=10时,对三种染料的吸附量最大,分别达到了1515,1423和1181 mg/g。实验发现,吸附的染料在无水乙醇中,99%以上发生脱附。经过9次循环吸附/脱附过程,仍能保持90%以上的吸附量。
3.天然产物京尼平为交联剂的壳聚糖/明胶基气凝胶的制备和吸附性质
以天然产物京尼平为交联剂,以天然高分子甲壳素的脱乙酰基产物壳聚糖和来源于胶原蛋白的明胶为原料,通过溶胶—凝胶过程和超临界CO_2干燥,成功制备了壳聚糖/京尼平气凝胶,壳聚糖/明胶/京尼平气凝胶。首先将2 g壳聚糖溶解在100 mL 1%(v/v)醋酸水溶液中,磁力搅拌10 h以上使其完全溶解,过滤除去少量不溶物。分别加入0.5%,1.0%,1.5%,2%,2.5%(wt%)的京尼平,60℃条件下磁力搅拌1 h,溶液由透明的珍珠白色逐渐变为墨绿色,停止搅拌,密封,静置,胶凝时间约为5-7 h。湿凝胶在密封条件下老化24-72 h,直至形成弹性凝胶,然后用无水乙醇交换溶剂,最后通过超临界CO_2干燥得到壳聚糖/京尼平气凝胶。类似的过程制备壳聚糖/明胶/京尼平气凝胶。壳聚糖和明胶的质量比设定为1:2,1:1,2:1,京尼平的质量百分比设定为0.5%,3%。对于壳聚糖/京尼平气凝胶,壳聚糖的浓度和京尼平的浓度都对气凝胶的质构产生影响。其中1%的京尼平和2%的壳聚糖得到的气凝胶具有最大的比表面积567 m~2/g,最可几孔径为10.2 nm。对于壳聚糖/明胶/京尼平气凝胶,随着京尼平含量增加,交联度增大,孔径变小,比表面积增大,最大比表面积为563 m~2/g,相应的最可几孔径为19 nm。SEM表明气凝胶由纤维状网络结构组成。测定了气凝胶对阴离子染料日落黄和柠檬黄的吸附性质。pH=3时,对日落黄和柠檬黄的最大吸附量分别为1149 mg/g和975 mg/g,均优于文献报道值。同时,在0.05 M的NaOH溶液中,吸附的染料首次脱附率达到了98%,5次循环吸附—脱附后,仍能达到最大吸附量的95%以上。
4.卡拉胶基有机及碳气凝胶的制备和吸附性质研究
以天然高分子卡拉胶为原料,通过冷冻干燥和超临界CO_2干燥,以及高温碳化,制备了相应的碳气凝胶。分别将1.5 g、2.5 g、3.5 g和4.5 g卡拉胶溶液在100 mL去离子水中,在磁力搅拌下升温至沸腾,得到半透明银白色溶胶。停止搅拌,冷却至室温,得到半透明银白色水凝胶。将水凝胶直接进行冷冻干燥,得到相应的冷冻气凝胶(cryogels)。用无水乙醇交换水凝胶中的溶剂,得到醇凝胶(alcogels),然后将醇凝胶进行CO_2超临界干燥得到超临界干燥气凝胶(aerogels)。然后将两种方法制备的气凝胶在管式炉中,在N_2保护下进行高温碳化,制备了相应的碳气凝胶。结果发现两种方法制备的碳气凝胶具有接近的比表面积和孔径分布,最可几孔径均为3.9 nm,1000℃条件下碳化的比表面积达到了1185 m~2/g。实验发现,卡拉胶基碳气凝胶对阳离子染料甲基紫和结晶紫有优异的吸附性能,温度从25℃升高到45℃,吸附量逐步增大,最大吸附量分别达到了1725 mg/g和2207 mg/g。并且被吸附的染料在无水乙醇中95%以上会发生脱附,碳气凝胶被重复利用5次,吸附量仍能达到最大吸附量的90%。
The nanostructured natural polymers based organic and carbon aerogels were synthesized by a sol-gel technique.The preparation process and the microstructures of aerogels were studied,and the effects of preparation parameters,as well as the adsorption properties of the prepared aerogels were investigated.Based on the experiments,the formation mechanisms of the natural polymers based aerogels and their carbon aerogels were proposed. This study enriched the basic theory and applications of organic aerogels and carbon aerogels prepared on the basis of the sol-gel process.
