纳米纤维素复合凝胶的制备和表征及其物化性能增强的研究
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摘要
纤维素作为地球上最丰富的可再生生物资源，具有价格低廉、产量丰富的特点，以天然纤维素为原料来获得纳米纤维素的各种制备手段已经非常成熟。纳米纤维素作为生物高聚物增强相，具有其他增强相无可比拟的特点。本论文并采用共聚法，以纳米纤维素为填料与聚合物基体复合构筑纳米纤维素复合凝胶，考察了纳米复合凝胶的合成机制，表征了纳米复合凝胶的表面形貌，并探讨了纳米复合凝胶在废水处理中的应用和吸附机制，为天然纤维素的高值化利用提供了一条新的途径。
在85%的磷酸溶解的纤维素溶液中，通过自由基接枝聚合反应制备了超吸水性的丙烯酸接枝纤维素（C-g-AA）水凝胶。分析了C-g-AA水凝胶在水溶液中的溶胀行为，考察了对废水中阳离子染料和重金属离子的去除行为。研究了接枝过程单体含量对于水凝胶性能的影响，以及水凝胶吸附过程受溶液pH值，吸附时间，初始离子浓度和竞争离子等各因素的影响。结果表明凝胶在水溶液中的溶胀具有明显的pH敏感性和pH可逆性，凝胶的溶胀率随着接枝制备中丙烯酸单体的增加而增加，最高可达73倍；凝胶对亚甲基蓝的平衡吸附量可达2197mg/g，对重金属离子，Cd2+、Pb2+和Ni2+的吸附容量分别为562.7，825.7和380.1mg/g，竞争吸附的亲和力顺序为Pb2+>Ni2+>Cd2+；凝胶具有重复利用性，70%的MB可以在弱酸溶液体系中被脱除，且重复使用三次后对重金属离子的吸附能力仍能达到原来的85%；水凝胶对阳离子染料和重金属离子的吸附等温线和动力学均分别符合Langmuir模型和准二级动力学模型。
利用酸水解、TEMPO氧化和超声机械水解三种不同的制备方法得到纳米纤维素。考察了纳米纤维素的形貌特征、表面电荷及尺寸分布。结果表明三种不同制备技术得到的纳米纤维素质量差异明显，TEMPO氧化得到的纳米纤维素具有较高的长宽比，高产率（37%）和高的表面电荷（-47mV）；酸水解得到的纳米纤维素具有高的结晶度（88.1%）和较好的尺寸分散性。通过溶液浇铸法制备不同纳米纤维素含量的PVA复合凝胶膜，研究和探讨了复合膜的机械性能、热性能以及界面交互性能。膜断裂面SEM分析发现AH和TEMPO方法得到的纳米纤维素能均一的分散在PVA基体中；力学性能测试发现在加载6wt%的纳米纤维素时，AH薄膜具有高的断裂伸长率，断裂伸长率为51.6%，而TEMPO薄膜的拉伸模量和拉伸强度都有不同程度的提高，分别提高21.5%和10.2%；此外TMO/PVA显示了较优的热稳定性。
以羧基化纳米纤维素纤维（CCNFs）为填料，与羧甲基纤维素基体共聚制备纳米纤维素复合凝胶微球。结果表明，CCNFs用量，溶液的pH值，体系温度以及盐溶液的种类和浓度均会对复合凝胶的溶胀行为造成影响；当CCNFs含量高至2.5wt%时，凝胶的溶胀量从245.8急剧增加至458.7g/g；CCNFs的加入提高了水凝胶的抗盐性能，使复合凝胶具有较慢的去溶胀率以及在平衡退溶胀时较高的保水能力；同时纳米复合水凝胶呈现更好的pH响应行为以及在不同温度下的高的保水能力；通过凝胶化法制备了CCNFs和胺基铁粒子两种纳米粒子混合填充的磁响应壳聚糖水凝胶微球。SEM分析发现磁性铁纳米粒子很好地分散在整个三维空间结构，CCNFs互相交织的特性使得水凝胶网络结构的空隙变窄，使得结构更加密集。水凝胶的磁响应性来源于添加的铁纳米粒子的磁响应性，可以在外部磁力的帮助下很容易与该溶液分离；复合凝胶对Pb2+离子有较高的吸附能力，吸附量高至171.0mg/g。
通过定向冷冻模塑技术成功的制备了纳米纤维素微晶（CNWs）气凝胶，在常用载体水溶液中加入少量DMSO（0.5%~1.5%v/v）作为混合溶剂，能够显著的影响气凝胶的孔的形态。混合溶剂中DMSO浓度越高，SEM观察到的气凝胶的微观结构越粗糙。当混合溶液中DMSO含量增加时，气凝胶层状结构会相应的产生变化，层厚度，层间距，和顶部孔直径均会提高。跟未添加DMSO溶剂的体系相比，当DMSO的浓度继续增加到1.5%时，气凝胶的密度从22.2增加至45.3kg·m-3，压缩应力和压缩模量分别提高至94.6kPa和526.8kPa。冷却条件的不同会影响气凝胶的孔洞特性，也同样会直接反应在气凝胶材料的抗压缩强度上。定向冷冻条件下得到具有方向性的孔洞形貌的气凝胶材料相比非定向条件下得到的具有不规则孔洞形貌的气凝胶显示更优的机械性能。
Cellulose is a high-molecular weight linear homopolymer constituted of repeatingβ-D-glucopyranosyl units joined by l→4-glycosidic linkages, is the most abundant, renewableand biodegradable natural polymer. Many techniques have been developed to obtainnano-scaled cellulose from natural cellulose material. These nanocelluloses are able toprovide reinforcement in a wild variety of composites. In this work, nanocellulose was usedas nanofillers in the polymer matrix to build nanocomposite hydrogels, provides a new way totake advantage of high-value natural cellulose.