1.Chitosan-based aerogels with high adsorption performance
New natural polymer-based aerogels,cross-linked chitosan-based aerogels, were prepared by the sol-gel route with glutaradehyde,glyoxal,and formaldehyde as cross-linkers.The alcogels were dried by supercritical carbon dioxide(CO_2) fluid extraction.The resulting materials were characterized using scanning electron microscopy(SEM),nitrogen adsorption/desorption analysis,and Fourier transform infrared(FT-IR) spectroscopy.The Brunauer-Emmett-Teller(BET) analyses indicate that the largest surface areas for the chitosan-glutaraldehyde/-glyoxal and -formaldehyde aerogels are 569,707,and 845 m~2/g,respectively.We believe that the N_2 adsorption-desorption hysteresis is a permanent type.Every aerogel sample was tested for 3 times repeatedly for the N_2 adsorption-desorption experiment;the adsorption-desorption hysteresis curves and the PSD curves are same.This indicates the mesopores are stable.IR spectra of chitosan and cross-linked chitosan-based aerogels indicate that the primary amine peak at 1653 cm~(-1) decreased as the chitosan was crosslinked, while a new peak for C=N amine appeared at 1653-1656 cm~(-1).The peak at 1602 cm~(-1) disappeared in the aerogels due to the loss of free amines, indicating a Schiff-base amine functionality.The key factor to obtaining stable aerogels with a high specific surface area is the full replacement of the solvent with absolute ethanol.If the solvent is not fully replaced by absolute ethanol,only a broken wet-gel will be produced.The decomposition of the chitosan-based aerogel is observed from ca.220 to 450℃,and the profiles of the TG curves for both non-cross-linked and cross-linked materials are similar. It was also found that carbon aerogels could not be produced after calcining the chitosanbased aerogels under a flow of nitrogen because the thermal degradation of the main chains in chitosan and chitosan-based aerogels during heating destroyed the network structure.Furthermore,the adsorption of the anionic surfactant sodium dodecylbenzene-sulfonate(SDBS) from aqueous solution by the materials was investigated.The aerogels exhibit high adsorption capability,can remove SDBS from acidic aqueous solutions,and have potential applications in controlling SDBS pollution.
2.Starch derived carbon aerogels with high-performance for sorption of cationic dyes
A synthetic strategy to prepare CAs by the carbonization of starch aerogels from its corresponding wet-gels through the ambient pressure drying process. The textural characteristics of CAs could be tailored by adjusting the carbonization temperature and activation time.Thus the technique of CA synthesis is relatively simple and with low cost for the short gelation time and ambient pressure drying.To prepare CAs,the esculent and soluble starch was dissolved into water to form the wet-gels,after the water in the gels was exchanged by acetone,the acetone gels were dried at ambient pressure to obtain the white starch aerogels,which were carbonized in N_2 flow.SEM images show that the starch aerogels exhibit a fibrillar solid network with a diameter of 30-40 nm and CAs consist of flakes with a side-length of 60-120μm as the starch aerogels were carbonized at 850℃for 2.0 h.When the magnification is 200,the carbon aerogels keep the same shape after activating with CO_2.SEM image of ACAs show high mesoporosity,obviously. However,SEM image of CAs don't show mesoporous structure.The N_2 adsorption measurements indicate that the specific surface area of CAs is 137 m~2/g and the average pore size is 1.54 nm,only few mesopores are observed according to the BET pore size distribution(PSD).However,the specific surface areas of starch aerogel(calculated using BET model) was 103 m~2/g and PSD ranged from 3 nm to 80 nm,typical of mesoporous and macroporous solids.Further experiments show that the suitable activation conditions could increase the specific surface areas and pore volume of CAs,which increased with the activate time prolonging.After activations the CAs contained both micropores and mesopores,its average micropore size is 0.89 nm,and all the mesopore size are in the range of 2-10 nm whatever the activation time is, which reveals that the activation process creates new micropore and mesopore structures.For example,the largest specific surface areas of CAs increased to 1571 m~2/g after being activated at 800℃for 7.0 h under CO_2 flow.The pH value of solution considerably affected the adsorption amounts of basic dyes on the CAs.For example,as the pH value of dye solution is 10 and dye's solution is 500 ppm,the absorption amount is the largest,those for CV,MV and MB are respectively 1515,1423 and 1181 mg/g.
3.Synthesis,characterization and application of chitosan/gelatin/genipin aerogels
New natural polymer-based aerogels,cross-linked chitosan aerogels and chitosan-gelatin aerogels,were prepared by the sol-gel route with genipin as cross-linkers.The alcogels were dried by supercritical carbon dioxide(CO_2) fluid extraction.The resulting materials were characterized using scanning electron microscopy(SEM),nitrogen adsorption/desorption analysis.The Brunauer-Emmett-Teller(BET) analyses indicate that the largest surface areas for the natural polymers based aerogels are 567 m~2/g.The key factor to obtaining stable aerogels with a high specific surface areas is the full replacement of the solvent with absolute ethanol.If the solvent is not fully replaced by absolute ethanol,only a broken wet-gel will be produced.It was also found that carbon aerogels could not be produced after calcining the chitosan based aerogels under a flow of nitrogen because the thermal degradation of the main chains in chitosan and chitosan-based aerogels during heating destroyed the network structure.Furthermore,the adsorption of the anionic dyes sunset yellow and tartrazine from aqueous solution by the materials was investigated.The aerogels exhibit high adsorption capability, can remove sunset yellow and tartrazine from acidic aqueous solutions,and have potential applications in controlling anionic dyes pollution.
4.Synthesis,characterization and application of carrageenan based organic and carbon aerogels
Carrageenan based organic cyrogels and aerogels were prepared by the sol-gel route and freeze drying and supercritical carbon dioxide(CO_2) drying from its corresponding wet-gels,and carrageenan based carbon aerogels and cyrogels were prepared by the carbonization of carrageenan aerogels and cyrogels,respectively.The textural characteristics of carrageenan based carbon aerogels and cyrogels could be tailored by change dry method.Thus the technique of CA synthesis is relatively simple and with low cost for the short gelation time and freeze drying.To prepare CAs,the esculent and soluble carrageenan was dissolved into water to form the wet-gels,after the water in the gels was exchanged by alcohol,the alcogels were dried at supercritical carbon dioxide(CO_2) or freeeze to obtain the white carrageenan aerogels and cyrogels,which were carbonized in N_2 flow at 1000℃.SEM images show that the carrageenan aerogeis exhibit a fibrillar solid network with a diameter of 20 nm and carbon aerogels and cyrogels consist of carbon particles.SEM image of aerogels and cyrogels show high mesoporosity, obviously.However,SEM image of carbon aerogels don't show microporous structure.The N_2 adsorption measurements indicate that the largest specific surface area of organic aerogels is 346 m~2/g and the average pore size is 2.98 nm.However,the specific surface area of carbon cyrogels(calculated using BET model) was 1185 m~2/g and the average pore size are 0.85 and 3.9,typical of mesoporous and microporous solids.The pH value of solution considerably affected the adsorption amounts of basic dyes on the CAs.For example,as the pH value of dye solution is 10 and dye's solution is 500 ppm,the absorption amount is the largest,those for CV,MV are respectively 2207,1725 mg/g at pH 10.