Cellulose-graft-acrylic acid (C-g-AA) hydrogels were prepared via free radicalpolymerization in85%homogeneous phosphoric acid solution. The results showed that thehydrogels have obvious pH sensitivity and pH reversibility. The swelling ratio in distilledwater was increased with increasing of AA components in hydrogels, it can exceeded7327%with mole ratio of6:1(AA/Cellulose); The C-g-AA hydrogels have a porous network innerstructure with cellulose as the backbone, it has excellent dye and metal ions equilibriumadsorption capacity, for methylene blue (MB) was2197mg·g-1and for the heavy metal ionswere562.7(Cd2+),825.7(Pb2+), and380.1mg/g (Ni2+), respectively. The observed affinityorder of competitive ions adsorption is Pb2+>Ni2+>Cd2+in mmol/g. The effects of mole ratioof AA to cellulose, the pH of adsorption medium and the initial concentration on MB or metalions adsorption capacity of hydrogels were investigated. Both the adsorption isotherm andkinetics fit the Langmuir model and the Pseudo-second-order model well, respectively. SEMimages and FTIR spectra before and after adsorption on the hydrogels revealed that thecomplexation between dye (or metal ions) and carboxyl groups on hydrogels was the mainadsorption mechanism.
Three techniques including acid hydrolysis (AH), TEMPO-mediated oxidation (TMO)and ultrasonication (US) were introduced to obtain nanocellulose. Important differences werenoticed in fiber quality of nanocellulose and film properties of poly(vinyl alcohol)(PVA)nanocomposite films. The TMO treatment was more efficient in nanocellulose isolation withhigher aspect ratio, surface charge (-47mV) and yields (37%). While AH treatment resultedin higher crystallinity index (88.1%) and better size dispersion. The fracture surface, thermalbehavior and mechanical properties of the PVA nanocomposite films were investigated bymeans of SEM, DSC, TGA and tensile testing. The results shown that both the TMO-derivedand AH-derived nanocellulose could homogeneous disperse in the PVA matrices. AH/PVAfilms had higher elongation at break (51.59%at6wt%nanocellulose loading) as compared with TMO/PVA, while TMO/PVA films shown superior tensile modulus and strength withincrements of21.5%and10.2%at6wt%nanocellulose loading. The thermal behavior of thePVA nanocomposite films was higher improved with TMO-derived nanofibrils addition.