1.壳聚糖基气凝胶的制备和吸附性质研究
以天然高分子甲壳素的脱乙酰基产物壳聚糖为原料,分别以甲醛、乙二醛、戊二醛为交联剂制备了水凝胶,进一步通过溶剂交换和超临界CO_2干燥,首次成功合成了交联的高比表面积的壳聚糖基气凝胶。本研究选用自然界储量丰富,具有良好生物相容性,价格低廉的壳聚糖为前驱体,首先将不同质量的壳聚糖溶解在1%(v/v)的醋酸溶液中,磁力搅拌10 h以上,使其最大限度完全溶解,过滤除去少量不溶物。然后配制不同浓度的甲醛,乙二醛,戊二醛水溶液,在剧烈搅拌下将交联剂溶液倒入壳聚糖溶液中,一直剧烈搅拌至胶体粘度变大,磁子搅拌不动,取出磁子。密封条件下凝胶老化24 h,然后用无水乙醇交换溶剂得到醇凝胶。将醇凝胶用超临界CO_2进行干燥,得到块状的气凝胶。壳聚糖/甲醛气凝胶的最大比表面积为845 m~2/g,相应的最可几孔径为9.28 nm;壳聚糖/乙二醛气凝胶的最大比表面积为707 m~2/g,相应的最可几孔径为5.38 nm;壳聚糖/戊二醛气凝胶的最大比表面积为569 m~2/g,相应的最可几孔径为4.59 nm。壳聚糖的浓度和交联剂的浓度和种类都对气凝胶的质构产生明显的影响。三种气凝胶的表面在pH＜10条件下都带有正电荷。通过研究三种气凝胶对阴离子表面活性剂十二烷基苯磺酸钠(SDBS)的吸附表明,在pH=3条件下,壳聚糖基气凝胶对十二烷基苯磺酸钠有较大的吸附量,得益于此酸度条件下三种气凝胶均带有高的正电荷。同时,在0.1 M的NaOH溶液中,约97%的吸附的SDBS发生脱附。经过十次重复使用后,吸附量仍能达到最大吸附量的90%。对于去除废水中SDBS的污染提供了新的思路和解决方案。
2.高比表面积淀粉基有机及碳气凝胶的制备和吸附性质研究
以天然高分子淀粉制备的可溶性淀粉为原料,通过常压干燥,制备了淀粉气凝胶,然后在N_2保护下,高温裂解制备了淀粉基碳气凝胶。将一定量的可溶性淀粉加入到去离子水中,在磁力搅拌条件下将悬浮液加热至90℃以上,直至形成半透明溶胶。冷却至室温,得到白色水凝胶。用无水丙酮交换溶剂,得到白色酮凝胶。在50℃条件下常压干燥得到白色淀粉气凝胶。将淀粉气凝胶放入管式炉中,在N_2流中,温度以5℃/min分别升至800℃、810℃、830℃、850℃、870℃和900℃,使淀粉气凝胶发生分解碳化得到碳气凝胶。在通N_2情况下冷却至室温,然后通入CO_2,温度升至800℃,保温不同时间,降至室温,得到活化碳气凝胶。实验结果发现,碳化温度和活化时间对碳气凝胶的质构性质有重要影响。当碳化温度为850℃,CO_2活化时间为7 h时,得到的活化后的碳气凝胶的具有最大的比表面积,达到了1571 m~2/g。当活化时间低于7 h时,随着活化时间的延长,比表面积逐渐增大。而活化时间高于7 h,比表面积开始减小。Zeta电势测定表明,活化碳气凝胶在水溶液中的等电点时pH=5.2,当pH＞5.2时,随着pH的升高,活化碳气凝胶的表面负电荷逐渐增加。而当pH＜5.2时,随着pH值的降低,活化碳气凝胶的表面正电荷逐渐增加。实验测定了活化碳气凝胶对三种阳离子染料结晶紫,甲基紫和亚甲基蓝的的吸附性质,pH=10时,对三种染料的吸附量最大,分别达到了1515,1423和1181 mg/g。实验发现,吸附的染料在无水乙醇中,99%以上发生脱附。经过9次循环吸附/脱附过程,仍能保持90%以上的吸附量。
3.天然产物京尼平为交联剂的壳聚糖/明胶基气凝胶的制备和吸附性质
以天然产物京尼平为交联剂,以天然高分子甲壳素的脱乙酰基产物壳聚糖和来源于胶原蛋白的明胶为原料,通过溶胶—凝胶过程和超临界CO_2干燥,成功制备了壳聚糖/京尼平气凝胶,壳聚糖/明胶/京尼平气凝胶。首先将2 g壳聚糖溶解在100 mL 1%(v/v)醋酸水溶液中,磁力搅拌10 h以上使其完全溶解,过滤除去少量不溶物。分别加入0.5%,1.0%,1.5%,2%,2.5%(wt%)的京尼平,60℃条件下磁力搅拌1 h,溶液由透明的珍珠白色逐渐变为墨绿色,停止搅拌,密封,静置,胶凝时间约为5-7 h。湿凝胶在密封条件下老化24-72 h,直至形成弹性凝胶,然后用无水乙醇交换溶剂,最后通过超临界CO_2干燥得到壳聚糖/京尼平气凝胶。类似的过程制备壳聚糖/明胶/京尼平气凝胶。壳聚糖和明胶的质量比设定为1:2,1:1,2:1,京尼平的质量百分比设定为0.5%,3%。对于壳聚糖/京尼平气凝胶,壳聚糖的浓度和京尼平的浓度都对气凝胶的质构产生影响。其中1%的京尼平和2%的壳聚糖得到的气凝胶具有最大的比表面积567 m~2/g,最可几孔径为10.2 nm。对于壳聚糖/明胶/京尼平气凝胶,随着京尼平含量增加,交联度增大,孔径变小,比表面积增大,最大比表面积为563 m~2/g,相应的最可几孔径为19 nm。SEM表明气凝胶由纤维状网络结构组成。测定了气凝胶对阴离子染料日落黄和柠檬黄的吸附性质。pH=3时,对日落黄和柠檬黄的最大吸附量分别为1149 mg/g和975 mg/g,均优于文献报道值。同时,在0.05 M的NaOH溶液中,吸附的染料首次脱附率达到了98%,5次循环吸附—脱附后,仍能达到最大吸附量的95%以上。
4.卡拉胶基有机及碳气凝胶的制备和吸附性质研究
以天然高分子卡拉胶为原料,通过冷冻干燥和超临界CO_2干燥,以及高温碳化,制备了相应的碳气凝胶。分别将1.5 g、2.5 g、3.5 g和4.5 g卡拉胶溶液在100 mL去离子水中,在磁力搅拌下升温至沸腾,得到半透明银白色溶胶。停止搅拌,冷却至室温,得到半透明银白色水凝胶。将水凝胶直接进行冷冻干燥,得到相应的冷冻气凝胶(cryogels)。用无水乙醇交换水凝胶中的溶剂,得到醇凝胶(alcogels),然后将醇凝胶进行CO_2超临界干燥得到超临界干燥气凝胶(aerogels)。然后将两种方法制备的气凝胶在管式炉中,在N_2保护下进行高温碳化,制备了相应的碳气凝胶。结果发现两种方法制备的碳气凝胶具有接近的比表面积和孔径分布,最可几孔径均为3.9 nm,1000℃条件下碳化的比表面积达到了1185 m~2/g。实验发现,卡拉胶基碳气凝胶对阳离子染料甲基紫和结晶紫有优异的吸附性能,温度从25℃升高到45℃,吸附量逐步增大,最大吸附量分别达到了1725 mg/g和2207 mg/g。并且被吸附的染料在无水乙醇中95%以上会发生脱附,碳气凝胶被重复利用5次,吸附量仍能达到最大吸附量的90%。
The nanostructured natural polymers based organic and carbon aerogels were synthesized by a sol-gel technique.The preparation process and the microstructures of aerogels were studied,and the effects of preparation parameters,as well as the adsorption properties of the prepared aerogels were investigated.Based on the experiments,the formation mechanisms of the natural polymers based aerogels and their carbon aerogels were proposed. This study enriched the basic theory and applications of organic aerogels and carbon aerogels prepared on the basis of the sol-gel process.