Nanocomposite hydrogels based on carboxylated cellulose nanofibrils (CCNFs) andcarboxymethyl cellulose-g-poly(acrylic acid-co-acrylamide) were synthesized. A series ofexperiments were performed to evaluate the influence of factors such as CCNFs amount,solution pH, temperature, salt solution type and concentration on the swelling behaviors of thehydrogels. The swelling capacity in distilled water increased dramatically from245.8to458.7g/g with the addition of CCNFs up to2.5wt%. The incorporation of CCNFs improved saltresistance properties of the hydrogels with slower deswelling rate and higher water retentioncapacity at deswelling equilibrium. Furthermore, the nanocomposite hydrogels presentedbetter responsive behavior in relation to pH presence and showed an increase in waterretention capacity at various temperatures.
Novel magnetic hydrogel beads (m-CS/PVA/CCNFs), consisting of CCNFs,amine-functionalized magnetite nanoparticles and PVA blended chitosan, were prepared byan instantaneous gelation method. SEM, XRD, and TGA techniques were applied toinvestigate the structure of the hydrogel materials. SEM revealed that magnetite nanoparticlewas well dispersed in space throughout the3D structure. The average diameter of CCNFsblended magnetic hydrogels was quite smaller than that of the unblended samples for theCCNFs narrowed the voids network in hydrogels and rendered the structures denser. Themagnetic nature of m-CS/PVA/CCNFs hydrogels was validated as magnetite nanoparticle.Hydrogels can be separated easily from the solution with the help of an external magneticforce. The hydrogels exhibit higher Pb2+adsorption capacity with the value of171.0mg/g.
Free-standing cellulose nanowhikers (CNWs) foams were successfully prepared inH2O-DMSO binary solvent through freeze-casting technique. The addition of0.5%~1.5%v/vDMSO in water had a significant influence on the pore morphology of the foams, with higherDMSO concentrations, the structure sizes, including the pore diameter on the top view, thelamellae thickness and interlamellae spaces on the side view can be increased to a certainextent. Compared with foams prepared from water, the foams in H2O-DMSO mixture showspotential for strongly improved mechanical properties. The cooling conditions also stronglyimpact the porosity features, and have a direct repercussion on the compressive strength.