1.Chitosan-based aerogels with high adsorption performance
New natural polymer-based aerogels,cross-linked chitosan-based aerogels, were prepared by the sol-gel route with glutaradehyde,glyoxal,and formaldehyde as cross-linkers.The alcogels were dried by supercritical carbon dioxide(CO_2) fluid extraction.The resulting materials were characterized using scanning electron microscopy(SEM),nitrogen adsorption/desorption analysis,and Fourier transform infrared(FT-IR) spectroscopy.The Brunauer-Emmett-Teller(BET) analyses indicate that the largest surface areas for the chitosan-glutaraldehyde/-glyoxal and -formaldehyde aerogels are 569,707,and 845 m~2/g,respectively.We believe that the N_2 adsorption-desorption hysteresis is a permanent type.Every aerogel sample was tested for 3 times repeatedly for the N_2 adsorption-desorption experiment;the adsorption-desorption hysteresis curves and the PSD curves are same.This indicates the mesopores are stable.IR spectra of chitosan and cross-linked chitosan-based aerogels indicate that the primary amine peak at 1653 cm~(-1) decreased as the chitosan was crosslinked, while a new peak for C=N amine appeared at 1653-1656 cm~(-1).The peak at 1602 cm~(-1) disappeared in the aerogels due to the loss of free amines, indicating a Schiff-base amine functionality.The key factor to obtaining stable aerogels with a high specific surface area is the full replacement of the solvent with absolute ethanol.If the solvent is not fully replaced by absolute ethanol,only a broken wet-gel will be produced.The decomposition of the chitosan-based aerogel is observed from ca.220 to 450℃,and the profiles of the TG curves for both non-cross-linked and cross-linked materials are similar. It was also found that carbon aerogels could not be produced after calcining the chitosanbased aerogels under a flow of nitrogen because the thermal degradation of the main chains in chitosan and chitosan-based aerogels during heating destroyed the network structure.Furthermore,the adsorption of the anionic surfactant sodium dodecylbenzene-sulfonate(SDBS) from aqueous solution by the materials was investigated.The aerogels exhibit high adsorption capability,can remove SDBS from acidic aqueous solutions,and have potential applications in controlling SDBS pollution.
2.Starch derived carbon aerogels with high-performance for sorption of cationic dyes
A synthetic strategy to prepare CAs by the carbonization of starch aerogels from its corresponding wet-gels through the ambient pressure drying process. The textural characteristics of CAs could be tailored by adjusting the carbonization temperature and activation time.Thus the technique of CA synthesis is relatively simple and with low cost for the short gelation time and ambient pressure drying.To prepare CAs,the esculent and soluble starch was dissolved into water to form the wet-gels,after the water in the gels was exchanged by acetone,the acetone gels were dried at ambient pressure to obtain the white starch aerogels,which were carbonized in N_2 flow.SEM images show that the starch aerogels exhibit a fibrillar solid network with a diameter of 30-40 nm and CAs consist of flakes with a side-length of 60-120μm as the starch aerogels were carbonized at 850℃for 2.0 h.When the magnification is 200,the carbon aerogels keep the same shape after activating with CO_2.SEM image of ACAs show high mesoporosity,obviously. However,SEM image of CAs don't show mesoporous structure.The N_2 adsorption measurements indicate that the specific surface area of CAs is 137 m~2/g and the average pore size is 1.54 nm,only few mesopores are observed according to the BET pore size distribution(PSD).However,the specific surface areas of starch aerogel(calculated using BET model) was 103 m~2/g and PSD ranged from 3 nm to 80 nm,typical of mesoporous and macroporous solids.Further experiments show that the suitable activation conditions could increase the specific surface areas and pore volume of CAs,which increased with the activate time prolonging.After activations the CAs contained both micropores and mesopores,its average micropore size is 0.89 nm,and all the mesopore size are in the range of 2-10 nm whatever the activation time is, which reveals that the activation process creates new micropore and mesopore structures.For example,the largest specific surface areas of CAs increased to 1571 m~2/g after being activated at 800℃for 7.0 h under CO_2 flow.The pH value of solution considerably affected the adsorption amounts of basic dyes on the CAs.For example,as the pH value of dye solution is 10 and dye's solution is 500 ppm,the absorption amount is the largest,those for CV,MV and MB are respectively 1515,1423 and 1181 mg/g.