在85%的磷酸溶解的纤维素溶液中，通过自由基接枝聚合反应制备了超吸水性的丙烯酸接枝纤维素（C-g-AA）水凝胶。分析了C-g-AA水凝胶在水溶液中的溶胀行为，考察了对废水中阳离子染料和重金属离子的去除行为。研究了接枝过程单体含量对于水凝胶性能的影响，以及水凝胶吸附过程受溶液pH值，吸附时间，初始离子浓度和竞争离子等各因素的影响。结果表明凝胶在水溶液中的溶胀具有明显的pH敏感性和pH可逆性，凝胶的溶胀率随着接枝制备中丙烯酸单体的增加而增加，最高可达73倍；凝胶对亚甲基蓝的平衡吸附量可达2197mg/g，对重金属离子，Cd2+、Pb2+和Ni2+的吸附容量分别为562.7，825.7和380.1mg/g，竞争吸附的亲和力顺序为Pb2+>Ni2+>Cd2+；凝胶具有重复利用性，70%的MB可以在弱酸溶液体系中被脱除，且重复使用三次后对重金属离子的吸附能力仍能达到原来的85%；水凝胶对阳离子染料和重金属离子的吸附等温线和动力学均分别符合Langmuir模型和准二级动力学模型。
利用酸水解、TEMPO氧化和超声机械水解三种不同的制备方法得到纳米纤维素。考察了纳米纤维素的形貌特征、表面电荷及尺寸分布。结果表明三种不同制备技术得到的纳米纤维素质量差异明显，TEMPO氧化得到的纳米纤维素具有较高的长宽比，高产率（37%）和高的表面电荷（-47mV）；酸水解得到的纳米纤维素具有高的结晶度（88.1%）和较好的尺寸分散性。通过溶液浇铸法制备不同纳米纤维素含量的PVA复合凝胶膜，研究和探讨了复合膜的机械性能、热性能以及界面交互性能。膜断裂面SEM分析发现AH和TEMPO方法得到的纳米纤维素能均一的分散在PVA基体中；力学性能测试发现在加载6wt%的纳米纤维素时，AH薄膜具有高的断裂伸长率，断裂伸长率为51.6%，而TEMPO薄膜的拉伸模量和拉伸强度都有不同程度的提高，分别提高21.5%和10.2%；此外TMO/PVA显示了较优的热稳定性。
以羧基化纳米纤维素纤维（CCNFs）为填料，与羧甲基纤维素基体共聚制备纳米纤维素复合凝胶微球。结果表明，CCNFs用量，溶液的pH值，体系温度以及盐溶液的种类和浓度均会对复合凝胶的溶胀行为造成影响；当CCNFs含量高至2.5wt%时，凝胶的溶胀量从245.8急剧增加至458.7g/g；CCNFs的加入提高了水凝胶的抗盐性能，使复合凝胶具有较慢的去溶胀率以及在平衡退溶胀时较高的保水能力；同时纳米复合水凝胶呈现更好的pH响应行为以及在不同温度下的高的保水能力；通过凝胶化法制备了CCNFs和胺基铁粒子两种纳米粒子混合填充的磁响应壳聚糖水凝胶微球。SEM分析发现磁性铁纳米粒子很好地分散在整个三维空间结构，CCNFs互相交织的特性使得水凝胶网络结构的空隙变窄，使得结构更加密集。水凝胶的磁响应性来源于添加的铁纳米粒子的磁响应性，可以在外部磁力的帮助下很容易与该溶液分离；复合凝胶对Pb2+离子有较高的吸附能力，吸附量高至171.0mg/g。
通过定向冷冻模塑技术成功的制备了纳米纤维素微晶（CNWs）气凝胶，在常用载体水溶液中加入少量DMSO（0.5%~1.5%v/v）作为混合溶剂，能够显著的影响气凝胶的孔的形态。混合溶剂中DMSO浓度越高，SEM观察到的气凝胶的微观结构越粗糙。当混合溶液中DMSO含量增加时，气凝胶层状结构会相应的产生变化，层厚度，层间距，和顶部孔直径均会提高。跟未添加DMSO溶剂的体系相比，当DMSO的浓度继续增加到1.5%时，气凝胶的密度从22.2增加至45.3kg·m-3，压缩应力和压缩模量分别提高至94.6kPa和526.8kPa。冷却条件的不同会影响气凝胶的孔洞特性，也同样会直接反应在气凝胶材料的抗压缩强度上。定向冷冻条件下得到具有方向性的孔洞形貌的气凝胶材料相比非定向条件下得到的具有不规则孔洞形貌的气凝胶显示更优的机械性能。
Cellulose is a high-molecular weight linear homopolymer constituted of repeatingβ-D-glucopyranosyl units joined by l→4-glycosidic linkages, is the most abundant, renewableand biodegradable natural polymer. Many techniques have been developed to obtainnano-scaled cellulose from natural cellulose material. These nanocelluloses are able toprovide reinforcement in a wild variety of composites. In this work, nanocellulose was usedas nanofillers in the polymer matrix to build nanocomposite hydrogels, provides a new way totake advantage of high-value natural cellulose.