3.Synthesis,characterization and application of chitosan/gelatin/genipin aerogels
New natural polymer-based aerogels,cross-linked chitosan aerogels and chitosan-gelatin aerogels,were prepared by the sol-gel route with genipin as cross-linkers.The alcogels were dried by supercritical carbon dioxide(CO_2) fluid extraction.The resulting materials were characterized using scanning electron microscopy(SEM),nitrogen adsorption/desorption analysis.The Brunauer-Emmett-Teller(BET) analyses indicate that the largest surface areas for the natural polymers based aerogels are 567 m~2/g.The key factor to obtaining stable aerogels with a high specific surface areas is the full replacement of the solvent with absolute ethanol.If the solvent is not fully replaced by absolute ethanol,only a broken wet-gel will be produced.It was also found that carbon aerogels could not be produced after calcining the chitosan based aerogels under a flow of nitrogen because the thermal degradation of the main chains in chitosan and chitosan-based aerogels during heating destroyed the network structure.Furthermore,the adsorption of the anionic dyes sunset yellow and tartrazine from aqueous solution by the materials was investigated.The aerogels exhibit high adsorption capability, can remove sunset yellow and tartrazine from acidic aqueous solutions,and have potential applications in controlling anionic dyes pollution.
4.Synthesis,characterization and application of carrageenan based organic and carbon aerogels
Carrageenan based organic cyrogels and aerogels were prepared by the sol-gel route and freeze drying and supercritical carbon dioxide(CO_2) drying from its corresponding wet-gels,and carrageenan based carbon aerogels and cyrogels were prepared by the carbonization of carrageenan aerogels and cyrogels,respectively.The textural characteristics of carrageenan based carbon aerogels and cyrogels could be tailored by change dry method.Thus the technique of CA synthesis is relatively simple and with low cost for the short gelation time and freeze drying.To prepare CAs,the esculent and soluble carrageenan was dissolved into water to form the wet-gels,after the water in the gels was exchanged by alcohol,the alcogels were dried at supercritical carbon dioxide(CO_2) or freeeze to obtain the white carrageenan aerogels and cyrogels,which were carbonized in N_2 flow at 1000℃.SEM images show that the carrageenan aerogeis exhibit a fibrillar solid network with a diameter of 20 nm and carbon aerogels and cyrogels consist of carbon particles.SEM image of aerogels and cyrogels show high mesoporosity, obviously.However,SEM image of carbon aerogels don't show microporous structure.The N_2 adsorption measurements indicate that the largest specific surface area of organic aerogels is 346 m~2/g and the average pore size is 2.98 nm.However,the specific surface area of carbon cyrogels(calculated using BET model) was 1185 m~2/g and the average pore size are 0.85 and 3.9,typical of mesoporous and microporous solids.The pH value of solution considerably affected the adsorption amounts of basic dyes on the CAs.For example,as the pH value of dye solution is 10 and dye's solution is 500 ppm,the absorption amount is the largest,those for CV,MV are respectively 2207,1725 mg/g at pH 10.
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