Cellulose-graft-acrylic acid (C-g-AA) hydrogels were prepared via free radicalpolymerization in85%homogeneous phosphoric acid solution. The results showed that thehydrogels have obvious pH sensitivity and pH reversibility. The swelling ratio in distilledwater was increased with increasing of AA components in hydrogels, it can exceeded7327%with mole ratio of6:1(AA/Cellulose); The C-g-AA hydrogels have a porous network innerstructure with cellulose as the backbone, it has excellent dye and metal ions equilibriumadsorption capacity, for methylene blue (MB) was2197mg·g-1and for the heavy metal ionswere562.7(Cd2+),825.7(Pb2+), and380.1mg/g (Ni2+), respectively. The observed affinityorder of competitive ions adsorption is Pb2+>Ni2+>Cd2+in mmol/g. The effects of mole ratioof AA to cellulose, the pH of adsorption medium and the initial concentration on MB or metalions adsorption capacity of hydrogels were investigated. Both the adsorption isotherm andkinetics fit the Langmuir model and the Pseudo-second-order model well, respectively. SEMimages and FTIR spectra before and after adsorption on the hydrogels revealed that thecomplexation between dye (or metal ions) and carboxyl groups on hydrogels was the mainadsorption mechanism.
Three techniques including acid hydrolysis (AH), TEMPO-mediated oxidation (TMO)and ultrasonication (US) were introduced to obtain nanocellulose. Important differences werenoticed in fiber quality of nanocellulose and film properties of poly(vinyl alcohol)(PVA)nanocomposite films. The TMO treatment was more efficient in nanocellulose isolation withhigher aspect ratio, surface charge (-47mV) and yields (37%). While AH treatment resultedin higher crystallinity index (88.1%) and better size dispersion. The fracture surface, thermalbehavior and mechanical properties of the PVA nanocomposite films were investigated bymeans of SEM, DSC, TGA and tensile testing. The results shown that both the TMO-derivedand AH-derived nanocellulose could homogeneous disperse in the PVA matrices. AH/PVAfilms had higher elongation at break (51.59%at6wt%nanocellulose loading) as compared with TMO/PVA, while TMO/PVA films shown superior tensile modulus and strength withincrements of21.5%and10.2%at6wt%nanocellulose loading. The thermal behavior of thePVA nanocomposite films was higher improved with TMO-derived nanofibrils addition.
Nanocomposite hydrogels based on carboxylated cellulose nanofibrils (CCNFs) andcarboxymethyl cellulose-g-poly(acrylic acid-co-acrylamide) were synthesized. A series ofexperiments were performed to evaluate the influence of factors such as CCNFs amount,solution pH, temperature, salt solution type and concentration on the swelling behaviors of thehydrogels. The swelling capacity in distilled water increased dramatically from245.8to458.7g/g with the addition of CCNFs up to2.5wt%. The incorporation of CCNFs improved saltresistance properties of the hydrogels with slower deswelling rate and higher water retentioncapacity at deswelling equilibrium. Furthermore, the nanocomposite hydrogels presentedbetter responsive behavior in relation to pH presence and showed an increase in waterretention capacity at various temperatures.
Novel magnetic hydrogel beads (m-CS/PVA/CCNFs), consisting of CCNFs,amine-functionalized magnetite nanoparticles and PVA blended chitosan, were prepared byan instantaneous gelation method. SEM, XRD, and TGA techniques were applied toinvestigate the structure of the hydrogel materials. SEM revealed that magnetite nanoparticlewas well dispersed in space throughout the3D structure. The average diameter of CCNFsblended magnetic hydrogels was quite smaller than that of the unblended samples for theCCNFs narrowed the voids network in hydrogels and rendered the structures denser. Themagnetic nature of m-CS/PVA/CCNFs hydrogels was validated as magnetite nanoparticle.Hydrogels can be separated easily from the solution with the help of an external magneticforce. The hydrogels exhibit higher Pb2+adsorption capacity with the value of171.0mg/g.
Free-standing cellulose nanowhikers (CNWs) foams were successfully prepared inH2O-DMSO binary solvent through freeze-casting technique. The addition of0.5%~1.5%v/vDMSO in water had a significant influence on the pore morphology of the foams, with higherDMSO concentrations, the structure sizes, including the pore diameter on the top view, thelamellae thickness and interlamellae spaces on the side view can be increased to a certainextent. Compared with foams prepared from water, the foams in H2O-DMSO mixture showspotential for strongly improved mechanical properties. The cooling conditions also stronglyimpact the porosity features, and have a direct repercussion on the compressive strength.
引文
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